NOVEMBER/DECEMBER 2016 | VOL 174 | NO 10

AN ASM INTERNATIONAL PUBLICATION

MATERIALS TESTING/CHARACTERIZATION CORRELATIVE MICROSCOPY OF NEUTRON-IRRADIATED MATERIALS P.16

22 3D LASER MICROSCOPY

26 BIOMATERIALS TESTING

HTPro and iTSSe NEWSLETTERS 31 INCLUDED IN THIS ISSUE

NOVEMBER/DECEMBER 2016 | VOL 174 | NO 10

AN ASM INTERNATIONAL PUBLICATION

MATERIALS TESTING/CHARACTERIZATION CORRELATIVE MICROSCOPY OF NEUTRON-IRRADIATED MATERIALS P.16

22 3D LASER MICROSCOPY

26 BIOMATERIALS TESTING

HTPro and iTSSe NEWSLETTERS 31 INCLUDED IN THIS ISSUE Like a kid in a Candy Store That’s how you’ll feel at goodfellowusa.com

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HEAT10.22-24.17 TREATING SOCIETY CONFERENCE & EXPOSITION CALL FOR PAPERS IS OPEN! Heat Treat 2017, the biennial co-located show from the ASM Society and the American Gear Manufacturers Association, is where heat treating professionals go to take stock of the industry and predict what’s coming in the future. Submit your 100-150 word abstract by December 30, 2016. Topics of interest include, but are not limited to:

• Additive Manufacturing/3D Processing • Advances in Heat Treating • Induction Heat Treating • and Cooling • Vacuum Processes and Technology

GREATER COLUMBUS CONVENTION CENTER COLUMBUS, OH, USA • OCTOBER 22-24 2017 CALL FOR ABSTRACTS DEADLINE: December 30, 2016

FOR MORE INFORMATION, VISIT THE WEB AT: WWW.ASMINTERNATIONAL.ORG/HEATTREAT

Organized By: Co-Located With: 2

16 On The Cover: High Flux Isotope Reactor CORRELATIVE MICROSCOPY OF core during a routine refueling NEUTRON-IRRADIATED MATERIALS operation. Courtesy of Oak Ridge National Laboratory, Samuel Briggs, Kumar Sridharan, and Kevin Field US Dept. of Energy. ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED Development of new, radiation-tolerant materials that maintain the structural integrity and safety margins over the course of a nuclear power reactor’s service life requires the ability to predict degradation phenomena.

26 29 69 TECHNICAL SPOTLIGHT METALLURGY LANE ASM NEWS BIOMATERIALS TESTING THE DECLINE OF THE The monthly publication about ASM members, chapters, events, awards, AND CHARACTERIZATION INTEGRATED affiliates, and other Society activities. Mechanical characterization of bioma- INDUSTRY—PART I terials, both natural and engineered, is Charles R. Simcoe usually achieved with a combination of From poor labor relations to delayed both static and fatigue testing. modernization, the U.S. steel industry began its steady decline in the late 1950s. 3 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

NOVEMBER/DECEMBER 2016 | VOL 174 | NO 10

FEATURES 22 ADVANTAGES OF 3D LASER SCANNING CONFOCAL MICROSCOPY John Shingledecker, John Siefert, Daniel Purdy, Jonathan Tedesco, and Andrew Szafarczyk 3D laser microscopy is opening new areas of study for metallic alloys and coatings in power generation applications.

31 iTSSe The official newsletter of the ASM Thermal Spray Society (TSS). This quarterly supplement focuses on thermal spray and related surface engineering technologies along 14 with Thermal Spray Society news and initiatives.

49 HTPro The official newsletter of the ASM Heat Treating Society (HTS). This quarterly supplement focuses on heat treating technology, processes, materials, and equipment, along with Heat Treating Society news and initiatives. 31 49

Advanced Materials & Processes (ISSN 0882-7958, USPS 762080) is published monthly, except bimonthly July/August and November/December, by ASM International, 9639 Kinsman Road, Materials Park, OH TRENDS INDUSTRY NEWS DEPARTMENTS 44073-0002; tel: 440.338.5151; fax: 440.338.4634. Periodicals postage paid at Novelty, Ohio, and additional 4 Editorial 8 Metals/Polymers/Ceramics 77 Classifieds mailing offices. Vol. 174, No.10, NOVEMBER/DECEMBER 2016. Copyright © 2016 by ASM International. All 6 Market Spotlight 10 Testing/Characterization 77 Editorial Preview rights reserved. Distributed at no charge to ASM members in the United States, Canada, and Mexico. In- 6 Feedback 12 Emerging Technology 77 Special Advertising Section ternational members can pay a $30 per year surcharge to receive printed issues. Subscriptions: $475. Single 7 OMG! 13 Process Technology 77 Advertisers Index copies: $51. POSTMASTER: Send 3579 forms to ASM International, Materials Park, OH 44073-0002. 14 Energy Trends 79 Stress Relief Change of address: Request for change should include old address of the subscriber. Missing numbers due 15 Surface Engineering 80 3D PrintShop to “change of address” cannot be replaced. Claims for nondelivery must be made within 60 days of issue. Canada Post Publications Mail Agreement No. 40732105. Return undeliverable Canadian addresses to: 700 Dowd Ave., Elizabeth, NJ 07201. Printed by Publishers Press Inc., Shepherdsville, Ky.

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ASM International serves materials professionals, nontechnical personnel, and managers wordwide by providing high-quality materials information, education and training, networking opportunities, and professional development resources in cost-effective and user-friendly formats. ASM is where materials users, producers, and manufacturers converge to do business. 4 THOUGHTFUL LECTURES OFFER ASM International 9639 Kinsman Road, Materials Park, OH 44073 INTRIGUE AND INSPIRATION Tel: 440.338.5151 • Fax: 440.338.4634 t is almost impossible to believe we are wrapping up the final edition of AM&P for 2016. With this in mind, it seems Frances Richards, Editor-in-Chief [email protected] that the annual Materials Science & Technology (MS&T) Iconference occurs at an ideal time—during October, while Julie Lucko, Editor [email protected] we still have a chance to think about the year to date and Ed Kubel and Erika Steinberg, Contributing Editors before we are distracted by the joys and challenges of the Jim Pallotta, Creative Director holiday season. The “big picture” lectures at MS&T con- [email protected] tinue to amaze and inspire, and this year is no exception. Kate Fornadel, Layout and Design Rapid changes in society and commerce were important themes of sev- Kelly Sukol, Production Manager eral talks at MS&T, in addition to global engineering challenges. As usual, the [email protected] Alpha Sigma Mu lecture was outstanding with Al Romig, FASM, speaking about Press Release Editor [email protected] the “14 grand challenges for engineering in the 21st century” as determined by the National Academy of Engineer- EDITORIAL COMMITTEE ing (NAE). Romig, executive offi- Somuri Prasad, Chair, Sandia National Lab cer of this academy, outlined the Adam Farrow, Vice Chair, Los Alamos National Lab Jaimie Tiley, Past Chair, U.S. Air Force Research Lab mega-engineering problems of our Ellen Cerreta, Board Liaison, Los Alamos day. All revolve around themes of National Lab “continuation of life on the planet, Tomasz Chojnacki, Caterpillar Inc. Mario Epler, Carpenter Technology Corp. and making our world more sus- Yaakov Idell, NIST tainable, safe, healthy, and joy- Hideyuki Kanematsu, Suzuka National ful.” For example, goals include College of Technology John Shingledecker, EPRI making solar energy economical, ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED Kumar Sridharan, University of Wisconsin engineering better medicines, pro- Signage in front of the Salt Lake City viding energy from fusion, prevent- Convention Center. ASM BOARD OF TRUSTEES ing nuclear terror, and engineering William E. Frazier, President the tools of scientific discovery. Romig highlighted the importance of the Grand Frederick E. Schmidt, Jr., Vice President Jon D. Tirpak, Immediate Past President Challenge scholar program to prepare future talent to solve these problems. Craig D. Clauser, Treasurer For more information, visit engineeringchallenges.org. Ellen K. Cerreta Speaking about other massive changes in how business is conducted today Kathryn Dannemann Ryan M. Deacon was Diran Apelian, FASM, of Worcester Polytechnic Institute. In a lively panel dis- Larry D. Hanke cussion on collaborative research programs, Apelian began his talk by posing Roger A. Jones four intriguing questions and providing the answers after the audience guessed: Sudipta Seal Tirumalai S. Sudarshan What company is the world’s largest taxi company? (Uber, but they own no David B. Williams vehicles.) What company is the world’s most popular media owner? (Facebook, John D. Wolodko but they create no content.) Who is the world’s most valuable retailer? (Alibaba, William T. Mahoney, Secretary and Managing Director but they have no inventory.) Who is the world’s largest accomodation provider? (Airbnb, but they own no real estate.) Apelian asserted that the most important STUDENT BOARD MEMBERS assets of these companies are knowledge and people, which is the same for Swetha Barkam, Allison Fraser, Rachael Stewart every organization—including universities. He went on to make some excellent Individual readers of Advanced Materials & Processes may, observations about what makes a successful collaboration. without charge, make single copies of pages therefrom for per- sonal or archival use, or may freely make such copies in such The plenary session was also intriguing and thought provoking. Julie numbers as are deemed useful for educational or research Christodoulou, FASM, provided a fascinating history of microscopy and charac- purposes and are not for sale or resale. Permission is granted to cite or quote from articles herein, provided customary terization tools beginning with Pliny the Elder and continuing through today’s acknowledgment of the authors and source is made. technological advancements such as dynamic 3D digital modeling and preces- The acceptance and publication of manuscripts in Advanced sion electron diffraction. Her main point was that with today’s wealth of sophis- Materials & Processes does not imply that the reviewers, editors, or publisher accept, approve, or endorse the data, ticated tools, scientists and engineers must choose projects carefully to use the opinions, and conclusions of the authors. powerful equipment at their disposal and move progress forward. David Mat- lock, FASM, then gave an interesting talk on fatigue performance of steel and con- cluded that a great need still exists to teach “good, common sense engineering.” In other news, we wish you all a happy and healthy holiday season! See you in 2017. 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METAL MATRIX COMPOSITES MARKET HOLDS PROMISE According to a new report from at a CAGR of 5.3%. The space research FEEDBACK BCC Research, Wellesley, Mass., inter- and defense systems market should est in metal matrix composites (MMCs) reach $52.5 million by 2020 from remains high due to properties such $37.6 million in 2015, at a five-year as greater stiffness, better wear resis- CAGR of 6.9%. The space and defense tance, lower density, and other bene- systems, nuclear energy, and aircraft SERIOUSLY SCARY Thank you for your astute insight on fits compared to standard materials. industry MMC markets should experi- artificial intelligence (AI), “Serious Matters,” Despite these advantages, however, ence the strongest growth. Geograph- October issue. Back in the 1960s, the movie the market remains modest compared ically, the most rapid consumption “2001: A Space Odyssey” profoundly affected with its potential, according to ana- will occur in China and other East my thinking on computers. An astronaut at lysts. MMCs combine high strength Asian nations as a sizeable share of the end of an interstellar voyage finds himself and stiffness, low weight, corrosion many key end-use market industries the lone survivor on board his spacecraft. resistance, and in some cases special migrate to China and elsewhere. Other astronauts are found dead in their electrical properties. This combination Reducing the cost of manufac- cryogenic beds. Dave, the live astronaut, makes them very attractive for aircraft turing MMC components would aid discovers that the computer, HAL 9000, has and aerospace structural parts among use in cost-sensitive industries such taken over the ship. Soon he is in back of the other applications. The most common as transportation. Both private sec- computer’s power supplies disabling it. As he MMCs are aluminum, magnesium, and tor and public initiatives seek to pro- begins shutting it down, the computer speaks

ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED copper/titanium alloys as a matrix, mote MMC use in non-transportation to him. “Dave? ... I wouldn’t do that if I were with aluminum oxide and silicon car- and non-aerospace applications. you Dave.” This is the signature line of the bide as reinforcements. Some technological and economic movie. I sure hope a takeover by AI wouldn’t The global MMC market is fore- barriers have been overcome, get that close before we recognized what cast to reach $431.1 million by 2020, although not at the pace most indus- could be done about it. up from $326.9 million in 2015, reflect- try participants prefer. High produc- Dana Wilson ing a five-year compound annual tion costs, availability, informational, SERIOUSLY SKEPTICAL growth rate (CAGR) of 5.7%. The larg- and technical issues continue to bar I’m a serious skeptic about AI. This might est application market, ground trans- market expansion. For more informa- be something to be used in smartphones and portation, should reach $203.2 million tion on Metal Matrix Composites: The computers, but can you imagine a machine by 2020 from $156.9 million in 2015, Global Market, visit bccresearch.com. being able to decide what makes for a good technical publication like AM&P? A machine Global MMCs Market by Industry, 2014-2020 ($ Millions) that can decide what a guy like me wants to see? NOT. I think your job is more than safe. In other news, have you been following the driverless car thing? One of the ladies in our group has placed an order for one of the TBD Tesla cars that will have that technology. She loves the idea. Granted, there are some bad drivers out there, but I don’t see this as an improvement. And I definitely put it in the “what could possibly go wrong” category. Two words that should strike fear into the hearts of even the most enthusiastic propo- nents of driverless cars? Software updates. T.R. We welcome all comments and suggestions. Send letters to [email protected]. Source: BCC Research 7 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

- - - - - micro Julie Lucko at Julie Lucko Materials Goodness? Goodness? Materials Send your submissions to submissions to Send your that exhibit OMG - Outrageous OMG - Outrageous that exhibit The vehicle relies on more than on more relies The vehicle Driving is controlled by a system a system by Driving is controlled [email protected]. Are you working with or have you you with or have working you Are Olli, an autonomous shuttle, at the Na- Olli, an autonomous tional Harbor in Maryland. discovered a material or its properties or its properties a material discovered eral software and tech partners. IBM is partners. tech and software eral but is providing not doing the driving can so passengers the user interface with Olli. Using “conversations” have help can recognition language natural pas the between relationship a create Bret IBM’s says vehicle, and the senger understands that vehicle “A Greenstein. walk can you where human language, that work,’ to get to like ‘I’d in and say, enjoy and relax as a passenger you lets he explains. journey,” your from of data and streams sensors 30 software, cloud. With the Watson IBM’s the vehicle ask how can passengers and why going, they are where works, decisions. driving Olli is making certain ques dreaded the answer it can And offer It also can yet?” there we tion, “Are popular restau for recommendations on user based sites or historical rants localmotors.com. preferences. in a matter of hours. of hours. in a matter factories with sev Motors Local developed by mon with a mobile app, like Uber. And itAnd Uber. like mobile app, with a mon in specification to be printed can tion sum solution can that passengers

------OMG! The team, led by professor Oral Oral professor led by The team, A new self-driving vehicle—a A new self-driving MIT researchers are seeking to redesign seeking to are MIT researchers blueprints. nature’s by following concrete tion: Oral Buyukozturk, obuyuk@mit. Buyukozturk, tion: Oral edu, web.mit.edu. and properties of natural materials such materials of natural and properties sponges. deep-sea and shells, bones, as observed, these biolog As researchers strong exceptionally are materials ical their pre to thanks in part and durable, at multiple cise assembly of structures the the molecular to from length scales, level. macro design- for approach bottom-up spired, are materials “These paste. cement ing with fashion, assembled in a fascinating in com arranging simple constituents that are configurations geometric plex see observe. to to We want beautiful exist what kinds of micromechanisms such superior within them that provide adopt a can we and how properties approach similar building-block-based cement, replace can If we concrete. for other some with totally, or partially and that may be readily materials can we in nature, amply available sustainability,” for objectives our meet informa more says. For Buyukozturk Buyukozturk, proposed a new a bioin proposed Buyukozturk, - minibus named Olli, capa 3D-printed ble of carrying unveiled 12 people—was Motors Local startup Arizona-based by D.C. Olli was outside Washington, designed as an on-demand transporta on-demand designed as an OLLI TAKES YOU FOR A RIDE YOU OLLI TAKES

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OUTRAGEOUS MATERIALS GOODNESS MATERIALS OUTRAGEOUS - mackenziefly Researchers at Massachusetts at Massachusetts Researchers “We have taken the best of everyof best the - taken have “We World champion angler Scott World champion angler Scott The Mackenzie FX1 is the first FX1 The Mackenzie double-handed salmon rod todouble-handed rod salmon use graphene.

Institute of Technology, Cambridge, Cambridge, of Technology, Institute fol by concrete redesign seeking to are The team blueprints. nature’s lowing paste—concrete’s cement contrasted the structure binding ingredient—with fishing.com. fishing.com. Mackenzie and NASA engineer Gary and NASA engineer Mackenzie they say made the first have Savage a dou- using graphene, fishing rod the called ble-handed rod salmon is recovery The fast FX1. Mackenzie further cast to it easier make said to are with little effort. in the rod Blanks in the UK using a unique built entirely a clave, auto A high-pressure process: parts make to used normally machine removes and aerospace, racing auto for mak rod air than the traditional more a much stronger creating ing process, is extremely blank. the FX1 This means or soften and won’t durable, strong, time. over lose performance One in Formula learned have thing we ever made. the best fly rod create to oppor exciting We had an incredibly fishing salmon of art the take to tunity a whole new harnessing level by to any before right way in the graphene changer game a is rod The else. one and less experienced both experts for says Savage. anglers,” CONCRETE GETS A MAKEOVER CONCRETE GETS A MAKEOVER GRAPHENE GOES FISHING 8 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 and steel components for thetrans COOLS SKIN PLASTIC CLOTHING 4°F cooler wore thanifthey cotton that would make thewearer feel nearly the bodyto discharge heat intwo ways thetic fabrics worn today. more efficientlythanthenatural orsyn- clothing, could cool aperson’s body far The plastic-based textile, ifwoven into reducing theneedfor airconditioning. basis for clothingthatcools thewearer, tic material that could become the sity, Calif., engineered alow-cost plas ings andmachinesiron, aluminum, factures gray andductileiron cast acquired BrillionIron Works Inc., the casting design andproduction BRIEFS ductile products. MPGmanu- of gray, ductile,andaustempered Brillion, Wis.,whichspecializes in portation andindustrialmarkets. Metaldyne Performance Group Inc. (MPG),Southfield,Mich., The material works by allowing Researchers atStanford Univer treatments to make acooling fabric. Courtesy ofL.A.Cicero. Stanford researchers modifiedasheet ofpolyethylene withaseriesofchemical METALS |POLYMERS |CERAMICS mpgdriven.com. - - - - EARTH MAGNETS RECOVERING RARE light. stanford.edu.light. through, anditisopaque to visible radiation, air, andwater vapor to pass clothing material—it allows thermal number ofcharacteristics desirable in to give polyethyleneand chemistry a blended nanotechnology, photonics, To textile, thenew develop researchers tion to pass through theplastic textile. person’s bodyemitsasinfrared radia clothing. It alsoallows theheat thata puter hard drives. Thepatent-pending rare earth magnets from usedcom an ORNLprocess designedto recover nonexclusive licensing agreement for tum Technologies, Dallas, signeda Laboratory (ORNL),Tenn., andMomen- research. autosteel.org. future. ItalsoidentifiesAHSS solutionsandrecommends areas for future mance, value, andhow AHSS meets thoserequirements now and inthe lated to design,fuel economy, strength, durability, environmental perfor high-strength steel (AHSS) material and manufacturing technologies re TechnologyIndustry Roadmap for Automotive, whichlooksatadvanced The Steel Market Development Institute, Detroit, released its 2016 Steel The DOE’s OakRidge National - - vehicles andwindturbines. energy technologies suchaselectric hard drives and cell phonesto clean fromare computer usedineverything side the U.S. The permanent magnets rare earth element that is minedout of magnets madeusingneodymium—a to economically recover large amounts Critical Materials Institute is designed process as developed part of DOE’s disassembly. Theprocess isdesigned may bepositionedfor correct robotic base ofeach make ofhard drive sothey measuring machine to populate a data- barcode scanning andacoordinate method usesamappingstation with drives onaconveyer for processing. The a uniquesystem to sortandalignhard cess for recovering magnets employs from usedcomputer hard drives. ORNL process helpsrecover magnets ORNL’s highlyautomated pro - - - - 9 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

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UV10 9/25/16 12:00 PM

EP51M LED401 mainmasterbond.com The surface of an aluminum strip was of an aluminum The surface etching with an electrochemical treated bonded with and permanently process of Courtesy thermoplastic by heating. Julia Siekmann/Kiel University. lock with each other in all directions other in all directions lock with each con a 3D puzzle. “These 3D puzzle like unbreakable. practically nections are usually the it was In our experiments, not the but or polymer that broke, metal notes. Carstensen itself,” connection www.uni-kiel.de/index.shtml. two treated metals, the surfaces inter the surfaces metals, treated two time Hackensack, NJ USA 07601 - - - www.masterbond.com wastingwastingwasting Rapid fixtureRapid time Speedy processing High performance Cost effective +1.201.343.8983 • Master Bond’s Master Bond’s Cure Fast Adhesives • • • • stop 1048LK_3.25x4.875_FastCure_40yr.indd 1 - con is metal a of surface The a 3D process, the etching Through lent, or improve their biocompatibility. their biocompatibility. lent, improve or The unique desired. modified as cally the does not damage process etching their stabil and does not affect metals permanently can we “In this way, ity. previously which could metals connect joined, such as copper not be directly Jürgen says researcher and aluminum,” Carstensen. an electrochemical etching process, in process, etching an electrochemical is a metal of layer the uppermost which a in scale on a micrometer roughened this Through manner. tightly controlled metals process, nanoscale-sculpturing or zinc can titanium, such as aluminum, all nearly be joined with permanently water-repel become other materials, which a semiconductor, into verted and specifi etched be chemically can If with tiny hooks is created. structure a bonding polymer is applied between - - - - Researchers at Kiel University, at Kiel University, Researchers The magnets may then be directly may then be directly The magnets Germany, changed the surface prop the surface changed Germany, their affecting without erties of metals char or physical stability mechanical on is based The method acteristics. ETCHING METAL CREATES CREATES METAL ETCHING BETTER BONDS to recover the magnets, their permalloy their permalloy the magnets, recover to and aluminum, boards, circuit brackets, destroying automatically while steel, security. ensure media to storage data manufactur drive hard by reused used in assemblies, motor or in ers or resizing through other applications rare to back or processed reshaping, can method The recycling metal. earth other consumer target to be adapted magnets, earth rare containing goods appli motors, such as used electric conditioning air and heating and ances, cmi.ameslab.gov. ornl.gov, systems. 10 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 steel. Specification for Additive Man- made of316L(UNS31603)stainless ufacturing Stainless Steel Alloy (UNS UNDER PRESSURE LAYERED MATERIALS BUCKLE layers whenthematerial iscompressed. rippling andbucklingofinterior atomic bulk materials called ripplocation—the structural deformation mechanismin typeof anew Philadelphia, observed published by ASTM International, West Conshohocken, Pa., for parts A new specificationA new for 3D-printed BRIEFS $4.2 billionfollowing receipt ofall S31603) withPowder BedFusion— Hillsboro, Ore., for approximately acquisition ofFEICompany Inc., stainless steel alloys willsoonbe Thermo FisherScientificInc.,

and mechanical requirements, required regulatory approvals. Waltham, Mass.,completed its The businesswillbecome part of ThermoFisher’s analytical F3184M—describes chemical corporate.thermofisher.com. ripple andbuckle.Courtesy ofDrexel University. When amaterial iscompressed, ripplocation occurs astheatomic layers inside Researchers atDrexel University, among others. astm.org. instruments segment. instruments segment. TESTING |CHARACTERIZATION The finding sheds new lightonthe The findingshedsnew were consistent withripplocation. wereshow they notdislocations but tron microscope images ofthedefects High-resolution transmission elec loaded withaspherical indenter. phase,inwhichthelayersMAX were ples ofalayered ceramic known asa ies. Thenresearchers examined sam- self-assembled into kinkboundar of amultitude ofripplocations that thenucleation andmotion observed while compressing thematerial, they constraining theedges ofthesample tions onabulksampleofgraphite. By pating considerable amountsofenergy. returning to itsoriginalform whiledissi- ripplocation describesthematerial be permanentlyindented. Incontrast, original form—in an elastic material—or willeitherbouncethey back to their rials are loaded and unloaded edge-on when theplanesoflayered solidmate tion inthesematerials, whichsaysthat of deformaheld dislocation theory This evidence supplantsthepreviously microscopy. ucla.edu, berkeley.edu, colorado.edu. single imagingmethods suchasoptical, x-ray, nano-probe, andelectron will focus on advancing real-time imagingby combining and improving riod, withthepossibilityof anadditionalfive-year extension. Thecenter $24 millionfrom theNationalScience Foundation over afive-year pe geles andBerkeley) andtheUniversity of Colorado Boulder, willreceive collaboration between scientistsfrom University of California (Los An- The Science andTechnology Center onReal-Time Functional Imaging,a The team ran atomistic simula - - - - - CLOSE LOOK MATERIAL INTERFACES GETA formations. drexel.edu. from asliver ofgraphite to geologic behavior ofmostlayered materials, scale resolution oflessthanone. created atasynchrotron, withatomic- reflectometry, whichexploits x-ray light ysis software based on resonant x-ray spacings. approach The new uses anal- ties change, often justa few atomic and thescale over whichtheirproper lenging dueto theirvaried behaviors these interfaces has typically been chal- Studying thecharge characteristics of faces andto modeltheirproperties. to analyze transition-metal oxide inter Germany, demonstrated method anew team, physicistsatWürzburg University, Vladimir Hinkov. Courtesy ofJ.E. Hamann-Borrero and ic fieldwouldform between thelayers. reconstruction, anenormouselectrostat charged atomic layers. Withoutelectronic a sequence ofpositivelyand negatively Film oflanthanumcobalt oxide shows Together withaninternational - - - -

11 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 - - nvlpubs.nist.gov/nistpubs/spe ours) depend on it. on depend ours) Fracture of a sapphire dome. Courtesy a sapphire of Fracture of NIST. quantitative fracture analysis. Addition analysis. fracture quantitative how see help readers studies case ally, While hard the guide is used in practice. upon request, the available are copies of charge free guide may be accessed online. cialpublications/NIST.SP.960-16e2.pdf. www.TiniusOlsen.com

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The first name in materials testing. materials in name first The The National Institute of Standards of Standards Institute The National tions of recent documentary standards, documentary standards, tions of recent tech on new microscopy material on chapter niques, and an expanded and Technology (NIST), Gaithersburg, Gaithersburg, (NIST), and Technology edition expanded new, a released Md., Practice Recommended of the NIST and of Ceramics Guide, “Fractography 960- Publication Special (NIST Glasses” in 2007, the guide issued 16e2). First and engineers help developedto was in patterns fracture scientists analyze consumer in used glasses and ceramics medical and building materials, goods, and implants. This edition, with devices which are of 1000 images—300 nearly than its predecessor new—is 15% larger such as descrip and includes updates NEW NIST GUIDE BREAKS GUIDE NEW NIST SCENE ONTO - com lossless such as in applications processors. memory puter ultrafast and www.uni-wuerzburg.de/en.

- - - terial to end product. To international standards and your toughest specifications. Reputations and (yours specifications. toughest your and international standards To product. to end terial Busted! program QA company’s This reputation AND Like Humpty Dumpty, it is hard to put the pieces back together once a real world product quality disaster strikes. The ultimateThe of cost strikes. disaster quality product world a real once together back pieces the to put hard is it Dumpty, Humpty Like place. first the in program far greater assurance a quality in any than investing or not savings corners from cutting far, be will a recall from quality assure you help can Olsen Tinius support, technical and software, machines, testing of physical spectrum broad our With ma Physicists applied the technique the technique applied Physicists to thin films of lanthanum cobalt cobalt of lanthanum thin films to and of positively sequence oxide—a layers, atomic charged negatively In these on a 15-nm-thin film. stacked fields enormous electrostatic materials, high this avoid To layers. between form rearranges nature cost, field energy process a either through the charges, smoothness— that preserves film face a reconstruction—or electronic called sur in a corrugated that results process on based devices which hinders face, especially when mate film interfaces, atomic on an change rial properties reflectometry x-ray The resonant scale. news the promising reveals method occurs reconstruction that electronic interfaces. oxide at transition-metal other be applied to could This method of these mate properties microscopic as the electronic rials as well—such and orbitals atomic of occupation their use to lead spin orientation—and 12 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 LEARNS MATERIALS MACHINE LEARNING microstructure research andmaterials testing underextreme conditions. research, theMDLisontrack to receive LEEDGold certification. The labwillhouse laboratory andoffice space, oflabspace including10,000sq.ft. for radiological between energy andmaterials scientists.Encompassing of roughly 115,000sq.ft. Energy Quad,agroup offour adjoiningbuildings designedto maximize collaboration Argonne National Laboratory, Ill.Thefacility Lemont, willcomplete Argonne’s Materials onthenew Construction isunderway DesignLaboratory (MDL)attheDOE’s BRIEF tries or research labs. “Big companies ically categorize visual data for indus was previously published,orautomat journal archives to determine if a photo ple, itcould beusedto search scientific try, publishing,andacademia. For exam- could findapplication inresearch, indus materials science. to thevast image libraries amassedin more data, are they especiallysuited designed to improve encounter asthey structures. Because thealgorithms are nize and categorize images of micro search users—to automatically recog- algorithms—familiar to Google image Professor Elizabeth Holmisusingthe visual data sets inmaterials science. to search, classify, sort, and identify that usesmachinelearning algorithms sity, Pittsburgh, asystem developed professor atCarnegie Mellon Univer images by hand,amaterials science on humanexperts to identifyresearch

Google-like algorithms are now beingusedto categorize micrographs. Holm’s machinelearning system In a field that hashistorically relied The new Materials Design LaboratoryThe new atArgonne NationalLaboratory broke ground inSeptember. EMERGING TECHNOLOGY - - - - -

PROVEN AFTERLONG STRETCH INSTABILITY PREDICTION theory experimentally—untiltheory now. The scientists hadbeenunableto prove the predicted thebehavior, butmaterials applied mathematicianRonald Rivlin ly deform into athin,flatplate. In1948, thick cubeofsoftmaterial willsudden- With therightamountoftensile force, a proves true: that adecades-old theory Mass., demonstrated for the first time Applied Sciences (SEAS),Cambridge, A. Paulson SchoolofEngineeringand facturing processes. cmu.edu. are mostappropriate for additive manu understand what types of raw materials powder micrographs inorder to better of experimental andsimulated metal and herteam are compiling adatabase is application inmetal 3Dprinting.Holm derstand theirproducts.” The next step wantthey to usethatdata to better un one wants to lookthrough those,but research images,” explains Holm.“No can have archives ofmore than600,000 Researchers attheHarvard John anl.gov. - -

harvard.edu. triggers to change theirgeometry.” between behaviors by usingsimple ate materials thatcan suddenlyswitch SEAS. “Withthisinstability, we can cre former graduateOvervelde, student at their functionality,” saysJohannesT.B. use instabilities to change orenhance space for architected new materials that andbecomingsymmetry suddenlyflat. ter deformed, breaking thegeometrical Under biaxialtension, thesample’s cen made of silicon rubber at each corner. stretchedthey soft elastomer a thick, deforming itinto aflatsurface. To doso, in acentimeters-thick elastomer block, Harvard team triggered this instability of Harvard SEAS. Courtesy andbecomingsymmetry flat. sample’s center deforms, breaking the Under biaxialtension, theelastomer “This research widensthedesign

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13 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 -

To suppress shear banding, banding, shear suppress To Shear band formation is a long-standing is a long-standing formation band Shear At manufacturing. in metals problem wavy as a left, the phenomenon appears right, a Top strip. in a titanium structure a shear across traced was “micromarker” right, (yellow). Bottom an electronband as a the band reveals image backscatter about dark region severely deformed, 4 µm thick. of Purdue. Courtesy resulting groove-like “micromarkers” “micromarkers” groove-like resulting deformations serrated large revealed liquid resemble that, surprisingly, to Turning an interface. past flowing used equations typically mathematical the team fluid flow, viscous analyze to in form bands shear that determined within just occurs phases. The first two of cutting when a microseconds a few in the metal. is created interface weak phase, gradual more second, the In interface slides along the weak metal shape. the wave producing then shears, added a wedge-shaped researchers channel the cutting tool, die opposite the machined metal ing the chip from - The die con tools. the two between deform it to forcing the metal, strains and eliminating the uniformly more sliding phase. purdue.edu. ------An international team led by led by team An international In CSP, water or acid is applied to is applied to or acid water In CSP, The University N.M., and The University Albuquerque, Sandia National Laboratories, collaborate to agreement research a master approved Ohio, Akron, of of Areas research. materials and advanced manufacturing on additive in coatings, of adhesion, friction, and wear include the roles interest nanotube-based as the use of as well and adhesives, lubricants, heat better and provide formation, inhibit ice drag, reduce to coatings of In addition, biomimicry in the context will be studied transfer. applications. engineering and biological for adhesives advanced uakron.edu. sandia.gov, researchers at Purdue University, West University, at Purdue researchers microscopic Ind., discovered Lafayette, banding of shear of the process details con to and developed a simple method trol the defect in metals manufacturing. manufacturing. metals in defect the trol the displacement studied team The etched was when metal created profiles The processed. then marks, tiny with SHEAR GENIUS densify some materials to over 95% of over to materials densify some minutes. density in 15 their theoretical to CSP used researchers example, For and thermoplastic ceramic co-sinter high density at to polymer composites 120°C in 15-60 minutes. sur particle causing powder, ceramic faces to partially dissolve and produce and produce dissolve partially to faces inter particle-particle at phase liquid a and pressure, With temperature faces. densify and to begin the solid particles the inter or ions leave of atoms clusters minimizes This aids diffusion, faces. - parti allows and energy, free surface is a pre The key together. pack cles to pressure, of moisture, cise combination the capture to heat, and time required crys fully so the material rates reaction and achieves very high density. tallizes - 50 unique com has verified The team for including formulas binations so far, and ceramic-nanopar ceramic-ceramic ceramic-metals, ticle composites, Applications and ceramic-polymers. include thermal insulation, biomedical components. implants, and electronic psu.edu. - - - PROCESS TECHNOLOGY PROCESS norsktitanium.com. this year. later ing facility Researchers at Penn State, Univer State, at Penn Researchers Artistic interpretation of cold sinter of cold Artistic interpretation ing of ceramic particles (white) and (white) particles ing of ceramic using low (green) polymer strands mol- added water evaporate to heat M. of Jennifer ecules (blue). Courtesy McCann/MRI. and Qualification Center will Center and Qualification incorporate Norsk’s “ultra lean lean “ultra Norsk’s incorporate for 3D printing, heat treatment, treatment, 3D printing, heat for line that turns CAD files into fin- CAD files into line that turns The Plattsburgh Demonstration Demonstration The Plattsburgh Norsk Titanium US Inc., Platts US Titanium Norsk machining in less than 40 hours. machining in less than 40 hours. nondestructive testing, and final testing, nondestructive burgh, N.Y., a subsidiary of Norsk N.Y., burgh, ished aerospace parts and allows and allows parts ished aerospace Norway, will open a AS, Norway, Titanium BRIEFS - and train 70,000-sq-ft production cell,” featuring a 120-ft production a 120-ft production featuring cell,” sity Park, Pa., developed a new method developed a new method Pa., sity Park, of previously compounds producing for also that could materials incompatible many types of for costs energy lower temperature The low manufacturing. process sintering cold called method, less energy uses significantly (CSP), can and methods, traditional than COLD SINTERING PROCESS COLD SINTERING PROCESS MIXES THINGS UP 14 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 COULD BEGAMECHANGER ENERGY STORAGE MODEL [email protected], www.cornell.edu. For more information: Hector Abruña, charge for atleast 10,000cycles. COF films, as well as stable charge-dis response compared withunmodified film exhibits a10-fold highercurrent conducting substrate. Theresulting COF pores oftheCOF, whichisgrown ona ically conducting polymer)withinthe phene) known asPEDOT (anelectron film ofpoly(3,4-ethylenedioxythio itation by electropolymerizing a thin awaydeveloped to overcome thislim to theirpoorconductivity. Thegroup tial for electrical energy storage due Conventional COFs have limited poten blocks withavariety ofapplications. be fashioned into lightweight building porous structures crystalline thatcan the bodyofcar itself. incorporatingand even thedevice into cess, extending single-charge range, tive by speedingupthecharging pro numerous industriessuch as automo ing polymerthinfilm—could benefit infused withan electronically conduct on acovalent organic framework (COF) storage device. Thetechnology—based up withapowerful electrical energy charge rate of supercapacitors to come batteries withthesuperiorcharge-dis the large energy-storage capacity of Ithaca, N.Y., away developed to combine

efficiently. framework (red andblue)works withtheframework to store energy rapidly and A conductive polymer(green) formed insidethesmallpores ofacovalent organic The research centers on COFs— A team from Cornell University, ENERGY TRENDS ------

PERSONALITIES METAL HAS MULTIPLE at work. Whilebothformsat work. ofdeposits there are two different mechanisms these depositsform, andreports that the mostdetailed analysisyet ofhow Cambridge, says it has carried out Massachusetts Institute ofTechnology, damage ordisablethebattery. formance and lead to shortcircuits that metal surface, whichcan hamperper fingerlike lithiumdepositsform onthe research Asbatteries effort: are charged, problem thathasstymiedmuchofthis But lithiuminthismetallic form hasa store withoutincreasing theirweight. amount ofenergy thatbatteries can leading contenders for improving the focusing onlithiummetal electrodes as mossy deposits. of ceramic material thatlimitsgrowth of images showtheeffect ofablockinglayer which grows from SEM thetips.At left, the needlelike dendritictype(bottom), (top), whichgrows from itsbase, and lithium deposits,thebulky, mossytype SEMimages showtwotypesof On right, Now, ateam ofresearchers at researchersBattery have been - IS JUST RIGHT FUEL CELLMEMBRANE [email protected], [email protected], For more information: MartinZ.Bazant, responsible for mostoftheproblems. ers say, are harder to deal withandare their tips. The dendritic type, research- ing “dendritic” projections grow onlyat The muchsparser andrapidly advanc roots andare relatively easy to control. which form at low rates, grow from their Clustered,current. “mossy”deposits, way grow they dependsontheapplied are composed oflithiumfilaments,the sandia.gov. commercial PEMfuel cell membranes. and lastthree timeslonger thanmost respond well to changes inhumidity, range oftemperatures from 176°-320°F, exhibit stable performance over awide ammonium-biphosphate ionpairs the Sandia-patented membrane. The ratory—combines phosphates with ated atLos AlamosNationalLabo ammonium ion-pair fuel cell—cre to Fujimoto andhiscolleagues. Their commercial products, accordingble three timeslonger thancompara- over awidetemperature range, lasts says chemistCy Fujimoto. querque, N.M.,seemsto work justright, Sandia NationalLaboratories, Albu- polyphenyline membrane patented by cold to bemaximally effective. Now a at temperatures eithertoo hot or too in automobile fuel cells often work out pollutants. However, membranes Montoya. fuel cell membranes. Courtesy ofRandy demonstrate theclarityof theirnew Cy Fujimoto, andMichaelHibbs right, The membrane, whichoperates Fuel cells provide power with-

- - - 15 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

------To create the brushes, a substrate the brushes, a substrate create To The stop-flow photopatterning method photopatterning The stop-flow polymer brush patterns. enables intricate of Christian Pester. Courtesy izing and engineering surfaces with pat with surfaces engineering and izing polymer brushes. terned deposited) (with initiating molecules and a cell is enclosed in a stop-flow with in. Irradiation solution streamed A the reaction. then initiate light can is positioned over photomask separate some only allowing of the cell, the top Next, the light is growth. light-activated solution is drained first the off, turned one is and a second the cell, from the polymers. functionalize in to flowed neither the mask nor the sub Because only the mole moved, has been strate light to been exposed have that cules These functionalized. and grown are with varia may be repeated steps basic sub light source, tions in the reactants, create to photomask or positions, strate - in a single con polymer brush patterns information: more For tinuous process. [email protected], Christian Pester, www.ucsb.edu. features a new platform for functional for a new platform features - - - - -

At the University of California, the University At Scientists at ANU developed a new spray- of Courtesy material. on, water-repellant Hay/ANU. Stuart Santa Barbara, researchers are looking are researchers Barbara, Santa cre brush on polymer improve greatly to ation with a method of micron-scale sur of micron-scale ation with a method that not only patterning chemical face moneyand time the spent decreases also adds versa but in manufacturing, called designs. Their method, tility to photopatterning,” “sequential stop-flow CREATING POLYMER BRUSHES BRUSHES POLYMER CREATING FOR ENGINEERED SURFACES forming on airplanes, and protect boat boat on airplanes, and protect forming com The team corroding. hulls from bined two plastics, one tough and one plastics, one tough bined two fishing interwoven two like “It’s flexible. says materials,” made of different nets, William Wong. The super Ph.D. student is also transparent coating hydrophobic ultraviolet to resistant and extremely www.anu.edu.au. radiation.

------SURFACE ENGINEERING SURFACE innovative process for depositing super thin films. Courtesy of University of of University thin films. Courtesy depositing super for process innovative Boulder. Colorado Gallium nitride film is deposited on silicon substrate at 27°C (80°F) using an at substrate on silicon deposited Gallium nitride film is Scientists at The Australian Scientists at The Australian Researchers at the University of at the University Researchers as elec is known The new method National University (ANU) developed a National University with a remark material new spray-on The coating water. repel able ability to waterproof used to be eventually could from ice mobile phones, prevent tron-enhanced atomic layer deposition layer atomic tron-enhanced developed as part recently and was of Materials Control Local of DARPA’s demon The team Synthesis program. deposition room-temperature strated as nitride as well and gallium of silicon specific etch controllably the ability to spatial precise to leading materials, in 3D. colorado.edu. control Colorado Boulder developed a new Colorado ma synthesizing ultrathin for approach break temperature—a at room terials that industrial approaches over through of 800°C or more. temperatures require a creating to opens a path advance The thin-film unattainable host of previously by whose production microelectronics, has been impos methods conventional lose many components sible because when subjected functions their critical high temperatures. to SPRAY-ON WATER PROOFING PROOFING WATER SPRAY-ON ROOM-TEMPERATURE ATOMIC ATOMIC ROOM-TEMPERATURE DEPOSITION LAYER 16 MATERIALS TESTING/CHARACTERIZATION MATERIALS CORRELATIVE MICROSCOPY OF NEUTRON-IRRADIATED MATERIALS

Development of new, radiation-tolerant materials that maintain the structural integrity and safety margins over the course of a nuclear power reactor’s service life requires the ability to predict degradation phenomena.

Samuel A. Briggs* and Kumar Sridharan, FASM,* University of Wisconsin, Madison

Kevin G. Field, Oak Ridge National Laboratory, Tenn.

*Member of ASM International 17 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

. ------[2] , but [3]

C. Though the ° r-Al e-C . An understanding . An understanding [4] Fe-Cr-Al alloys are being consid are alloys Fe-Cr-Al Some examples of radiation- Some examples are susceptible to radiation-induced radiation-induced to susceptible are and embrittlement due to Cr-rich of nanoscale the precipitation at tem particles αʹ phase precipitate 475 below peratures ered as a possible replacement for for as a possible replacement ered cur cladding materials fuel Zr-based for LWRs used in commercial rently and enhanc margins safety increasing of the as part tolerance ing accident Campaign Fuels Advanced DOE’s kinetics for formation of this phase at phase this of formation for kinetics LWR-relevant temperatures are slow, slow, are temperatures LWR-relevant be to has been shown this process - radi neutron-induced by accelerated ation damage Similar to other high-Cr ferritic alloys, alloys, other high-Cr ferritic Similar to high tem excellent have alloys Fe-Cr-Al and radia aqueous corrosion perature resistance swelling tion-induced of how the formation of this phase is the formation of how the and how composition by affected with evolves microstructure precipitate to is essential in order dose radiation in the embrittlement response mitigate CHARACTERIZATION OF CHARACTERIZATION F IRRADIATED analysis and allows for multiple TEM TEM multiple for and allows analysis from be prepared specimens to and APT extremely sample, it is a single bulk scientific and maximizing the for useful of a single bulk irradi value monetary sample. ated being defects microstructural induced include using these techniques studied bubbles, gas cavities, loops, dislocation Charac and precipitates. segregation, features these nanoscale of terization microscopy advanced necessitates that often equipment and techniques when considerations special require or analysis collection data performing This article materials. radioactive for use of these advanced the illustrates precipitates characterize to techniques at alloys Fe-Cr-Al in neutron-irradiated utilized extensively ORNL, which have reactors research the aforementioned lab characterization and user facility the techniques However, oratories. extended be readily can described here as well. other materials to ------. [1] An important tool within these within tool important An Fortunately, modern PIE exper Fortunately, active bulk specimen can be reduced be reduced bulk specimen can active that it no lon volume such a minute to risk. exposure poses a significant ger have As even a single bulk sample can irradia after cost associated significant the HFIR, extracting like tion in a reactor from information amount of maximum As these samples is crucially important. site-specific targeted, produce can FIB terization laboratories is the focused is the focused laboratories terization spec prepare to used (FIB), beam ion probe both TEM and atom imens for characterization. (APT) tomography FIB tech through Sample preparation impactful niques has been particularly materials with radioactive in working smaller working the significantly due to increased to leading sample volumes individual from scientific yield gained performed carefully Using experiments. a highly radio techniques, FIB lift-out user facilities and radiological charac and radiological user facilities iments can make use of specialized use of specialized make iments can and dedicated reactors high-flux test to in order facilities characterization The some of these issues. circumvent at Idaho (ATR) Reactor Test Advanced (INL) and the High National Laboratory Oak at (HFIR) Reactor Isotope Flux (ORNL) are Laboratory National Ridge nuclear specialized of two examples of capable in the U.S. designs reactor structures damage inducing neutron to compared rates at much greater to access Further, LWRs. commercial character radiation-friendly dedicated, through available laboratories ization Sci the Nuclear such as facilities user atrnsuf.inl. (NSUF, Facilities User ence and per the resources provide can gov) limit occupational to sonnel necessary of the spread and prevent exposure contamination. radioactive mens. Although these methods provide provide these methods Although mens. irradi a material’s insight into valuable not completely they are ation response, in the differences due to predictive particles charged mechanism in which the crys to energy impart and neutrons structure tal use high-energy ion beam accelerators accelerators beam ion use high-energy dam- neutron emulate to in attempts rate faster at a much processes age in speci radioactivity without inducing ------

- incredi an is core reactor nuclear that environment bly demanding chal unique several presents

Historically, performing the neu- performing Historically, A lenges for materials performance. Mate performance. materials for lenges (LWR) reactor light water rials in modern in decades survive must several cores (300-350°C) aqueous high-temperature while being subject conditions corrosion neu amounts of high-energy large to reactor Next-generation irradiation. tron cool corrosive use more designs seek to salts) and even greater ants (e.g., molten doses. The neutron and temperatures and uniquehigh amounts of disorder micro and defects crystallographic by induced effects segregation chemical deg property to lead inevitably radiation struc Maintaining of materials. radation over margins and safety integrity tural thus life service of the reactor’s the course and understand the ability to necessitates phenomena in these degradation predict radiation-tolerant developnew, to order required the maintain can that materials conditions. in these extreme performance characterization damage radiation tron tolerance assess radiation to necessary primary two has faced and performance undue First, preventing challenges. and contamination exposure radiation absorption as neutron is problematic, isotopes radioactive generate to tends materi make which can in a material, without spe als handling hazardous As equipment and facilities. cialized sample preparation such, the required (PIE) examination post-irradiation for in shielded be performed needs to often that functions to and is limited hot cells Practically therein. performed be can access precludes this often speaking, character microstructural advanced to elec such as transmission tools ization (TEMs) and makes microscopes tron procedures characterization even basic neutron Second, costly. much more have typically experiments irradiation achievingas time, turnaround long a end- produce to necessary doses the and mechanical microstructure of-life that requires in a material properties in a commercial specimens be exposed a length of time equiva for core reactor As lifetime. service the expected lent to in this field often a result, researchers 18 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 at atarget temperature of320 13.8 displacements peratom (dpa) various nominal damage doses up to TABLE 2— *S, O,N,andPcontents atorbelow 10ppm. INVESTIGATED INTHISRESEARCH TABLE 1 specimens machined into SS-J2 sub-sized tensile shown inTable 1.Thesematerials were emission spectroscopy (ICP-OES), are inductively coupled plasmaoptical Alloy compositions, asdetermined by from 10-18wt%Crand2.9-4.8Al. with nominalcompositions ranging formed onfour Fe-Cr-Al modelalloys and PIEanalysisstudies were per for LWR claddingapplications. designing anuclear-grade Fe-Cr-Al alloy using room temperature andelevated ment oftensile behaviorwas performed ditions are shown inTable 2. lifetime. Details offinalirradiation con- end of the typical LWR fuel cladding properties andmicrostructure atthe reasonable approximation ofmaterial condition are expected to provide a rial. Thespecimensinthe13.8dpa of incidentparticles for agiven mate on thefluence andenergy spectrum getic particles. Dpa iscalculated based lattice site for agiven fluence ofener of timesanatom isdisplaced from a and is defined as the average number commonly describesradiation damage time ofapproximately 4900hrs. Dpa responding to amaximumexposure Capsule ID Fe-18Cr-2.9Al Fe-15Cr-3.9Al Fe-12Cr-4.2Al Fe-10Cr-4.8Al FCAY-03 FCAY-02 FCAY-04 FCAY-01 FCAY-05 To this end, neutron irradiation Following irradiation, anassess Alloy — [5] F SUMMARY OFF e andirradiated inHFIRto -C r -A l MODELALLOY COMPOSITIONS Exposure (hours) wt% wt% wt% wt% time 2456 4914 614 301 120 e -C r bal. bal. bal. bal. ° Fe -A C, cor l ALLOY CAPSULE IRRADIATION CONDITIONS Neutron flux E >0.1MeV - - - - - 17.51 15.03 11.96 10.01 8.74 ×10 8.84 ×10 8.54 ×10 8.74 ×10 8.54 ×10 (n/cm Cr (b) (a) and 13.8dpa (near end-of-life) conditions. 320°C after irradiation demonstrated of-life doses.Tensile tests performed at transgranular cleavage fracture atend- early-life dosestransitioning to brittle, ical dimpleductilefracture at observed men failure mode (Fig. 1a-b), with typ demonstrate clear differences inspeci- lowing room temperature tensile tests dose condition oftheFe-18Cr-2.9Al fol- ORNL. Fractographs for alow- andhigh- and Testing (IMET)HotCellFacility at at theIrradiated Materials Examination (SEM) fracture surface analysisin-cell sequent scanning electron microscopy temperature tensile testing withsub Fig. 1— 2 s) 14 14 14 14 14 2.93 3.92 4.22 4.78 Al

Comparison offracture surfaces for Fe-18Cr-2.9Al alloyirradiated to 1.8dpa (early life) 0.017 0.035 0.027 0.038 Y Neutron fluence E >0.1MeV 9.25 ×10 3.69 ×10 1.95 ×10 1.55 ×10 7.73 ×10 (n/cm 0.005 0.005 0.005 0.005 C 2 ) 20 21 20 21 22 <0.01 <0.01 0.01 0.01 Si Dose rate - - 7.7 ×10 8.1 ×10 7.7 ×10 7.9 ×10 7.8 ×10 (dps/s) (d) (c) here (volume ~8mm unpaired electrons. Bulksamples used nuclei orwiththemagnetic momentof tically scattered by interactions with an incidentbeam ofneutrons iselas structive analysistechnique inwhich the microstructure. SANSisanonde analysis ofnanoscale αʹprecipitates in beamline atORNL for diffraction-based small-angle neutron scattering (SANS) and shippedto thegeneral purpose pared, packaged for on-road shipping, each material condition were thenpre conditions studied (Fig.1c-d). ductile failure mechanismsinalldose detector configurations. Anexample of at room temperature atthree different sional diffractograms were collected ratio in the SANS data. Two dimen maintain anadequate signal-to-noise and allow for sufficientscattering to fit the4-mm-diameter aperture sizes specimens are necessary inorder to minimize userinteraction. Theselarger is taken duringSANSinvestigations to cant radiological threat, sospecial care -7 -7 -7 -7 -7 Broken half-tensile heads from (dpa) Dose 13.8 0.8 0.3 1.8 7.0 temperature 3 340.5 ±25.7 319.9 ±12.7 Irradiation 355.1 ±3.4 334.5 ±0.6 381.9 ±5.4 ) poseasignifi (°C) - - - - - 19 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

, - - - [8] Fig. 4. APT results results APT 4. Fig. on a single APT microtip cou microtip on a single APT 3 μm pon) promotes ease of handling when ease pon) promotes A repre at these laboratories. working of a Fe-15Cr- reconstruction sentative at dpa 7 to specimen irradiated 3.9Al in shown is 320°C to appear additions Al that reveal of precipitates the Cr content reduce binary to alloys Fe-Cr when compared Atom probe reconstruction reconstruction probe Fig. 4 — Atom Fe- in microstructure showing precipitate at 320°C. 7 dpa to irradiated alloy, 15Cr-3.9Al displayed using 34 at.% are Cr Precipitates (purple) with 2% isosurfaces concentration (black). shown atoms matrix Fe of total and the observed precipitate morphol and the observed precipitate with those in agreement are trends ogy the validating seen in the SANS study, but the significant volume reduction reduction volume but the significant (< 100

------C. ° were [7] APT investigations allowed for an for allowed investigations APT ning transmission electron microscopy microscopy electron ning transmission of examples investigations, (STEM) in Fig. 3. shown which are and morphology composition cipitate within a very analysis volume. small using performed was collection Data Elec Instruments Local the Cameca (LEAP) 4000X HR at Probe Atom trode Nanophase Mate for either the Center (CNMS) at ORNL or at the rials Sciences Studies Energy Advanced for Center capa are (CAES) at INL. Both facilities samples, ble of handling radiological then used to prepare microtip needles microtip prepare then used to scan and lamellae for analyses APT for of individual pre study atomic-scale personal protective equipment (PPE) protective personal specimens Polished and dosimetry. remotely- a in installed then were FIB Dual-Beam 3D Quanta FEI operated in room that is housed in a lead-lined radiation from shield personnel to order FIB equipment of Operators exposure. handle the radio to specially trained are on is placed samples and a focus logical minimize to practices efficient loading specimens. the radioactive to exposure techniques lift-out Standard (b)

(b) ------°C . Much less material is . Much less material [6] Fig. 2a, in which the precip (a) Raw SANS diffractogram for Fe-18Cr-2.9Al alloy, irradiated to 13.8 dpa at 341 to 13.8 dpa irradiated alloy, Fe-18Cr-2.9Al for SANS diffractogram (a) Raw Sections from the remaining the remaining Sections from a diffractogram for the Fe-18Cr-2.9Al the Fe-18Cr-2.9Al for a diffractogram at 340 13.8 dpa to specimen irradiated (a) analysis, (a) APT for specimens prepared Fe-Cr-Al of representative Fig. 3 — SEM micrographs analysis. and (b) TEM and STEM in is shown red-orange a as manifests signal itate zero- central the around ring contrast reduction Radial (black contrast). beam one-dimen to of these diffractograms sional curves models analytical allows which bulk- from the data, be fit to to infor morphology precipitate averaged (Fig. 2b). be extracted mation can the specimens opposite half-tensile cut using a low- neck were strained and shipped speed saw in the hot cells Devel Materials Activation the Low to facility Analysis (LAMDA) opment & FIB sample preparation. at ORNL for designed facility is a specialized LAMDA of characterization state-of-the-art for and metal fuel threat low-radiological lic specimens (a) Fig. 2 — (b) Final SANS scattering intensity curve, combining data from three distinct detector config distinct detector three from data curve, intensity combining (b) Final SANS scattering the data. model to fit of analytical example and urations, required for FIB sample preparation FIB sample preparation for required and subsequent analyses compared reduction SANS, and the volume to allow sufficient to was in the hot cell speci hand polishing of out-of-cell for - metal standard using LAMDA in mens with appropriate techniques lographic 20 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 tion looporotherdefect sites. bulk material, withnobiasfor disloca- appear to nucleate homogenously inthe ure 5demonstrates that of EDSspectra inthesematerials. Fig Cr-K Fig. 5—(a)Colored STEM-ADF image, acquired onthe[111]zone axis.(b)STEM/EDS mapfor (a) niques sensitive electron microscopy tech- necessitating theuseofchemically the Cr-rich precipitates in this system, techniques are notuseful for studying tional diffraction contrast-based TEM particles in an such asVandMn,are alsoidentified. responding to transmutation products, uent elements. In addition, peaks cor natural isotopic abundances ofconstit that are inconsistent withexpected spectrum asmanifested by peak ratios inthegeneratedobserved time-of-flight resulting from neutron absorptionare sis. Artifacts ofnuclear transmutation models usedinthescattering analy irradiated to 7.0dpa at320°C. of dislocation loops axis, allowing for simultaneous imaging dark field(ADF)images onthe[111]zone collected concurrently withannular disc specimens.Thex-ray mapswere specimens over more traditional 3mm significantly reduced withFIB prepared x-rayobserved spectrum;thiseffect is teristic x-rays, potentially muddlingthe easily detected along with the charac decay from irradiated samplescan be as theenergetic emissionsofradioactive be taken when performing data analysis oftheFEITalosciency system, care must the LAMDA facility. Dueto thehigheffi the FEITalos F200XS/TEMlocated in EDS data collection was performed on the precipitate microstructure. STEM/ with STEM to acquire spectral images of x-ray spectroscopy (EDS)was coupled α x-rays. (c)Coloroverlay ofADFimage and EDSmap. All images from theFe-18Cr-2.9Al alloy Due to thesemi-coherency of [9] . Assuch,energy dispersive α- matrix, conven- [10] andcollection α ʹ precipitates (b) αʹ ------MATERIALS RESEARCH THE FUTUREOFNUCLEAR other in-core components. tured materials isbeingexplored for strengthened (ODS)andnanostruc radiation tolerance ofoxide-dispersion 60 to 80years. Additionally, improved mercial LWR operating licenses from investigation inorder to extend com- vessel (RPV)materials are alsounder that mayembrittlereactor pressure nologies. Late-blooming phases(LBP) particle fuel for gas-cooled reactor tech ding material and for advanced TRISO tigated bothasanalternative LWR clad example, SiC is being extensively inves fordeveloped nuclear applications. For many material systems currently being material inthenear future. a nuclear-grade Fe-Cr-Al LWR cladding erance withthegoal ofrecommending ment additionsonalloy radiation tol study the effect ofminor alloying ele undergoing irradiation inHFIRto tions based onthiswork are currently alloys withdown-selected composi Generation IIFe-Cr-Al engineering DOE’s Advanced Fuels Campaign. alloy program development ofthe design decisionswithintheFe-Cr-Al cipitation inthissystem hasinformed mechanisms anddependenciesofpre resulting detailed analysis of the ant nuclear fuels applications. The Fe-Cr-Al alloys for accident-toler precipitation inneutron-irradiated alloys, asdemonstrated for of nanoscale precipitation in events in-depth, multifaceted investigation acterization capabilities allow for an Fe-Cr-Al alloys are justoneof Modern nuclear materials char (c) α ʹ phase ------ACKNOWLEDGMENTS nuclear applications. informed materials for development pated to playacentral role inenabling nuclear materials researchers is antici to ampleaccess to thisequipmentby techniques andequipmentinaddition adoption ofadvanced characterization tion effects in materials. The continued terization research onnanoscale radia greatly facilitated high-qualitycharac zation capabilities discussedhere have tion andTesting (IMET)hotcell facility, the CAES,Irradiated Materials Examina- the authors acknowledge the staff of diation capsule designefforts. Finally, ysis, andR.H.Howard for leading irra the materials for irradiation andanal thank Y.they Yamamoto for providing Inaddition, niques usedinthiswork. assistance analysistech indeveloping P.D. EdmondsonandK.C.Littrell for versity Programs. Nuclear Energy’s Nuclear Energy Uni was provided by theDOEOffice of the NSUF. Aportionoffunding for SAB Energy, Fuel Cycle R&D Program and provided by the DOE, Office of Nuclear TheFEI Talosexperiment. F200X TEM is DE-AC07-051D14517 aspart ofaNSUF DOE IdahoOperations Office Contract the DOEOffice ofNuclear Energy under portion of this work was supported by MaCS Laboratory at the CAES at INL. A Office ofScience User Facility andthe conducted attheCNMS,whichisaDOE of BasicEnergy Sciences, DOE.APT was Scientific User Facilities Division, Office HFIR userfacility was sponsored by the irradiation of Fe-Cr-Al alloys at ORNL’s the Fuel Cycle R&DProgram. Neutron Energy, Advanced Fuels Campaign of sponsored by DOE’s Office ofNuclear performance. Themoderncharacteri- demanding environments for materials eration reactor more designswitheven enabling theconstruction ofnext-gen mercial LWR technologies inadditionto taining andimproving theexisting com nuclear fuels is critical for both main ation-tolerant alloys, ceramics, and nology robust anddeveloping radi The authors would like to thank researchPrimary funding was Advancing nuclear materials tech ------21 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 - - , Vol 107, No. 2007, p 761-766, 2007. 2007, p 761-766, No. 107, , Vol TRUST Instron

7. M.K. Miller and K.F. Russell, Atom Russell, Atom K.F. Miller and 7. M.K. with a Preparation Specimen Probe Ultramicros SEM/FIB Miller, Dual Beam copy - al., Irradia et Edmondson, 8. P.D. in α’ Precipitation tion-Enhanced , Mater. Scr. Alloys, Model FeCrAl 116, p 112-116, 2016. Vol Ori- Ribis and S. Lozano-Perez, 9. J. and Interface Relationships entation Embed- of α-Cr Nanoclusters Structure α-α’ Demixing Matrix After ded in α-Fe Oxide Dispersion Irradiated in Neutron , Lett. Mater. Material, Strengthened 74, p 143-146, 2012. Vol of al., Application et 10. C.M. Parish, Investigat for Characterization STEM Fe-based in BCC effects ing Radiation 9, 30, No. , Vol Res. Mater. J. Alloys, p 1246-1274, 2015. … - ed-Materials Microscopy at Oak Microscopy ed-Materials Microsc. Laboratory, National Ridge 21, p 1003-1004, , Vol Microanal. 2015. , Vol 448, No. 1-3, p 374-379, 1-3, p 374-379, 448, No. , Vol Mater. 2014. - Development3. E.A. Little, of Radia Advanced for Materials tion Resistant - Tech Sci. Plant,Mater. Power Nuclear 5, p 491-518, 2006. No. 22, nol., Vol - SANS Investi al., A et 4. M.H. Mathon, α-α′ of the Irradiation-Enhanced gation - in 7–12 Cr Martensi Phases Separation 312, , Vol Nucl. Mater. J. tic , 2003. 2-3, p 236-248, No. Tolerance al., Radiation 5. K.G. Field, et Model Fe-Cr-Al of Neutron-Irradiated 465, , Vol Nucl. Mater. J. Alloys, p 746-755, 2015. Irradiat al., LAMDA: et 6. C.M. Parish, - - designs and manufactures systems used extensively by the biomedical industry biomedical the the meet by to extensively used systems and manufactures designs 825 University Avenue, Norwood, MA 02062 | 1.800.564.8378 | go.instron.com/bio Norwood, MA 02062 | 1.800.564.8378 Avenue, 825 University ® Samuel A. Samuel Founded in 1946, Instron in 1946, Founded growing requirement for full evaluation of materials from concept to finished product. Applications range from testing testing range from Applications finished product. to concept from materials of full evaluation for requirement growing wire. plastics and nitinol medical-grade using devices testing to tissues, and bio-engineered as human such biomaterials, When Materials Performance is Critical When Materials Performance LAMDA, and GP-SANS facilities in addi in facilities GP-SANS and LAMDA, - and Irra Thermal Hydraulics the tion to at (THIEG) Group diation Engineering their support.ORNL for ~AM&P information: more For Uni- assistant, research Briggs, graduate is on permanent of Wisconsin, versity and may be reached assignment at ORNL or 503.302.4439. at [email protected] References Allen, Intercompar and T.R. 1. G.S. Was Under Evolution ison of Microchemical Irradiation, of Particle Types Various 205, p 332-338, 1993. , Vol Nucl. Mater. J. Tolerant al., Accident Zinkle, et 2. S.J. Nucl. J. A Perspective, LWRs: for Fuels 22 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 L *Member ofASMInternational high-resolution images can beobtained image stitching capabilities, large-area ponents. Withanautomated stage and option for imaging materials and com- This makes lasermicroscopy afaster out additionalsurface preparation. to 28,000×)are possibleinairwith tion images (withmagnifications up compared to SEMisthathighresolu A key advantage oflasermicroscopy opticalbeyond microscopy isrequired. (SEM) istypically usedwhenresolution measuring device (Fig.2). without theneedto properly place a measure surfaces on an entire area data. Thelaseralsomakes iteasier to stylus, whichprovides more accurate beam diameter ismuchsmallerthana because itisnon-contact andthelaser used on soft and hard materials alike or quantified.Alasermicroscope can be than thestylustipcannot bemeasured Additionally, surface changes smaller damage, particularly for softmaterials. ditional contact methods risksurface characterization. ing to opportunities new for materials tion andlarge area mapping,are lead along withthepossibilityofhighresolu ety ofmaterials andcomponents. This, ness andfilmthicknessdata onavari- resolution to measure surface rough Jonathan Tedesco andAndrew Szafarczyk, Keyence Corp., Itasca, Ill. John Shingledecker,* andDanielPurdy,* JohnSiefert, ElectricPower Research Institute, Charlotte, N.C. alloys andcoatings inpower generation applications. 3D lasermicroscopy isopeningnew areas ofstudy for metallic MICROSCOPY SCANNING CONFOCAL ADVANTAGES OF3DLASER nanometer profile level (depth) copy (Fig.1)provides non-contact, aser scanning confocal micros Scanning electron microscopy To measure surface profiles, tra ------wafer roughness, andfilmthickness ments andfailure investigations, silicon lens characterization, MEMsmeasure range ofapplications inCCD micro chemical industriesincluding awide suited for and theelectronics industry non-contact mannerisparticularly well depth and soft/optical materials in a ety ofindustries.Theabilityto measure which isnotpossiblewithaSEM. associated 3Ddepthinformation, while retaining spatial distances and Fig. 1— Laser microscopy is used in a vari- Keyence VK-X lasermicroscope. - - ment inrecent years. for materials inpower generation equip expanded characterization applications butes ofthelasermicroscope have ledto roughness. Inaddition,theuniqueattri als characterization, specifically surface microscopy isalsowidelyusedfor met rials suchasglasses and lenses. Laser characterization oftransparent mate CASE STUDIES Institute’s (EPRI)laboratories inChar At theElectric Power Research - - - - - 23 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 - - - - - Internal and external oxidation oxidation and external Internal evi - are bands slip Furthermore, for ~24,500 hours. Using careful sample careful Using ~24,500 hours. for a final ~20 hour including preparation optical the step, polishing vibratory pro was scale of the ID oxide image 3a. in Fig. duced evi- is clearly of nodules in the form about little information dent.However, morphology oxide and structure grain under to is critical which revealed, is Chemical behavior. material standing such evaluate be used to could etching this shows experience but features, scales. in the oxide artifacts to leads the same as-polishedUsing sample and and area large the laser microscope, were images high-resolution area small charac including detailed obtained 3b Figure of nodule regions. terization 2000×. at approximately results shows On the as-polished the grain material, is observed. of steel structure as the original SP process dent from of multiple oxide evidence as clear well form morphologies and voids scale sur oxide ing at the inner and outer Figs. 3a and 3b clearly Comparing face. offers that the laser microscope shows detailed possibilities for enhanced without of materials understanding which can etching, surface the need for to lead and potentially scales damage results. erroneous - . To improve under improve . To [1] Inner diameter (ID) shot-peening (ID) shot-peening Inner diameter (SP) of austenitic stainless steel boiler steel stainless (SP) of austenitic has been used (SH) tubing superheater (<10,000 hour) short-term manage to and exfoliation oxidation steam-side in utility boilers standing of long-term behavior of this of long-term standing SH SP-304H EPRI received technique, in a utility boiler exposure after tubing Unetched (as-polished) laser image of the inner diameter surface of a shot-peened of a shot-peened surface of the inner diameter (as-polished) laser image Fig. 3b — Unetched of service. ~24,500 hours after tube superheater steel 304 H stainless ------Optical image of steam-side scale. of steam-side image Optical Comparison between contact profiler and laser microscope. and profiler contact between Comparison Fig. 3a — lotte, N.C., a Keyence VK-X160K has VK-X160K N.C., a Keyence lotte, re and in some cases augmented, Fig. 2 — characterization alloy metallic placed, done using either opti traditionally electron or scanning microscopy cal red a uses VK-X160K The microscopy. laser (658 nm wave semiconductor (depth) length) with maximum z-axis of 5 nm, maximum display resolution of 19,200×, and motor magnification of 100 × 100 with a range stage x-y ized show ability to mm. The microscope’s de relief, in surface subtle differences met area large high-resolution velop maps, and quantify surfaces allurgical has profilometry non-contact through opened up new in research. avenues 24 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 test coupon. Fig. 4— wear resistant coatings/claddings for valves after high-temperature laboratory wear testing. HARDFACING ALLOYS LASER MICROSCOPY FOR Fig. 5— cal for providing materials comparisons how thisdamage accumulates iscriti components. Characterizing therate of these interactions damage one or both tions between two bodies.Ingeneral, Tribology isthescience ofinterac Highresolution 3D color heightmapusedto characterize ahigh-temperature erosion Quantifiabledifferences inhigh temperature wear behaviorofpotential high-temperature - - mation above traditional and beyond microscope can quickly provide infor tribological examinations isthatthe erosion resistance. alternative materials andcoatings for alloys for high-temperature valves and has been studying advanced hardfacing under expected service conditions. EPRI The valueThe oflasermicroscopy in - face textures suchasadhesion. total aswell asvarious volume lost, sur mum andaverage depthofdamage and ples oftheseparameters includemaxi parameters to bedetermined. Exam and enablevaluable andquantifiable topography mapoftheentire specimen scope can rapidly provide adetailed 3D of damage. Alternatively, alasermicro vides alinear profile ormaximumdepth provide asingle2Dtrace, whichpro profilometry techniques thatgenerally dard high-temperature erosion test stan port of of the development ASTM G211 quantify the above parameters in sup ning vialasermicroscopy was usedto DAMAGE EVALUATING EROSION in quantifiableterms optical comparisons can beexplained rent ASTM standards that onlyrely on these techniques hasshown thatcur differences. Infact, research using can beusedto reliably quantifythese maps produced from laser microscopy the sametest conditions. The3Dheight significant gouging andadhesionunder experimental GTAW cobalt alloy shows tent low wear rate whiletheStellite 728 HVOF spray coating shows a consis Fig. 5.Here, theDiamalloy 4060NS behave differently asillustrated in eration, various hardfacing materials wear for advanced power cycle gen- sion rates by more than20%. under oroverestimate actual metal ero found thattraditional 2Dmethods can laser images and2Dcontact methods this case, comparisons between the3D bations forming aseriesofripples.In sample in Fig. 4shows surface pertur ment’s inconsistencies. Analysisofthe material orrelated to thetest equip relevant to thesuccess orfailure ofa topographical features thatmaybe from lasermicroscopy can illuminate entrapped inthesteam system. In the pipes occasionally exfoliate andare high-temperature boilertubes and appearing on the inside surfaces of lenge to utilities.Steam-grown oxides valve stems presents a reliability chal- [2] In solidparticle erosion, 3Dscan In elevated temperature sliding Erosion damage insteam turbine . In addition, the level ofdetail. Inaddition,thelevel [3] . ------

25 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 - 6.2 2.6 2.4 all depth Average Average of erosion of ver r

2 ISO 17025 ters ) Ove 30 models to co common tests major test systems Laser extensometers (3 to 250+ mm) 1% to 2000% strain 0.125 to 10+ inches from -265 to 1600°C Compatible with all Measuring ranges from Gauge lengths from Temperature ranges 307 733-8360 Jackson, WY 83001 USA 3975 South Highway 89 www.epsilontech.com 3 • • • • 2.4 259 618 (mm per 100 mm Eroded volume volume Eroded me ) 3 so 1.6 194 303 (mm Eroded Eroded volume volume Strain measurement for materials testing Nanostructured coating after service after coating Nanostructured ten ) 2 75 49 Area Area (mm measured measured Ex 2013.15 AMP Dir b&w ad_2002.02 ad 1/2/14 10:41 AM Page 1 2013.15 AMP Dir b&w ad_2002.02 ad 1/2/14 - - - Laser microscope measurements on large steam turbine valve stems after service com service after stems valve turbine steam on large measurements Laser microscope Vol 320, p Vol Wear, Stem with 30 micron with 30 micron Stem thick nanocoating in erosion Improvement coating due to resistance Old stem (no coating) Old stem national, p 821-831, 2014. J.S. Swaminathan, 2. V.P. Gandy, Smith, and D.W. Solid High-Temperature Testing Erosion Particle Advanced for Standard Plant Materials Power Advances and Coatings, Technology in Materials Plants, Power Fossil for the from Proceedings Seventh International Oct. 22-25, Conference, Hawaii. 2013, Waikoloa, ASM Inter Published by national, 2014. and S. Babu, Siefert 3. J. - Observa Experimental in Spec tions of Wear ASTM to imens Tested G98, Fig. 6 — the from Proceedings Seventh International Oct. 22-25, Conference, Hawaii. 2013, Waikoloa, ASM Inter Published by 111-119, 2014. paring performance of uncoated and coated stems after nominally equivalent operating history. operating nominally equivalent after stems and coated of uncoated performance paring Uncoated stem after service after stem Uncoated ------μm thick, nanostruc 3D laser microscopy is opening new 3D laser microscopy Figure 6 compares two valve stems stems valve two 6 compares Figure areas of study for metallic alloys and alloys metallic for of study areas applica generation in power coatings being currently are studies tions. Further distri- void quantify creep to conducted samples and ser creep butions in large on unetched components vice-exposed charac deformation samples, examine includ of small sample tests teristics of and location of size ing identification models accurate more build to cracking - hard and examine behavior, of material depth measure accurately ness indents to The rapid, profiles. in surface and changes quantifica and high resolution accurate, combination a unique is materials of tion in other be exploited that is hoped to and or augment optical replace to areas and elimi microscopy electron scanning sur contact 2D surface the need for nate ~AM&P profilometry. face John Shingle information: more For cross manager, is senior program decker Electric Power technologies, sector 420 Hillview Ave., Institute, Research CA 94304, 704.595.2619, jshin Alto, Palo www.epri.com. [email protected], References al., Managing Oxide et 1. A.S. Sabau, with TP347H in Bilers Exfoliation Scale in Mate Advances Tubes, Superheater Plants, Power Fossil for rials Technology FUTURE POSSIBILITIES tured TiSiCN coating. Without a tool like like Without a tool TiSiCN coating. tured of quantification the laser microscope, not be would performance materials and nature the tortuous possible due to damage. of the erosion area large valve stem, the combination of small of small combination the stem, valve high veloci and particles oxide hard damage erosion severe cause ties can and EPRI have Utilities cases. in certain options for material been investigating dam the severity of erosion reducing intervals. maintenance extend to age nominally after unit same the from history (hours, operating equivalent the large cycles). and In this case, starts, microscope laser the of field of depth both the amount quantify used to was service after loss and depth of metal The data erosion. localized due to 2.4 times improvement 1.6 to shows that stem a valve for in performance included a ~30 26 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 B TECHNIQUES MECHANICAL TESTING TECHNICAL SPOTLIGHT also encompasses testing, simplecyclic tensile, and flexural testing. However, it ally refers to monotonic compression, stress-relaxation. ties andthusexhibit bothcreep and rials exhibit proper time-dependent motion viafriction.Viscoelastic mate which resists eled using a dashpot, using aspringandviscosity ismod mechanical terms, elasticityismodeled state after undergoing deformation. In of amaterial to return to itsoriginal to flow, whileelasticityisthetendency is themeasure ofafluid’s resistance cous andelasticproperties. Viscosity elastic because feature they bothvis static andfatigue testing. usingacombinationachieved ofboth engineered biomaterials isusually characterization ofbothnatural and ries: softandhard tissues.Mechanical erally bebroken down into two catego testing industry, biomaterials can gen challenging. Inthephysical materials cal properties ofabiomaterial maybe effectively characterize themechani consistent andrepeatable metrics to dons, ligaments, andhair—achieving biological asbone,ten tissues—such another. Given thenatural variability in ical properties asthosethatmake up will nothave theexact samemechan materials thatmake uponeindividual characterization ofbiological materials iscritical. tissues for patient andaging,proper mechanical disease, injury, As scientistsandengineerscontinuetodevelop andinvestigate replacement CHARACTERIZATION BIOMATERIALS TESTING AND Static mechanical testing gener Biological materials are visco multifaceted. As such, the bio and engineered, are inherently iological materials, bothnatural ------decrease nomatter how longtheweight sion ofthespringwould notincrease or constant over time,theinitial exten weight were appliedto aspringandheld not change over time.For example, ifa displacement in a material that will sion orcompression willcreate some elastic material, an applied load in ten sion underaconstant load. Inapurely that involves holdingaspecimen inten align fibers to condition thematerial. cling soft tissues before failure helps and isreferred to aspre-cycling. Pre-cy conducted atthebeginning ofthetest strength, testing simplecyclic isoften cal materials. Whentesting biomaterial the viscoelastic properties of biologi which can helpproperly characterize creep, andstress-relaxation testing, Tensile testing ofbiological tissues. Creep testing isatypeofstatic test - - - - - time. Biological materials primarily to the same amount of strain over stress will decrease or relax in response materials thatexhibit stress-relaxation, would remain constant over time. In resulting force or stress on the spring spring ispulledto adisplacement, the Forment. example, ifapurely elastic tension ataconstant strain ordisplace that involves holdingaspecimen in constant load. will undergo plasticdeformation under over time.Materials thatexhibit creep strain ormaterial extension willincrease fibers, underconstant load, atendon’s as atendon containing mostlycollagen However, inviscoelastic materials such expected in purely elastic materials. is kept on the spring. This behavior is Stress-relaxation isastatic test

- 27 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 ------When tensile testing soft tissues soft testing tensile When Tensile testing of an insect wing. testing Tensile crucial to achieving consistent results. results. achieving consistent crucial to of soft biomaterials nature The delicate in physi- with testing in combination gripping a makes conditions ological in physio tissues Testing challenge. mimic properly to conditions logical inside the human the environment achieve using to easy body is relatively consistently However, bath. a heated grips of set a in specimen a inserting be diffi can in a bath while submerged spec sure and make time save cult. To using a imen alignment is repeatable, rec mechanism is lifting with a bath ommended so that the specimen can the grips and then sub into be inserted place. into raises as the bath mersed gripping mechanism choosing a When soft tissues, side-acting grips that for or pneu manual, spring actuated, are well. work closed generally matically should In addition, the gripping face with high friction to a material feature while mini specimen slippage avoid clamping force. mizing the necessary force maximum determine to failure to calculat at break, or maximum strain extension the machine’s from ing strain This as suitable. is widely accepted is calcu strain of measuring method cross machine’s the taking by lated and dividing it by data extension head However, separation. the initial grip ------Highly sensitive force measure force Highly sensitive gripping the proper Determining ing how those materials will behave will behave those materials ing how the In addition to in the human body. mate biological to inherent variability biomate for setup rials, experimental challenge. a presents also testing rials be can materials biological Testing highly for need the challenging due to delicate measurement, force sensitive and grip, difficult to specimens that are impos that is often measurement strain extensometers. sible with traditional testing mechanical ment is needed for Soft tissue spec of soft biomaterials. usually small and the loads imens are apart pull these materials to required range. in the gram-force generally are that require materials With biological it failure, pull to before pre-cycling that the force ensure to is important accu for is not only verified transducer pre-cycling, for range in the load racy measure to but also has the capacity at specimen failure. force test, all testing methods are critical to to critical are methods test, all testing the bulk mechanical understanding and predict of biomaterials properties is biomaterials testing solution for - - - - While mechanical testing of tis of testing mechanical While also known as also known testing, Fatigue Flexural testing of rat bone. of rat testing Flexural sues can range from a quick pull or pull quick a from range can sues a months-long to fatigue test failure TESTING PARAMETERS PARAMETERS TESTING dynamic testing, helps to character helps to dynamic testing, of materials properties the lifetime ize mechanical constant that experience a human heart example, For loading. 35 million times approximately beats an that ensure to order In year. per used in the tissue material engineered will last a minimum of 10 years, heart at to be subjected the tissue needs to 350 million cycles of mechanical least this test complete to In order loading. the time, of amount reasonable a in ing run at a high machine needs to testing a dynamic testing Using frequency. could machine at 100 Hz, a researcher on a mate of wear 10 years simulate testing Fatigue weeks. rial in just a few the that ensure helps biomaterials of dam- become yield, not will material lifetime. within the required or fail aged, composed of smooth muscle, such as composed a high level of will exhibit the bladder, relaxation. stress for hard tissues such as bone or dental static and fatigue testing to understand enamel, using an extensometer to mea- both bulk and lifetime material proper- sure strain is required. Further, for both ties. Given the natural variability of bio- hard and soft tissues, it is considered materials, it is critical that mechanical best practice to use an extensometer to testing design reduces test variables measure properties such as modulus. such as low force measurement, speci- During a tensile or compression test, a men gripping, and strain measurement. force is applied to a material causing While data sheets with mechanical test deformation. For hard tissues with high specifications are available for materi- stiffness, the material will deflect under als such as polymers, elastomers, and load and some test system deflection metals, biomaterial mechanical prop- (compliance) will also occur. To avoid erties are still largely unknown or only having system compliance factored published academically. As scientists into the specimen’s strain measure- and engineers continue to develop ment, using an extensometer is recom- and investigate replacement tissues mended. Because soft biomaterials are for patient disease, injury, and aging, delicate and fragile, a noncontacting proper mechanical characterization of extensometer such as a laser or video biological materials is critical. ~AM&P model is required. For more information: Elayne Gor- SUMMARY donov is biomedical assistant market Mechanical characterization of manager, Instron, 825 University Ave., both natural and engineered biomate- Norwood, MA 02062-2643, 800.877.6674, rials is done through a combination of www.instron.us.

Tensile testing of hydrogels using a video extensometer.

AMP-NSL-Oct2016-3rd-A.indd 2 10/7/16 1:28 PM 29 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 -

s. There were 21 BOFs in operation in operation 21 BOFs were There - new technol accept to Reluctance Philip Murray, first president of United president first Philip Murray, of Courtesy of America. Steelworkers usw.org. ment made after WWII. Molten metal metal WWII. Molten ment made after was the from delivered this with fewer workers and produced and produced workers this with fewer a superior product. New plants built those replace to and Japan in Europe new implemented in the war destroyed BOFs. (USS) Corp. Steel States United before at the Duquesne plant two built its first in 1963, and 29 units when in Pittsburgh two its first installed Steel Bethlehem in 1964, replacing Point at Sparrows That same open hearths. 40-year-old at BOFs two built the company year, 2.5 mil- which produced Lackawanna, produced The U.S. per year. lion tons in 1965, using BOFs only 17% of its steel as 55%. As late produced while Japan and U.S. the for 48% was ratio this 1970, Japan. 79% for casting the continuous to extended ogy develop European process—another ------The 1959 strike was the longest the longest was The 1959 strike use declined 1957-1962, steel From fully to remove Clause 2b, and the strike and the strike Clause 2b, remove to fully point in the history a pivotal became strike the As industry. steel U.S. the of seri became customers continued, about supply sources ously concerned imported was recourse only their and exporter had been a net The U.S. steel. but in during the 20th century, of steel the for exports 1959 imports exceeded imports reaching time with total first 4.7 million tons. Michigan in company steel small a lier, fur oxygen basic the first had installed (BOF) and Jones & Laughlin Steel nace in these furnaces installed (J&L) Corp. in invented was 1959. The BOF process BOF vessels II. World War after Austria Bessemer the earlier similar to were they used oxygen except converters, from carbon remove to air of instead pro be could steel of A heat iron. cast compared hour than an less in cessed fur open hearth for six or eight hours to accomplished BOFs Importantly, naces. in steel history at 116 days. Grievances history Grievances at 116 days. in steel pensions, and paid included wages, unsuccess fought holidays. Bethlehem market although the total 8% per capita same the At slowly. still growing was industry tryingtime, the steel was to The lack capacity. and expand upgrade adoption was modern technology of built a new evident when Bethlehem shop in 1958 at Sparrows open hearth ear years $200 million. Four for Point be the source of labor problems at labor problems of be the source come. to years for Bethlehem STRIKE OF 1959 AND LAGGING OF 1959 AND LAGGING STRIKE ADOPTION TECHNOLOGY ------

he strike of 1959 was a watershed watershed a of 1959 was he strike moment in the historythe U.S. of The industry. steel integrated

Even so, McDonald never had the so, Even In the early 1950s, David J. McDon David J. 1950s, In the early ald replaced Philip Murray, longtime Philip Murray, replaced ald union. of the steelworkers president moder a be to expected was McDonald expe his limited due to negotiator ate he union. However, in the steel rience Reuther with Walter rivalry had a bitter union who had been elected of the auto of Industrial Orga of the Congress head In subse Murray. (CIO) after nizations tried McDonald quent negotiations, of the ahead the steelworkers keep to 1959, steelworkers By autoworkers: per hour 38 cents roughly earning were (15% more). than autoworkers more as same support of union members in overreached always did, so he Murray seri- A loyal. them keep to attempt his in 1956 with work place took ous strike 35 days. The final settlement out for ers Bethlehem included Clause 2b—for guarantee a union the gave only—that not reduce would that new technology This would the number of employees. strike itself was not the main event, itself was strike industrywidebut it exposed problems many for that had existed and failures poor labor Among them were years. an modernization, delayed relations, mix, and inconve product unbalanced nient mill locations in relation to the to in relation nient mill locations included steady Other factors market. contracts union cover to increases price improvements, than productivity rather by be controlled to had pollution that who staff rulings, and management EPA of any incomes highest the paid were industry. FROM POOR LABOR RELATIONS AND DELAYED MODERNIZATION TO AN UNBALANCED PRODUCT MIX AND PRODUCT AN UNBALANCED TO MODERNIZATION AND DELAYED POOR LABOR RELATIONS FROM 1950 IN THE LATE DECLINE BEGAN ITS STEADY THE U.S. STEEL INDUSTRY LOCATIONS, INCONVENIENT MILL THE DECLINE OF THE INTEGRATED STEEL INDUSTRY—PART I INDUSTRY—PART STEEL OF THE INTEGRATED THE DECLINE T Metallurgy Lane, authored by ASM life member Charles R. Simcoe, is a yearlong series dedicated to the early history of the U.S. metals history metals the early of the U.S. to series dedicated is a yearlong R. Simcoe, member Charles life by ASM authored Lane, Metallurgy and developments. with key milestones industries along and materials METALLURGY LANE METALLURGY 30 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 RISING IMPORTS LOFTY PROJECTS AMID preparation for thefinishingmills. reducing them by forging or rolling in casting ofmetal into large molds and rolling mills.Thisprocess replaced the it solidifiedandwas prepared for the the metal through a container where teemed into amachinethatchanneled lehem’s chairman,ArthurB.Homer. Homer Research Laboratory after Beth - and supportpersonnel andwas named dated over 1000research engineers not complete until1969.Itaccommo buildings andareflecting pool—was tain. The$35millionproject—eight on 1000acres bulldozed from amoun 1957. Bethlehem builtahuge campus with USS who had built its own labin central research laboratory to compete Courtesy ofusw.org. workers unionduringthestrike of1959. David J. McDonald,president ofthesteel in downtown Pittsburgh. U.S. Steel corporate headquarters In 1961,Bethlehem Steel builta - - - AND LAYOFFS CONSOLIDATIONS turned, bothUSS andBethlehem built joined J&LintheLTV Steel Division. it soldallremaining plants to LTV and terminated 5000employees. In 1979, in Youngstown inthelate 1970sand Co. (YS&T). ItclosedtheCampbellplant was Youngstown Iron Sheet andTube pany to disappear from theindustry grated steel industry. Thenext com first casualty in the decline of the inte Steel Division.Thus,J&Lbecame the ownership ofJ&Landcalled ittheLTV later, the company completed total ence in owning a . A few years Vought (LTV)—who hadzero experi a Texas conglomerate, Ling-Temco- an interest in the company in 1968 to increasing imports was sold J&L. They to beaffected market by thenew with make itafully integrated plant. furnaces andBOFs were addedlater to from Johnstown andLackawanna. Blast operations andingots were shippedin of construction was limited to finishing efficient inthecountry. Thefirst phase Itbecame themost equipment. the-art productioning a new layout and state-of- millatBurnsHarbor,a new Ind.,featur als andexporting finishedproduct. ports for ease ofimportingraw materi plantslocatednine new attidewater lion to 100milliontons annuallyfrom had increased production from 25mil imported steel came from Japan, which U.S. steel consumption. Mostofthe increased from 8%to 17%oftotal Laboratory. Courtesy oflehigh.edu. Bethlehem Steel’s HomerResearch Though thewindsofchange had The first integrated steel company In 1964,Bethlehem decidedto build From 1960to 1970,imports

------gmail.com. Simcoe can be reached at crsimcoe1@ For more information: yearsjust seven earlier. oratory and Martin Tower facilities built year, 800from theHomerResearch Lab minated 2500white-collar workers that Lackawanna plants. The company ter closing parts oftheJohnstown and loss ofnearly $500millionandbegan during thenext decade. during the1970s,butincreased to 22% imports heldsteady atroughly 15% U.S. integrated steel industry. Foreign capacity compared with11%for the continuous casting 46%oftheirsteel Atplant. thistime,theJapanese were ous cast slabsin1969attheJohnstown abandoning its first attempt to continu- ous caster atBurnsHarbor in 1975after conditions. outdated to compete market in thenew become obvious thatthemillswere too and asheet millinstalled in1935.Ithad naces andfinishingmillsasold1900 in 1979,aplantwithopenhearth fur later only20,000workers remained. 120,000 in the mid 1970s, but 20 years of $200million.Employment reached tons offinishedproduct andearnings hem hadpeak production of16million $35 million.Thesameyear, Bethle tower 21-story Martin. Thenew cost Pa., namedfor itschairman,Edmund hem builtMartinTower inBethlehem, downtown Pittsburgh. In1972,Bethle officeing a $50 million, 64-story in early 1970s.USS was construct first, corporatenew headquarters inthe Steel inBethlehem, Pa. Martin Tower, headquarters ofBethlehem In 1977,Bethlehem reported a Bethlehem finally built a continu- USS closeditsYoungstown plant Charles R. ------

NOVEMBER/DECEMBER 2016 | VOL. 11 | ISSUE 4 Thermal Spray Society ASM INTERNATIONAL

THE OFFICIAL NEWSLETTER OF THE ASM THERMAL SPRAY SOCIETY

THERMAL SPRAY COATINGS IN EMERGING TECHNOLOGIES

SOCIETY NEWS 3 JTST HIGHLIGHTS 13

tss.asminternational.org WE DO

IT ALL

EQUIPMENT | CONSUMABLES | DEVELOPMENT

www.coatingsolutions.saint-gobain.com [email protected] 1-800-243-0028 33 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 iTSSe TSS 1

ISSUE 4 ISSUE | 11 VOL. 12 CASE STUDY—ONLINE CASE STUDY—ONLINE TOOLS DIAGNOSTIC THERMALIMPROVE PROCESS SPRAY | 2016 NOVEMBER/DECEMBER HIGHLIGHTS 6 8 BOUT THE COVER AEROSOL METHOD FOR ROOM TEMPERATURE DEPOSITION THICK-FILM COLD SPRAY: ADVANCED CHARACTERIZATION METHODS— CHARACTERIZATION ADVANCED SPRAY: COLD DIFFRACTION X-RAY DEPARTMENTS 2 | EDITORIAL NEWS SOCIETY 3 | ASM THERMAL SPRAY 13 | JTST fed into the arc gun at controlled speeds. When wires are brought together at the contact at the contact together brought are speeds. When wires gun at controlled arc the into fed tips. Compressed melt the wire continuously to enough heat create point, opposing charges form to surface the workpiece it onto and accelerate material molten atomize air is used to the coating. A usually of the same composition, wires, uses two metallic process spray wire The electric arc as the coating feedstock. The two wires are electrically charged with opposing polarity and charged electrically are feedstock. The two wires as the coating -

THE OFFICIAL NEWSLETTER OF THE ASM THERMAL SPRAY SOCIETY OF THE ASM THERMAL SPRAY THE OFFICIAL NEWSLETTER EDITORS Charles M. Kay Bamola Rajan EDITOR MANAGING Julie Lucko DIRECTOR CREATIVE Jim Pallotta AND DESIGN LAYOUT Fornadel Kate MANAGER PRODUCTION Kelly Sukol MANAGER ACCOUNT NATIONAL Erik Klingerman ext. Ohio 440.338.5151 5574 Park, Materials [email protected] SOCIETY THERMAL SPRAY COMMITTEE EXECUTIVE President Douglas G. Puerta, President Past Immediate Christian Moreau, President McDonald, Vice André Dan C. Hayden, Secretary/Treasurer EDITORIAL OPPORTUNITIES OPPORTUNITIES EDITORIAL IN 2017 iTSSe FOR in 2017 reflects iTSSe for focus The editorial of thermal spray applications established and such as power generation technology as new as well applications transportation, for opportunities the latest representing engineering. and surface coatings Issue: February Industry/Military Applications Aerospace Julie Lucko an article, contact contribute To at [email protected]. Erik Klingerman, advertise, contact To at [email protected]. ™ is pub Engineering & Surface Thermal Spray International lished quarterly by ASM International®, 9639 Kinsman Road, 9639 Kinsman Road, by ASM International®, lished quarterly OH 44073; 440.338.5151; asminternational.org. Park, Materials 4. Copyright© 2016 by ASM International®. 11, No. Vol. All rights reserved. - of manuscripts in Internation and publication The acceptance Engineering does not imply that & Surface al Thermal Spray or endorse approve, accept, or ASM International® the editors Although of the authors. opinions, and conclusions the data, & Spray Thermal manuscripts published in International significance, have archival to intended Engineering are Surface to insufficient frequently are and interpretations data author’s testing, specific design, production, to translatable be directly - without independent examina applications or performance by and suitability of their applicability tion and verification qualified personnel. professionally ASM INTERNATIONAL ASM Thermal Spray Society Spray Thermal 34 iTSSe TSS EDITORIAL A HISTORY LESSON

ears ago, trying to be an encourag- With this in mind, during the remainder of this year and ing father, I bought my children a into 2017, leading technologies focused on state-of-the-art book that outlined history in chart advancements will be presented first at the Cold Spray Con- formY showing different time periods with ference in Edmonton, Canada, and next year at the annual notable events including influential peo- International Thermal Spray Conference (ITSC 2017) in Dus- ple, politics, wars, science, medicine, no- seldorf. Throughout this issue, you will find advancements table discoveries, art, music, and much that may influence thermal spray and cold spray technol- more. My baseline to give some meaning ogies and how we think about these topics for decades to was the white oak tree in my backyard in Kay come. And the progress never stops—thanks to the high Ohio that is approximately 350 years old. energy group of TSS volunteers and associates around the I should also mention that at the time I was doing this, the in- globe. ternet was just beginning! Just think, perhaps one day general history books will In that same vein, one TSS founding father and influence have a section devoted to thermal spray that children will most of us know, Dr. Christopher Berndt, has undertaken sim- bring home and share with their parents. ilar initiatives to outline the history of thermal spray as well Happy spraying! as influential people and companies. For many of us in the field, the history is rather fascinating when you see the impact and growth through decades of thermal spray use showcas- Charles M. Kay ing the advancements in science, technology, and everyday iTSSe co-editor applications. ASB Industries ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED TSS iTSSe

2 35

SOCIETY NEWS iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

REVIEW ARTICLE New board members elected for a three-year term AVAILABLE ON COLD include Komal Laul, senior process engineer, Chromal- SPRAY DEPOSITION loy; James A. Ruud, materials scientist, General Electric; president, VandenBergh & Asso- The September issue of In- Maurice E. VandenBergh, ciates Inc. ternational Materials Reviews features the article “The Unique Two student members were also appointed to the Abilities of Cold Spray Deposi- board for a one-year term: Ankur Gupta, University of Cen- tion” by Victor Champagne and tral Florida, and Gregory Smith, Stony Brook University. Dennis Helfritch. The review is useful to those new to cold spray, members of the cold spray community, and prod- uct developers in need of cold spray capabilities. Descriptions of equipment and techniques used to create cold-spray deposits are helpful to those seeking to produce products requiring similar characteristics. The jour- nal is co-owned by ASM International and IOM3. Visit http:// tinyurl.com/j5lp5lr to purchase and download the article. Puerta Moreau McDonald

NOMINATIONS SOUGHT FOR ASM THERMAL SPRAY SOCIETY BOARD The ASM TSS Nominating Committee is currently seeking nominations to fill three board member positions. Candidates may be from any segment of the thermal spray community. Nominees must be a member of the ASM Thermal Spray Society and must be endorsed by five TSS members. Board members iTSSe whose terms are expiring may be eligible for nomination and Hayden Laul Ruud possible re-election on an equal basis with any other nominee. Nominations must be received no later than March 1, 2017. Forms can be found at tss.asminternational.org. For more infor- mation, contact Christian Moreau, nominating committee chair, at [email protected]. TSS

SEEKING STUDENT MEMBERS FOR TSS BOARD The ASM Thermal Spray Society is seeking applicants for the two student board member positions. Nominations are due VandenBergh Gupta Smith by March 1, 2017. Students must be a registered undergradu- ate or graduate during the 2016-2017 academic year and must 3 be studying or involved in research in an area closely related to the field of thermal spray technology. For more information, visit tss.asminternational.org.

TSS ANNOUNCES NEW BOARD MEMBERS The ASM Thermal Spray Society elected officers and board members for 2016. Douglas G. Puerta, director–aerospace product qualifications, Element Materials Technology, succeeds as president of TSS, while Christian Moreau, FASM, TS-HoF, professor, Concordia University, remains on the board as im- mediate past president. André McDonald, associate professor, University of Alberta, is elected vice president. Officers serve a two-year term. In addition, Dan C. Hayden, president, Hayden Corp., continues on the board as secretary/treasurer for a one- year term. 36 iTSSe TSS EDITORIALSOCIETY NEWS

TSS PRESIDENT’S AWARD FOR MERITORIOUS SERVICE This award recognizes exceptional service to the Ther- mal Spray Society and community. Jeganathan Karthikeyan, FASM, (right) director of research and development, ASB In- dustries, received the 2016 TSS President’s Award for Meritori- ous Service from TSS President Christian Moreau on June 20 at a company picnic held in his honor.

ASM DISTINGUISHED LIFE MEMBER AWARD Albert Kay, FASM, president, ASB Industries, Barber- ton, Ohio, received this year’s ASM Distinguished Life Member Award “in recognition of outstanding innovation and early commercialization of emerging thermal spray technolo- gies including high-velocity oxyfuel and cold spray; ex- emplary development of a DeWAL business model that gained Where new ideas, like precision tapes, never run out. worldwide recognition; and Kay for dedication and unselfishness, unstinting per- sonal effort, and leadership on behalf of the Ther- mal Spray Society and ASM International.” The ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED High precision plasma award was established in 1954 and is conferred on tapes and taping solutions, leaders who have devoted their time, knowledge, manufactred in USA and and abilities to the advancement of the materials distributed worldwide. industries. His award will be presented during a future Akron Chapter meeting. DeWAL BlueShield conformal

TSS masking tape for HVOF MAKE PLANS TO ATTEND THE NORTH AMERICAN COLD SPRAY CONFERENCE The ASM Thermal Spray Society and the Canadian Cold Spray Alliance will jointly present the 2016 North American Cold Spray Conference iTSSe from November 30 through December 1 at Alber- Dozens of dependable thermal spray tapes ta Innovates – Technology Futures, Canada. The 4 biennial event showcases the latest technical insights from international experts in industry, government, and academia on new technol- ogy, exciting applications, and cutting-edge research. The conference also features a tabletop exhibition and ample networking opportunities for face-to-face interaction. Applicator kits for thermal spray tape The two-day multidisciplinary program includes invited presentations from prominent speakers in the areas of additive manufacturing; applications—case studies, cost analysis, and optimization; equipment and quality control; Quality of Product...First fundamentals: physics, science, modelling, and Narragansett, RI 02882 characterization; science and engineering of [email protected] 800-366-8356 powders; and the brand new, young profession- 001-401-789-9736 als’ student presentations. Visit asminternation- dewal.com/industries/thermal-spray-tapes al.org/coldspray for more information.

38 iTSSe TSS FEATURE ARTICLE

COLD SPRAY: ADVANCED CHARACTERIZATION METHODS—X-RAY DIFFRACTION This article series explores the indispensable role of characterization in the development of cold spray coatings and illustrates some of the common processes used during coatings development. Dheepa Srinivasan, GE Power, GE India Technology Center, Bangalore

-ray diffraction (XRD) is a versatile tool for preliminary Due to the severe plastic deformation that takes place during characterization of phases in cold spray coatings. A high-pressure cold spray, the characteristic diffraction pat- collimated beam of x-rays with a wavelength of 0.5 to tern in the as-sprayed condition usually has broad peaks, as X2 Å is diffracted by the crystalline phases in the specimen ac- shown in Fig. 1(a) for an IN625 coating. Peak broadening in the cording to Bragg’s law. The diffraction pattern identifies the as-sprayed coating compared to the powders can be due to material’s structural properties, such as structure, lattice pa- two factors—particle size broadening and broadening due to rameter, strain (which is measured with great accuracy from strain (nonuniform). The full width at half maxima (FWHM) of the diffraction peaks), epitaxy, and size and orientation of the the diffraction peak is estimated from the Scherrer formula for crystallites. The probing depth is a few micrometers to tens of particle size broadening: micrometers, depending on the absorption coefficient of the d = 0.9λ/βcosθ material for the particular wavelength of the x-ray probe. Cold spray coating analysis starts with powder charac- where d is particle size, λ is the x-ray’s wavelength, β is FWHM ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED terization, followed by as-sprayed and heat treated coatings. of the x-ray peak (in radians), and θ is peak angle. Typically, the Scherrer formula is based on the assumption that peak broad- ening is caused by crystallite size. The nonuniform strain-in- duced broadening effect of the FWHM is obtained by the Williamson-Hall (WH) plot, which is derived by the equation:

TSS ε = βcosθ − A/2sinθ where A is expressed as Cλ/d, C is the correction factor ( 1), and d is particle size. Figure 1(b) shows the WH plot for an IN625 coating, with a grain size of 35 nm. XRD can identify coat∼ - ing phases and distinguish any changes to the phase equilib- ria during cold spray. Figure 2(a) illustrates cold spray titanium iTSSe

6 (a)

(b) Fig. 1 — (a) X-ray diffractograms comparing IN625 (nickel-base (a) (b) superalloy) powders and cold spray IN625 coating show broaden- Fig. 2 — X-ray diffraction patterns from (a) cold spray titanium coat- ing of diffraction peaks in the coating, indicative of macroscopic ing after removal of progressive layers from the coating compared strain. (b) Hall-Williamson plot taken from peak broadening data to with α titanium, indicating no phase transformation in the coating, calculate the extent of strain. FWHM, full width at half maximum. and (b) cold spray WC-Co without after cold spray. 39

FEATURE ARTICLE iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

(a) (b) (c) (d) Fig. 3 — X-ray diffraction patterns comparing (a) warm spray and (b) cold spray titanium coatings, along with the respective starting powders indicate the presence of TiO oxides and metal in the warm spray coating. Williamson-Hall plots for the (c) warm spray and (d) cold spray coat- ings indicate a lower degree of strain in the warm spray coating.

eliminate detrimental effects to the microstructure, such as oxide formation. Figures 3(b) and (c) compare the WH plots between warm- and cold-spray titanium, indicating that the coatings contain more nonuniform strain as compared to the powder. However, between the two coatings, the cold spray coating shows a higher level of strain than those in the thermally soft- ened process of warm spray coatings. Particle sizes indicated by the WH plots range between 38 and 40 nm. Peak FWHM is used to interpret the surface state of the

(a) (b) material. Figure 4(a) shows a representative FWHM taken from the work of Ghelichi and Bagherifard from their studies on an Fig. 4 — (a) Full width at half maximum (FWHM) from an x-ray Al7075 cold spray coating onto an aluminum substrate. A big diffractogram peak corresponding to a cold spray Al7075 coating. iTSSe jump at the interface between the deposited material and the (b) Mapping the FWHM through coating thickness and substrate to substrate is shown in Fig. 4(b), which represents the FWHM estimate grain size. measured through coating thickness into the substrate. In this case, by applying the de Keijser method, material grain size coating characterization with progressive removal of layers. A ranges between 20 and 50 nm, from a convolution of the dif- comparison between the as-sprayed coating and α titanium fraction pattern. TSS indicates that no phase transformations take place during Several reports have thus made use of XRD to charac- cold spray. terize powders, as-sprayed coatings, extent of lattice strain, Another example includes characterization of the ab- phase transformations in as-sprayed versus heat treated con- sence of decarburization in a WC-Co coating. In Fig. 2(b), a ditions, and grain size. Typically, flat samples are recommend- comparison between the powders and cold spray WC-Co coat- ed in order to obtain precise values of lattice spacing from the ing indicates the absence of any decarburization. Moridi, et x-ray diffractogram. Apart from this, no special care is needed 7 al., were able to distinguish between a cold spray coating and during sample preparation. The top surface should be slightly the substrate for a titanium alloy using XRD, and Rokni, et al., ground off so that any oxides on the surface do not lead to arti- showed an extensive peak broadening that is typically charac- facts or additional peaks in the XRD pattern. ~iTSSe teristic of cold sprayed coatings in the as-sprayed condition. Upon heat treatment, the peaks become sharper, indicative of For more information: Dheepa Srinivasan is a principal en- stress relaxation in the coatings. In all cases, coating residual gineer at GE Power, GE India Technology Center, Bangalore, stresses diminish with heat treatment to a more tensile value, [email protected], www.ge.com. This article series is as reflected by a sharpening of the peak, as shown in Fig. 1(a). adapted from Chapter 5, Cold Spray—Advanced Characteriza- Cold spray coatings are nearly always crystalline with tion, in High Pressure Cold Spray—Principles and Applications, sharp diffraction peaks. X-ray diffraction can identify phase edited by Charles M. Kay and J. Karthikeyan (ASM, 2016). formation during variations in the process, such as in the case illustrated in Figs. 3(a) and (b). Kim, et al., have done extensive characterization of cold spray versus warm spray using XRD, wherein the presence of oxides of titanium is prev- alent in the warm-spray coatings, and absent in cold spray. The authors conclude that solid-state spray can minimize or 40 iTSSe TSS FEATURE ARTICLE

AEROSOL METHOD FOR ROOM TEMPERATURE THICK-FILM DEPOSITION Aerosol deposition offers an alternative to conventional thin film processes when mesoscale coatings are needed. Pylin Sarobol,* Andrew Vackel, Jesse Adamczyk,* Thomas Holmes, Mark Rodriguez, James Griego, Mia Blea, and Harlan Brown-Shaklee, Sandia National Laboratories, Albuquerque, N.M.

eramic and metallic thick film (>5 µm) processing AD PROCESS RESULTS typically requires high temperatures or reactive en- Previous work has proven that submicron ceramic parti- vironments that limit integration of film/substrate cles undergo dislocation nucleation/slip, plastic deformation, Cmaterials with drastically different melting points or ther- fracture, and consolidation in the AD process at room tem- mal properties. In many spray processes, particle melting/ perature. Submicron ceramic particles with diameters >100 solidification and splatting lead to highly defective micro- nm capable of plastic deformation should be selected as feed- structures, containing splat boundaries, porosity, oxide in- stock for the aerosol deposition process. Submicron alumina clusions, and nonstoichiometric oxide formation. Moreover, particles can deform plastically via dislocation nucleation and melting/solidification associated with thermal spray can slip, as well as fracture without fragmentation, under qua- lead to loss of volatile elements, change in original crystal si-static compressive loading. Research also shows that im- structure, and altered properties. The aerosol deposition pact at high velocity can cause submicron alumina particles to (AD) process is being used to create readily integrated, high deform, change shape without fragmentation, and adhere to ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED density ceramic and metallic thick films on a variety of sub- the substrate as an anchor layer. strates at room temperature. Bonding between an individual splat and substrate is present near the middle of the splat whereas gaps remain AEROSOL DEPOSITION PROCESS around splat edges. Subsequent particles impacting on the In the AD process, thick films are produced by accel- splatted anchor layer produce a tamping effect. Gaps around erating submicron to micron sized particles onto a substrate in TSS the splatted particles and substrate are closed and bonding a low-vacuum environment chamber. AD is able to conformal- between the anchor layer and substrate is complete. Conse- ly deposit dense, thick films up to ~100 µm, which bridges the quently, film buildup relies on the tamping effect to deform, gap between coatings fabricated with thin film technologies fracture, and mechanically bond the arriving particles to the and traditional thermal spray technologies. AD takes advan- already deposited particles. An example of AD Al2O3 single tage of the low pressure within the vacuum by allowing spray splats and coatings is shown in Fig. 1. Splat boundaries within particles to maintain velocity and consolidate in the solid state

iTSSe the coatings are undistinguishable from other grain boundar- into a film on impact with the substrate and subsequent film. ies. The consolidated coating is polycrystalline with 15-30 nm When the carrier gas for the aerosol powder hits the substrate, nanocrystals. the gas compresses and creates a densified gas layer above the 8 The fundamental knowledge on deformation and bond- substrate, similar to the bow shock in cold spray. However, in ing gained from the previous work provides a strong founda- AD the bow shock/particle interaction is reduced in the vacu- tion to mature the aerosol deposition process for fabricating um, allowing small particles with low momentum to penetrate ceramic, metallic, and composite films on metallic, glass, and the bow shock layer and impact the substrate with sufficient plastic substrates at room temperature. Potential applications kinetic energy for deposition. of aerosol deposition being investigated include direct applied AD takes advantage of the small particle size and the abil- multilayered ceramic capacitors, electrically conductive elec- ity of ceramic and metallic particles to plastically deform at a trodes, thermally and chemically resistant barrier coatings, small length scale and bond as coatings. At Sandia National and electrically insulating films. Examples of AD material inte- Laboratories, fundamental experiments were performed to gration are shown in Fig. 2. understand how submicron ceramic particles deform and bond to the substrate in the AD process. Ultimately, the knowl- APPLICATION OF BaTiO3 DIELECTRICS edge gained is being used in R&D work, yielding new potential The application of BaTiO3 dielectrics for high tempera- applications. ture stable capacitors to enable high power electrical switch- ing devices is explored. The high sintering temperature of

*Member of ASM International BaTiO3 (T>1000°C) often prevents successful integration with 41

FEATURE ARTICLE iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 iTSSe

Fig. 1 — (Top row) SEM top view images of splatted Al2O3 particles from quasi-static loading (left) in the indentation experiment and impacting on the substrate in the AD process (middle). Cross-section TEM image of AD splatted particle showing nanocrystallinity (right). (Bottom row)

SEM top view images of AD Al2O3 films at low (left) and high (middle) magnifications. Cross-section TEM image of AD Al2O3 coating on sapphire shows nanocrystallinity and deformed substrate (right). TSS

9

Fig. 2 — Examples of integrated AD coatings—Al2O3-Cu graded coating on Kovar, Al2O3 on Si, Cu on alumina, patterned Ni interconnect on alumina, and Cu-BaTiO3-Cu on alumina. 42 iTSSe TSS FEATURE ARTICLE

low melting point substrates such as glass, metal, or plastic. resistance, dielectric constant, and dielectric loss are therefore

Moreover, BaTiO3 is susceptible to point defect formation by significantly impacted by melting/solidification in traditional highly reducing thermal processes. Thermal spray lends itself plasma spray. to electron-rich point defect formation due to volatilization The AD process was used to successfully integrate high

of typical A-site ­substitution cations, including bismuth or density thick BaTiO3 films with copper (Tm = 1085°C) at room

lead. In addition, oxygen vacancy formation that contributes temperature. The aerosol deposited BaTiO3 film crystal struc- to sub-band electrical transport is enhanced by the thermal ture, grain size, residual strain, and dielectric properties are processing and rapid quenching used in thermal spray pro- currently being investigated. Preliminary results show that

cesses. The associated dielectric properties, such as insulation 5-7 µm thick BaTiO3 films produce 1 nF capacitors with a 2 x 2 mm (providing a 4 mm2 area) gold electrode. A 3 x 3 matrix of electrodes was defined on the 1-cm deposition area. Each electrode spans a 4 mm2 area. Seven of the nine 4 mm2 elec- trodes demonstrate potential as capacitors with loss values in- dicative of continuous, non-cracked films. Figure 3 shows the frequency dependent capacitance and dielectric loss from 100 Hz to 1 MHz. As-aerosol-deposited films exhibit some space charge contribution to polarization. The permittivity of the films was calculated to be k~200, which is consistent with oth- er published research.

Although polycrystalline BaTiO3 capacitors generally exhibit k>1000 at room temperature, these films exhibit sig- nificant crystalline disorder and amorphous grain boundary volume. This combination of grain boundary volume and ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED crystalline disorder reduces polarization by hindering Ti4+ mobility within the unit cell and reduces domain wall motion by defect pinning. In addition, these films exhibit significant in-plane crystallographic strain quantified by XRD analysis. The in-plane strain is approximately 1% as determined by XRD analysis (Fig. 4), which corresponds to an approximate com- TSS pressive stress of 1 GPa. Fig. 3 — Frequency dependent capacitance and dielectric loss The as-deposited coatings also have very small grain (tan ∂) of 4 mm2 capacitors defined on as sprayed 5-7 µm thick films on Kovar. Low frequency dielectric loss is a common attribute of size (20-75 nm or less). Small grain size may be beneficial for structural ceramics, but larger grain size on the order of as-sprayed BaTiO3 that exhibits significant space charge contribu- tion to total polarization. iTSSe

10

Fig. 4 — XRD measurement and strain calculation on the 4 µm thick BaTiO3 film on Kovar substrate. The strain was on the order of ~1%, corre- sponding to ~1 GPa residual compressive in-plane stress. 43

FEATURE ARTICLE iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

100-1000 nm is generally required to maximize permittivity of an alternative to conventional thermal spray processes when ferroelectric ceramics. Post-deposition treatment is near 100% coating density and compatibility with a thermally required to achieve grain growth, improve crystal quality, and sensitive component is required. ~iTSSe relieve residual stresses, which increases dielectric constant and promotes ferroelectricity. For more information: Pylin Sarobol is senior technical staff member, coatings and additive manufacturing R&D at Sandia CONCLUSION National Laboratories, P.O. Box 5800, Albuquerque, NM 87185, Aerosol deposition is a solid state deposition process 505.284.7699, [email protected], www.sandia.gov. that is gaining interest as it can produce functional metallic, ceramic, and composite coatings at room temperature and Acknowledgment can potentially further device design, fabrication, and inte- The authors thank Donald Susan, Deidre Hirschfeld, gration. The fundamental knowledge behind particle plastic Rick Kellogg, and Aaron Hall for their support. This work is deformation and bonding for coating consolidation was inves- supported by Office of Electricity and Laboratory Directed tigated. The flexibility of the aerosol deposition process allows Research and Development Program at Sandia National Lab- investigation of a variety of potential applications, including oratories. Sandia National Laboratories is a multi-mission electrical interconnects, electrical insulating coatings, and di- laboratory managed and operated by Sandia Corp., a wholly electric coatings toward capacitor fabrication. The AD process owned subsidiary of Lockheed Martin Corp., for the U.S. DOE’s offers an alternative to conventional thin film processes when National Nuclear Security Administration under contract mesoscale coatings are required. The AD process also offers DE-AC04-94AL85000. iTSSe TSS

11 44 iTSSe TSS CASE STUDY

ONLINE DIAGNOSTIC TOOLS IMPROVE THERMAL SPRAY PROCESS

REASON TO CONSIDER RESURFACING VALUE OF INSPECTION Keeping a particle’s characteristics constant over time Nearly three decades ago, thermal spray researchers yields coatings with very similar properties. An experiment recognized the need for advanced diagnostic tools able to pro- was conducted where 8%-YSZ is sprayed for 37 hours starting vide spray material characteristics just before impingement with a brand new set of electrons. The torch is stopped and re- on the part, independently of upstream parameter controls. started every hour. Visual inspection of the inside of the nozzle This need was focused mostly around fundamental under- is carried out every hour and gun power is measured. Finally, standing of the spray process, validation of thermo- and flu- particle characteristics are monitored using an online spray id-dynamic models, development of advanced materials, and diagnostic tool from Tecnar, Canada. After 37 hours, the elec- development and optimization of spray equipment. Produc- trodes are worn, gun power has decreased, and the initial mi- tion managers, on the other hand, had different objectives

crostructure of the coating (TBC) has disappeared. However, in mind—namely improving coating reproducibility (Ppks and

after the 37 hours, spray parameters were modified to retrieve Cpks), extending electrode lifetime, reducing test coupons, im- the initial particle properties as well as corresponding coating proving DE, better forecasting of coating thickness, and spray- characteristics such as porosity, vertical crack network, and ing correctly the first time. deposition efficiency (DE). OPTION It is well known that lot-to-lot variations exist for com- mercially available powders, and that powders supposed to ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED be a direct replacement sometimes yield very different coat- ings. Below is an example where the same powder (reference) has been used for more than a decade. For various reasons, an alternate supplier is sought. Two other suppliers propose a direct replacement to the reference powder. The three mate- Fig. 1 — Effect of electrode wear on coating characteristics. rials are sprayed the same morning, with the same torch and TSS hopper, in the same spray booth, and by the same operator. Coupons are produced and, for each spray run, particle char- acteristics are measured using an online spray diagnostic tool.

BENEFITS Results clearly show that Alternate-1 succeeded in pro- iTSSe viding a direct replacement powder, which was confirmed by the coating microstructure. Alternate-2 provided a material 12 significantly different from the sensor standpoint, which was also confirmed by coating microstructure. ~iTSSe Fig. 2a — New electrode. Fig. 2b — Worn electrode. Average Average Powder velocity temperature Microstructure (m/s) (°C) Original 613 1549 Reference Same as Alternate-1 616 1535 reference Different (denser Alternate-2 652 1819 coating) For more information: Luc Pouliot is executive vice president, Tecnar, 1321 Hocquart St., Saint-Bruno-de-Montarville, QC, Canada, J3V 6B5, 450.461.1221 ext. 235, [email protected], www.tecnar.com.

Images courtesy of Christian Moreau/National Research Fig. 3 — Evolution of plasma power over time. Council of Canada. 45

JTST HIGHLIGHTS iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

The Journal of Thermal Spray Technol- Measurements are separated into two different parts: Cold ogy (JTST), the official journal of the ASM (without arc and particles) and hot (with arc and particles). Thermal Spray Society, publishes con- Results provide the first detailed understanding of the effect of tributions on all aspects—fundamental different LDS process parameters. A correlation between the and practical—of thermal spray science, gas parameter settings and the particle beam properties was including processes, feedstock manufac- found. Using established and adapted diagnostic tools, also ture, testing, and characterization. As the used in conventional TWAS processes, this special LDS process primary vehicle for thermal spray informa- was investigated and the results (gas and particle behavior) tion transfer, its mission is to synergize the rapidly advancing validated, thereby allowing explanation and comparison of thermal spray industry and related industries by presenting the diagnostic methods, which is the main focus. Based on research and development efforts leading to advancements error analysis, individual instabilities, limits, and deviations in implementable engineering applications of the technology. during the gas determinations and particle measurements are Articles from the October and December issues, as selected explained in more detail. The paper concludes with presenta- by JTST Editor-in-Chief Armelle Vardelle, are highlighted here. tion of the first particle-shadow diagnostic results and main The December issue also features the 7th Asian Thermal Spray statements regarding these investigations (Fig. 1). Conference (ATSC-7). In addition to the print publication, JTST is available online through springerlink.com. For more infor- MANUFACTURING AND PROPERTIES OF mation, visit asminternational.org/tss. HIGH-VELOCITY OXYGEN FUEL HVOF)-SPRAYED FeVCrC COATINGS ESTABLISHED AND ADAPTED DIAGNOSTIC Paolo Sassatelli, Giovanni Bolelli, Luca Lusvarghi, Tiziano TOOLS FOR INVESTIGATION OF A SPECIAL Manfredini, and Rinaldo Rigon TWIN-WIRE ARC SPRAYING PROCESS This paper studies the microstructure, sliding wear be- Johannes König, Michael Lahres, Stephan Zimmermann, havior, and corrosion resistance of high-velocity oxygen fuel and Jochen Schein (HVOF)-sprayed FeVCrC-based coatings. Various process pa- In a twin-wire arc spray (TWAS) process developed by rameters were tested to evaluate their effects on coating prop-

Daimler AG, known as LDS (Lichtbogendrahtspritzen), gas in- erties, which were also compared to those of HVOF-sprayed iTSSe jection and arc feed play a crucial role in separating molten NiCrBSi and Stellite-6 coatings. Fe-alloy coatings are com- particles from the wire ends. This paper describes an investi- posed of flattened splats, originating from molten droplets gation of the gas and particle behavior according to individual and consisting of a super-saturated solid solution, together LDS process parameters. Coating problems are not considered. with rounded particles, coming from partially unmolten ma- terial and containing V- and Fe-based carbide precipitates. All

process parameters, apart from extreme settings with excess TSS comburent in the flame, produce dense coatings, indicat- ing that the feedstock powder is quite easily processable by HVOF. These coatings, with a microhardness of 650-750 HV0.3, exhibit wear rates of ≈2 × 10−6 mm3/(Nm) in ball-on-disk tests

against sintered Al2O3 spheres. They perform far better than the reference coatings, and better than other Fe- and Ni-base 13

Fig. 2 — SEM micrograph of Sample 1 cross-section after electro- Fig. 1 — Laser doppler anemometry: Principle of setup. chemical polarization test. 46 iTSSe TSS JTST HIGHLIGHTS

alloy coatings tested in previous research. On the other hand, COLONIZATION OF BACTERIA ON corrosion resistance of the coating material (tested by electro- THE SURFACES OF COLD SPRAYED chemical polarization in 0.1 M HCl solution) is quite low. Even COPPER COATING ALTERS THEIR in the absence of interconnected porosity, this results in ex- ELECTROCHEMICAL BEHAVIORS tensive, selective damage to the Fe-base matrix. This coating Xinkun Suo, Peng Xia, Yi Liu, Leila Abdoli, Xiaotao Luo, material is therefore unadvisable for highly corrosive environ- Guanjun Yang, and Hua Li ments (Fig. 2). Copper coatings were fabricated on stainless steel plates EFFECT OF SOLID SHIELD ON COATING by cold spray. Attachment and colonization of Bacillus sp. on PROPERTIES IN ATMOSPHERIC the surfaces of cold spray copper coatings in artificial seawa- ter were characterized and their effects on anti-corrosion per- PLASMA SPRAY PROCESS formance of coatings were examined. Attached bacteria were Ting Liu, Lili Zheng, and Hui Zhang fixed and observed using field emission scanning electron This paper investigates the impact of shrouded shield microscopy (FESEM). Electrochemical behaviors including structure on plasma spray processes and optimal shield potentiodynamic polarization and electrochemical imped- structure selection. Plasma flame characteristics’ response to ance spectroscopy with and without bacterial attachment solid shield structures is studied first, and experimental inves- were evaluated using the commercial electrochemical analy- tigations are then performed for both atmospheric (APS) and sis station, Modulab. Results show that Bacillus sp. prefers to shrouded (SPS) plasma spray processes. Use of a conical shield settle on low-lying spots of coating surfaces in an early stage, with a divergence angle of 5.5° and 90-mm length is effective followed by recruitment and attachment of extracellular poly- to form a low-oxygen (<2%) and high-temperature (>3000 K) mers (EPS) secreted through metabolism of Bacillus sp. The region in the plasma flame, which covers the main area where bacteria survives on coating surfaces with the protection of particles pass by. The average particle temperature is higher EPS. The attachment model is proposed to illustrate bacteria in SPS than APS with the given conditions, and such behavior behaviors on the surface of copper coatings. Electrochemical ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED is intensified as solid shield length increases. Using SPS, more data shows that current density within the Bacillus sp. envi- disk-shaped splats are obtained and the oxygen concentration ronment decreases compared to that without. Charge-trans- in the coating is significantly reduced. The degree of oxidation fer resistance increases markedly in bacteria-containing ASW, in the coatings is further reduced as the length of the solid suggesting that corrosion resistance increases and corrosion shield increases from 50 to 90 mm. Applying the solid shield rate decreases. The influence mechanism of bacteria settle- leads to high flame temperature and low oxidation; howev- TSS ment on corrosion resistance of cold spray copper coatings is er, substrate overheating and velocity reduction may occur. discussed (Fig. 4). For the cases studied, optimal shield length is around 90 mm (Fig. 3). iTSSe

14

Fig. 3 — Optical micrograph of splat morphology: APS process. Fig. 4 — Surface morphology of copper powder. 47

JTST HIGHLIGHTS iTSSe TSS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

CORRELATION OF IMPACT CONDITIONS, INTERFACE REACTIONS, MICROSTRUCTURAL EVOLUTION, AND MECHANICAL PROPERTIES IN KINETIC SPRAYING OF METALS: A REVIEW Jaeick Kim and Changhee Lee Most studies into kinetic spray technology focus on basic research, but a large portion of current research is devoted to industrial applications of the technology. However, to advance studies on industrial applications of kinetic spray requires a profound understanding of the scientific foundations of the process. Nevertheless, there is not yet a well-organized sum- mary of the correlations among impact conditions, interface reactions, microstructural evolution, and mechanical prop- erties across the whole field of kinetic spray technology. This paper provides an overview of these correlations for kinetic spray of metals. For each correlation, interactions between the given conditions and material properties of the metal feed- stock powder are the most influential. These interactions are so complicated that it is difficult to systematically classify all cases into certain types. An attempt is made to explain and summarize the critical factors and their roles in each relation- ship (Fig. 5). Fig. 5 — EBSD characterization of Ni coating after nanoindentation: Euler angle map. iTSSe TSS

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51 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

EDITOR Frances Richards

TECHNICAL ADVISORS OBTAINING NADCAP ACCREDITATION: Aymeric Goldsteinas HELPFUL GUIDELINES FOR PASSING Stephen Feldbauer YOUR AUDIT, PART III Valery Rudnev Nathan Durham Olga Rowan Learn how to ease the process of receiving Nadcap HTS R&D Committee accreditation for your heat treating facility by paying heed to 6 some of the challenges others have experienced. CONTRIBUTING EDITOR Ed Kubel INDUSTRY 4.0 MEETS HEAT TREATING PRODUCTION MANAGER Satyam Sahay Kelly Sukol Industry 4.0 is in the early technology evolution stage with tremendous business expectations. NATIONAL SALES MANAGER Erik Klingerman 440.338.5151, ext. 5574 [email protected] 9

HEAT TREATING SOCIETY EXECUTIVE COMMITTEE COMPUTER MODELING SINGLE-SHOT Stephen G. Kowalski, President INDUCTION HARDENING OF A POWER Roger Alan Jones, Immediate Past President TRANSMISSION SHAFT Zhichao (Charlie) Li, B. Lynn Ferguson, James Oakes, Vice President Collin Russell, and Valery Rudnev Computer modeling is used in induction hardening process 12 design to improve component quality including hardness, beneficial stress distributions, and reduced distortion. EDITORIAL OPPORTUNITIES FOR HTPro IN 2017 The editorial focus for HTPro in 2017 1 reflects some key technology areas DEPARTMENTS wherein opportunities exist to lower manufacturing and processing costs, 2 | EDITORIAL reduce energy consumption, and improve performance of heat treated 4 | HEAT TREATING SOCIETY NEWS components through continual research and development. June Testing and Process Control ABOUT THE COVER September Thermal Processing in Complex components are routinely induction hardened. Courtesy of Inductoheat Inc., On/Off Highway Applications inductoheat.com November Atmosphere/Vacuum Heat Treating To contribute an article to one of the upcoming issues, contact Frances HTPro is published quarterly by ASM International®, 9639 Kinsman Road, Materials Park, OH 44073, 440.338.5151, Richards at frances.richards@asmint- asminternational.org. Vol. 4, No. 4 Copyright 2016 by ASM International®. All rights reserved. ernational.org. The acceptance and publication of manuscripts in HTPro does not imply that the editors or ASM International accept, approve, or endorse the data, opinions, and conclusions of the authors. Although manuscripts published in HTPro To advertise, contact Erik Klingerman are intended to have archival significance, authors’ data and interpretations are frequently insufficient to be directly at erik.klingerman@asminternational. translatable to specific design, production, testing, or performance applications without independent examination org. and verification of their applicability and suitability by professionally qualified personnel. 52 FEATUREGUEST EDITORIAL

HOW TO MOVE HEAT TREAT R&D FORWARD First, use the experience and knowledge of members to identify new work and the organizations that are perform- eat treating is an easily iden- ing development pertinent to the heat treating industry. The tifiable industry and ASM’s committee must track the work from Worcester Polytechnic Heat Treating Society (HTS) Institute’s Center for Heat Treating Excellence (CHTE), for- Horganizes successful exhibits and eign universities, EWI, and from newly formed consortiums conferences. Likewise, the Metal such as LIFT (Lightweight Innovations for Tomorrow), Amer- Treating Institute organizes a suc- ica Makes (National Additive Manufacturing Innovation Insti- cessful Furnaces North America tute), and the Digital Manufacturing and Design Innovation (FNA) event every two years. Both Institute. organizations and IHEA have course Second, the information must be disseminated if work available for heat treat training. There are clear issues allowed. Bringing forward work for conference papers around energy, safety, cost, and product performance. How- and publishing in HTPro are two ways to do that. Website ever, no one receives a degree in heat treating and there are updates and other member-friendly and timely ways must few universities and national labs that boost their prestige also be utilized. and funding by investigating and solving issues around heat treatment. Lastly, research and development must be encour- aged. The Thermal Manufacturing Industries Advanced Heat treating is an applied field relying on various Technology Consortium (TMI-ATC) is a great aid in this area. aspects of mechanical engineering and materials science. It A roadmap was published showing the areas where research is an industry but not an academic field where advancements and development are needed to advance industries like heat are self-propelled by motivated researchers at universities, treating. The committee must find ways to involve more uni- institutes, and national labs competing against one another versities, national labs, and companies in heat treat related for dollars and prestige. More motivation for development ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED research. comes from companies, but declining manufacturing infra- structure has certainly slowed this development within com- panies. It is with this backdrop that the HTS Research and Michael Pershing Development Committee has laid out three key activities: HTS R&D Committee Chair 1) Identify, 2) Disseminate, 3) Encourage. Sr. Technical Steward at Caterpillar Inc.

2

Order Yours Today: www.asminternational.org/handbook4e 53 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 3 ------

Deadline for nominations for Deadline ASM’s Heat Treating Society (HTS) is currently seek is currently (HTS) Society Treating Heat ASM’s visit hts.asminterna nomination rules and forms, For in 1997 established was award The ASM HTS/Bodycote ASM Mexico Chapter leadership, from left, Vic Zacharias, left, from Vic leadership, Chapter ASM Mexico Adriana Carrasco, Carlos Zarazúa, Erika Granados, Francisco Mendez. and Fabian Michaca, ing nominations for the George H. Bodeen Heat Treating Treating H. Bodeen Heat the George ing nominations for distinguished and which recognizes Achievement Award, through treating heat the field of to contributions significant management, or engineering development of leadership, impact. commercial substantial 1, 2017. is February and Soci & Networking and click on Membership tional.org submit a nomination, or to information more For Awards. ety Miller at 440.338.5151 ext. 5513, joanne. Joanne contact [email protected]. in heat advancement that represents a paper recognize to in a substantial treating heat promotes technology, treating in managing the advancement a clear or represents way, Body by is endowed The award treating. business of heat is open The contest America. Thermal Process-North cote at univer education, or part-time in full-time all students, to stu is also open to It or colleges. equivalent) sities (or their and years three within the past graduated dents who have NOMINATIONS SOUGHT FOR FOR SOUGHT NOMINATIONS TREATING H. BODEEN HEAT GEORGE AWARD ACHIEVEMENT HTS/BODYCOTE FOR ASM SOLICITING PAPERS CONTEST TREATING IN HEAT PAPER BEST English presentations simultaneously translated to over 274 over to translated simultaneously English presentations with all reception networking and ended with a attendees compa the 43 exhibiting including those from attendees, of this new event, another one is the success nies. Due to 2018. planned for - - - - - HEAT TREATING SOCIETY NEWS SOCIETY TREATING HEAT

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The full set is a set The full Set. Heat Treating ASM’s inaugural Heat Treat Mexico conference was conference Mexico Treat Heat inaugural ASM’s Volume 4E: Handbook,ASM Volume held September 20-23, organized by the Heat Treating Soci Treating Heat the by organized 20-23, September held exceeded sold out and far completely The event was ety. - “non-metal ASM’s with started day first The expectations. Professor by in Spanish taught course metallurgy” lurgical of Nuevo Leon University Colas at the Autonomous Rafael than 125 attendees of more and eneded with a reception ASM. The 12-session to Chapter the new Mexico welcoming and with Spanish off Wednesday kicked program technical Heat Treating of Nonferrous Alloys, of Nonferrous Treating Heat is now E. Totten, George by edited gives work This singular available. - and techni analysts, engineers, on heat source cians a one-stop and guide fundamentals treating of nonfer a wide variety lines for The new alloys. handbookrous volumes the series of five completes Handbook, ASM treating, on heat 4D, 4E 4A, 4B, 4C, Volumes processes, fundamentals, treating heat ing including steel and treatment heat for selection of steels and technologies; compo steels, treated of heat and properties the processing treatment; and heat induction heating ; nents, and cast informa more For alloys. of nonferrous treating and heat tion, visit asminternational.org/handbook4e, www.asmint the ASM International or call ernational.org/heattreatset, at 800.336.5152. Center Service comprehensive reference guide to all aspects of heat treat all aspects of heat guide to reference comprehensive HEAT TREAT MEXICO DEBUTS MEXICO TREAT HEAT TO SOLD-OUT CROWD TO NEW HEAT TREATING TREATING NEW HEAT RELEASED JUST HANDBOOK 54 4 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 440.338.5151 ext. 5513,[email protected] ext. ing Society, 9639KinsmanRd., Materials Park, OH44073, missions shouldbesentto Joanne Miller, ASMHeat Treat click onMembership &Networking, andSociety Awards. For and nominationform, visithts.asminternational.org and LEADER AWARD SURFACE COMBUSTION EMERGING NOMINATIONS SOUGHTFORASM HTS/ ship &Networking, andSociety Awards. paper submission,visithts.asminternational.org, Member plaque andcheckfor $2500. To rulesfor view eligibilityand graduate or post-graduate The winner receives student. a whose paper describes work completed while an under uum andatmosphere heat treating technologies. cate themselves to theadvancement andpromotion ofvac standards for HTS participation andinspires others to dedi The award acknowledges anindividualwhosets thehighest tion ofSurface Combustion’s 100-year in2015. anniversary heat treating industry. Theaward was created inrecogni accomplishments exhibit exceptional in achievements the ing early-to-midcareer heat treating professional whose Award was established in2013to recognize anoutstand- ASM_Publish_AD_half.indd 1 m Paper submissiondeadline isMarch 1,2017. The ASMHTS/Surface CombustionEmerging Leader k w a Deadline for nominationsisApril1,2017. y Visit usonlineto learn more abouthow to start theprocess: ASM isactivelyseekingproposals inthesubjectareas ofmaterials materials science,ASMcanhelpyoubuildcredibility andrespect within yourindustry. We inviteyoutosubmitabookproposal or selection, processing, evaluationandperformance.Asaleading

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c r - - - - Buying a Heat Treatment Furnace Essential To Ask Questions Buying a vacuum or atmosphere heat-treating system is much like purchasing a new car or a home – a lot of thought, research and careful consideration should go into the decision. However, unlike buying a car or home, it might be difficult to know all of the key items you should consider before making such a purchase. Our Ipsen experts have compiled a list of 11 essential questions every furnace buyer should ask themselves before committing to a furnace, as well as a few key considerations for reducing downtime and extending the lifespan of the furnace. Call Our Sales Team Buying a Furnace 1-800-727-7625 1. What is your budget? Make sure to do International: +1-815-332-4941 some research and acquaint yourself with the general cost of different furnaces, as well as the cost of optional How to Choose the Best features, auxiliary equipment, Hot Zone for Your Needs transportation and installation. Then decide on a budget that will best meet When it comes to graphite and all-metal hot zones, your needs. it may be difficult to decide which type best fits your needs. After all, each has its own unique 2. Will your parts be processed in vacuum designs and advantages. The first post in Ipsen’s or atmosphere? blog series, A Look Inside the Furnace, will: 3. What types of processes will you run in • Examine the reasons behind the shift to the furnace? graphite hot zones 4. How many parts do you want to process • Compare the different benefits of per month? This number will help graphite and all-metal furnaces determine … • Identify three basic questions that can help users choose the best hot zone for their heat-treating system

Bit.ly/ChoosingAHotZone Read the full blog post here: Read the full Bit.ly/FurnaceBuyingConsiderations blog post here: www.IpsenUSA.com 56 6 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 verifying thedesired scope ofaccreditation, scheduling ommended for executing asuccessful theseinclude audit; performing afew aninternal bestpractices audit, are rec Nadcap audit. guarantee theprocess anddemonstrate control through a standards. The only way to guarantee quality results is to of defects and meet the aerospace industry’s highquality must be validated in advance to ensure products are free the specifiedrequirements). Therefore, theseprocesses possible to completely verify thatthefinalproduct meets considered specialprocesses (i.e., processes where itisnot tain processes, such as heat treatment and brazing, are products. and adhere qualitystandards to industry for allaerospace nents—places you inthebestpositionto consistently meet aspectinvolved inmanufacturingevery aerospace compo control over your processes andequipment—essentially EXECUTING ASUCCESSFULOFFICIALAUDIT and completing theofficialaudit. cle looks at theofficialaudit process, auditor interactions, mances, andcompleting Thisfinalarti theinternal audit. HTPro) addressed the internal audit process, nonconfor Thesecondscheduling anaudit. part (September 2016, this series (June 2016, HTPro) looked at preparing for and ing for andexecuting asuccessful The first part audit. of cusses someoftherecommended resources for prepar thatdis daunting, aseriesofarticleshasbeendeveloped products. Whilepreparing for aNadcap auditcan seem high-qualitystandardssistent, for producing aerospace heat treating andotherspecialprocesses adhere to con are operating underaspecifiedstate ofcontrol objective activitydesignedtoindependent, verify thatyou in theNadcap accreditation process. Theofficialauditisan necessary documentation, theofficialauditisnext step A OBTAINING NADCAP ACCREDITATION: HELPFUL GUIDELINES In additionto preparing for theauditprocess and Close control ofyour processes isimportant ascer After performing an internal audit and submittingthe roles inensuringthatmanufacturers performing and theNadcap accreditation process playkey erospace Material Specification (AMS) standards Learn how to simplifytheprocess ofobtaining Nadcap accreditation for your heat treating facility by paying heedto someofthechallenges others have experienced. FOR PASSING YOUR AUDIT, PART III FEATURE Ipsen USA, Cherry Valley,Nathan Durham,IpsenUSA, Cherry Ill. [1] . Having ------Scheduling is crucial during the official audit. Inmost Scheduling iscrucialduring theofficialaudit. choose to talk withoneofthemduringtheofficialaudit. role in making the audit successful as the auditor may the auditprocess andconfirm understand thatthey their Itisalso importantequipment. to inform allpersonnel of day processes, aswell asthosewhoregularly operate the typically includethosemostknowledgeable aboutday-to- available duringtheofficialauditprocess. Key personnel ant to have personnel whoperformed theinternal audit nies thathave undergone itisimport aNadcap audit, finished verifying thescope. not remove oraddanyaccreditations once theauditor has the auditprocess. Itisalsoimportant to note thatyou can against are whattheauditor willgo over indetail during standards andspecifications you selected to beaudited mitted whenschedulingtheaudithasnotchanged. The the auditor isverify thatthescope ofaccreditation sub oneofthefirst thingsyouofficial audit, typically dowith schedule considerations. key personnel, andinforming theauditor inadvance ofany Images courtesy ofIpsen. specification checklists andbothhistorical and live jobs. auditor willspend asignificant portionoftimereviewing During theProcess segment the oftheNadcap audit, Informing theauditor ofschedule considerations: Scheduling personnel: According to somecompa- Verifying thescope ofaccreditation: When starting the

- - - 57 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 7 - - - - - FEATURE Based on discussions with aerospace suppliers and suppliers Based on discussions with aerospace step and most important findings. The first Reviewing Recommended methods for interacting with the interacting for methods Recommended pared, regardless of when the auditor wants to to wants of when the auditor regardless pared, audit, or job any avoid helps area review a certain delays in the audit process. . of a specification interpretation Explaining your how explain need to may be times when you There recommend Others a specification. interpreted you and procedures, documented data, having collected In discussions. on hand for additional information for an explanation provide addition, being able to not only helps you way do things a certain why you - specifica of various the nuances understand better decide if any refinements tions, but also helps you process. be made in your need to The auditor’s time is time is The auditor’s time. the auditor’s Balancing Because and shop floor. the office divided between review to the auditor days for only a few are there - con can job audit everything, each and because a daily provide to sume a lot of time, it is helpful being run and what are of when loads reminder Being pre available. are personnel times certain information from PRI, it is recommended that you fol that you PRI, it is recommended from information of the official audit, after regardless steps the proper low identical nearly are These steps or fail. pass you whether audit, the internal but with a few after those followed to differences. key you sure and make all findings with the auditor review is to do if you because is vital one. This step each understand will not be a finding, you received why you not understand the audit is action. After the corrective determine able to all findings, making sure to must respond you concluded, include: to FINISHING THE AUDIT PROCESS FINISHING THE AUDIT • understanding of specifications to reviewing findings. A reviewing to specifications of understanding informa credible is providing audit process of the part key as well as is controlled, the process on how tion and data auditors Nadcap manner. concise it in a clear, explaining and identify nonconformances to trained extensively are stan set the within specifications all to adherence ensure with the received you Discussing nonconformances dards. all aspects of the understand better to enables you auditor it. received as why you finding, as well executing for reasons your include presenting auditor manner in a factual way a certain process a particular specification a certain interpret you and discussing how might have any misunderstanding where determine to best prac key a few keep to it is vital We found occurred. are with the auditor interactions ensure in mind to tices including: and professional, calm • - - occurs in various ways ways in various occurs is approximately one day one is approximately The official audit is generally divided into two seg two divided into The official audit is generally The Quality System Audit The Quality System is approximately four days long. four is approximately Audit The Process with the auditor Interacting It is important to inform all personnel of the audit process of the audit process all personnel inform to It is important in making the their role that they understand and confirm with one of talk may choose to as the auditor audit successful them during the official audit. ments—the Quality System Audit and the Process Audit. and the Process ments—the Audit Quality System long. According to Performance Review Institute (PRI), the Review Institute Performance to long. According sufficient provided this audit if you will not perform auditor when scheduling quality system of an acceptable evidence quality system, the audit. an acceptable do not have you If Audit, which the Quality System will perform the auditor a for requirements the all meet you that verifying involves quality specification. depend- be longer, could segment the Process However, being are which you ing on the number of Primes for factors. other and accreditation, of scope the accredited, portion of time spends a significant the auditor Typically, and checklists and both historical specification reviewing of both should be available number jobs, so a large live Auditors website). review (as defined on the eAuditNet for jobs besides the ones historical different request typically job audits. live as perform as well prepared, discussing your from the official audit process, throughout THE AUDIT PROCESS THE AUDIT cases, the auditor is required to be on-site for four to five five to four for be on-site to is required the auditor cases, the audi inform to required are you days. Therefore, full which of the audit about the Primes for at the start tor is scheduled as what as well be approved, to want you are days (e.g., if there few the next over with production cycles). This enables the auditor furnace any upcoming maximizing while processes your evaluate effectively to productivity. 58 8 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 • • • • • • can affectandusingmore yourthanthe30extra merit, if more timeisneeded.However, usingtheseextra days four total responses allowed. Thirtyextra daysare allotted calendar daysto submiteach subsequent response with response concerning anyfindings.You thenhave seven from theendofofficialauditto submityour initial is alsoimportant to note thatyou have 21calendar days the corrective actionwas implemented. include thetraining schedulethathasbeenfollowed since operator training ataspecificfrequency. You should also ator training, thecorrective actionwould beto provide improperly located load thermocouples isalackofoper ple, ifyou determined thattheroot cause ofafindingfor the issueandcite thetimingofimplementation. For exam action, you shoulddefinetheresolution madeto address performing root-cause analysis.Inmaking acorrective essential part oftheofficialauditprocess. but knowing how to perform root-cause analysisisan necessarily mean thenumberoffindingswillbereduced, ultimate root cause. Havingasimilarroot cause doesnot can sometimes begrouped together, dependingonthe better understand how to identifythem asrelated findings root-cause training PRIoffers; thistraining will help you a recommended bestpractice isto take advantage ofthe cal to thesteps However, appliedduringtheinternal audit. forming root-cause analysisfor theofficial auditisidenti Objective evidence Action taken to prevent future reoccurrences Date ofcorrective actionimplementation Corrective actiontaken Product impact ofallnonconformances Root cause ofthenonconformance When going through thesesteps it after theaudit, Applying corrective actions.This Performing root-cause analysis. The process of per FEATURE is thenext step after - - - - ponents you process. enables you to enhance thequalityandsafety ofthecom audits. Continuallyrefining your processes andmethods ultimately helpscontribute to your success onfuture tion process, aswell asareas thatcould userefinement, CONCLUSIONS Performance Review Institute, p37,2013. 2. P. Evans andE.Jacklin,Nadcap SupplierTutorial, learn-about-quality/auditing. 1. American Society for Quality, asq.org/ References ipsenusa.com. 1), IpsenUSA, Valley, 984IpsenRd., Cherry IL61016, contact [email protected] or 844.464.7736(select solutions manager atIpsen.For technical information, For more information: NathanDurhamisanelectrical cessful experience each time.~HTPro your audit process will contribute to a positive and suc continuallyor 10thNadcap audit, refining anddeveloping refine andimprove theirprocesses. Whether itisyour first use theseproducts, butalsohelpscompanies continually tation process notonlyhelpsensure thesafety ofallwho ensure aircraft andtraveler safety. TheNadcap accredi that Primeshave established global qualitystandards to of theaerospace industry. Itisimportant to remember pliers successfully adhere to thehighqualitystandards set specifications. play a key They role in ensuring sup standards and noting any findingsthatdonotadhere to to anauditfailure days (ormore thantheallotted four responses) could lead Identifying successful practices from theaccredita Auditors are tasked withevaluating aspecificset of [2] . - - - - - 59 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 9 ------—mainly driven heuristically FEATURE Further, identifying the location of specific components components of specific identifying the location Further, connected gear-making process is illustrated in Fig. 3. Data in Fig. 3. Data is illustrated process gear-making connected which is typically operations, treating heat from collected pro to be leveraged purposes, would quality audit used for and post-op pre- improved sharing for data vide part-level chemical example, for data, of specific Transfer erations. could mill and the casting, the steel from data composition carburiz and annealing, reheating, of control better provide and man help mitigate would which in turn ing operations, components. in these precision distortion age design recipes better help to would type operations in batch Such individualized machining and finishing operations. for bring a transformational level would solutions at the part level. One of the big at the product quality control to change be with rec would operation treating in the heat changes gest is now which ipe management, and production amount of significant The trial and error. by models would mathematical with their together quality data treating heat and self-evolving develop self-learning help to and quality needs production current for suitable recipes, and health furnace of the current with due consideration Key business drivers for Industry of ThingsFig. 2 — Key for business drivers 4.0, or Internet industrial revolution. the fourth (IoT), - - INDUSTRY 4.0 MEETS HEAT TREATING MEETS HEAT 4.0 INDUSTRY John Deere Technology Center India, Pune Center Technology John Deere FASM,* S. Sahay, Satyam

Industry 4.0 is in the early technology evolution stage with tremendous business expectations. with tremendous evolution stage Industry technology 4.0 is in the early Four industrial revolutions in human civilization. Four

Key business drivers for this revolution include a higher this revolution for business drivers Key of Industry impact significantly 4.0 will emergence The Physical and virtual connectivity across product product across connectivity and virtual Physical development cycles including engineering, synergies, Multifunctional support and customer quality, manufacturing, - data connected from Higher level of intelligence models, which could and process products, bases, decisions and autonomous informed more to lead developed within the intelligence with self-learning organization ndustry 4.0, or Internet of Things (IoT), is an emerging of Things (IoT), ndustry or Internet 4.0, and is arena, in the manufacturing trend technology (Fig. 1). industrial revolution fourth the widely considered level of efficiency and quality achieved through individual- levelefficiencyof achievedthrough quality and level, or machine better component solutions at the ized the supply chain, across production of networked leverage (Fig. 2). In addition, equipment maintenance and proactive - knowl organizational on placed be will emphasis significant time. development over edge change The most significant as well. operations treating heat fromchanging i.e., mindset, current the in change a be will con to process treating silo view of the heat the current A operation. production of the connected sidering it part sioned, is characterized by: sioned, is characterized • • • IoT, where convergence of the virtual and real world is envi world real and of the virtual convergence where IoT, Fig. 1 — Integration of heat treating operations into the process chain for gear-making. chain for the process into operations treating of heat Fig. 3 — Integration

*Member of ASM International I 60 10 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 rationalization. obtained from different recipes indicate thepossibilityof recipe Fig. 5—Overlappingfrequency distributionsofqualitymetrics Fig. 4— INDUSTRY 4.0:HEAT TREATING STORY BOARDS operationally qualityproducts. efficientwithrobust, vision, thesechanges would alsomake heat treating more operating condition. Alignedwiththeoverall 4.0 Industry capabilities for heat treating recipes to become rationalized ating condition. Thesystem would alsohave self-evolving on thecurrent andfurnace part chemistry health andoper (Fig. 4).Thiswould alsoenablerecipe customization based tion ofrecipes withfeedback from historical qualitydata self-learning algorithms would enablecontinuous evolu part, whichwould eliminate mistakes inselection.Further, be accomplished through image recognition algorithms of a andmanaged.developed Recipe selectionwould primarily most significant impact onhow heat treating recipes are of production. 4.0would Itisexpected have the thatIndustry significant amountofrework and reject at initial stages levels recipe selectionfor parts new isalsoheuristic,resulting ina tions—continues to be heuristically Furthermore,developed. treating recipe—which isthecore ofheat treating opera furnace technology andautomation have occurred, theheat and intelligence capabilities, andbusinessvalue: with key characteristics ofsensing,connectivity, analytics for heat treating operations, describedinanIoT framework Recipe management: Althoughsignificant Recipe changes management: in Three 4.0willnow examples beillustrated ofIndustry Self-learning algorithms andintelligence created for autonomous recipe rationalization, selection,management, andfine-tuning. FEATURE - - - loads. opportunity to control distortion byfine-tuning recipes for specific range)chemistry onheat treating distortion, whichpresents an Fig. 6—Influence ofsteel chemical composition (withinspecified Further, dependingonquench-tank conditions andfurnace instantaneous recipe created incorporating thisinformation. the composition isknown attheheat treating step, andan control ofdistortion could ifinformation beachieved on directly linked to hardenability anddistortion. Significant agement strategies. For example, chemical composition is processing steps, whichprevents efficientdistortion-man reason for distortion isinadequate information atdifferent burizing andquenchingconditions impact distortion. Akey and forging, annealing andmachining conditions, andcar (Fig.6),processchemistry parameters duringreheating cant heat treating challenge. Critical parameters including mission components, suchasgears andshafts,isasignifi- robust product quality. opment to create value in terms of efficient operations and conditions; and long-term rationalization and recipe devel the recipe based oninstantaneous inputsandoperating correct reference recipe; intelligence capability to fine-tune furnace; connectivity andanalyticscapability to choosethe sensing capability for part shape,quantity, andweight inthe 4.0framework,dictable. heat IntheIndustry treaters need: ations willbemore efficientandproduct qualitywillbepre could bebetter managed. Consequently, heat treating oper decision dueto production disruption inpre- orpost-steps (Fig. 5)over timedueto changes inproduct mix.Anyrecipe Distortion control: Distortion control in precision trans ------61 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 11 ------FEATURE Industry 4.0 is in the early technology evolution stage evolution stage Industry technology 4.0 is in the early with tremendous business expectations and significant business expectations with tremendous - orga Few the technology. pursue to available grants research using and for in identifying cases the lead taken have nizations is nearly while the IT infrastructure applying this technology, lies in identifying val The challenge implemented. be to ready ue-driven use cases, which could impact efficiency and prod impact which could ue-driven use cases, an additional treating, of heat In the area and quality. uct cost of understanding deep a with talent finding be will challenge domain, treating and the industrial heat metallurgy physical into this understanding convert the ability to in addition to lever that intelligence and self-learning analytics, algorithms, of this the future need for The immediate IT systems. age is development of such interdisciplinary technology emerging obsta be the biggest (Fig. 8), which could engineering skillsets ~HTPro of this technology. scale-up successful cle to Fel S. Sahay is a John Deere Satyam information: more For Center Technology engineering, John Deere materials low, Mag- Cybercity, XIV, Tower India Pvt.India, John Deere Ltd., 411 013, India, [email protected]. Pune City, arpatta undergoing maintenance after a fixed time (Fig. 7). This time a fixed after maintenance undergoing under furnaces with operation, in suboptimal results often In the Industry late. 4.0 or too early too maintenance going temperature-time furnace for capability sensing framework, cycle after response such as the heat-up is needed, response moni skin temperature with together is loaded, a charge help to would and analytics capability Connectivity toring. basket and charge as such parameters, influencing identify burner health. for capability intelligence weight, provide to require and burner maintenance furnace trigger This would with maintenance of proactive in terms value create ments to The Industry reduction. 4.0 and energy efficient operation the mainte connect to architecture also provides framework either through alert systems, appropriate through staff nance solutions. or mobility and wearable system a computer CONCLUSION - In a heat treating shop with a shop with treating In a heat maintenance: Furnace Composition information and oil-quench tank furnace of both The health location Part - hard predict to capability Connectivity and analytics enability and distortion on based fine-tune recipes to capability Intelligence inputs instantaneous conditions Operating to finishing conditions Deriving location-specific - in preci distortion of mitigating in terms value create sion components battery of furnaces, the maintenance schedule is designed the maintenance of furnaces, battery with specific furnaces on a time interval, predominately Interdisciplinary skills needed to successfully leverage Industry 4.0 in the context of heat treating. of heat Industry leverage context 4.0 in the successfully Fig. 8 — Interdisciplinary skills needed to Time-based, staggered furnace maintenance schedule, maintenance furnace staggered Fig. 7 — Time-based, into a on efficiency if transformed impact which has a significant schedule. health-based furnace health, machining steps prior to could be fine- could carburizing prior to machining steps health, distortion manage and better distortion anticipate to tuned on the location depending product.in the final Furthermore, could finishing operations step, in the carburizing of the part dis having highly predictable specific, thereby be made part tortion in the product. Industry In the tortion sensing 4.0 framework, for: is required capability • • • • • • • 62 12 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 T hardness pattern, and production rate. The design must take workpiece geometry, temperature uniformity, required diameter andundercuts. modate workpiece geometrical features, suchaschanges in relieving selected regions ofthecopper inductor to accom half circumferential. Longitudinal leg sectionsare profiled by exception iscrossover segments where eddycurrent flow is eddy currents primarilyflow alongthelengthofpart.An cle onlyhalfoftheworkpiece circumference, andinduced legs andtwo crossover segments. Crossover segments encir for stepped inductor shafts.Asingle-shot consists oftwo distortion better thanscan andstatic hardening, particularly inductorsSingle-shot entire region to behardened isheated atthesametime. than theshaftorcoil moving relative to each other. The methods. method, Inthesingle-shot thepart rotates rather induction surface hardened using scanning and single-shot mize distortion. parameters andcoil design to prevent cracking and mini fields shouldbeevaluated to determine appropriate process form hardened patterns. Eddycurrent flow andtemperature ble size, andotherirregularities can produce severe nonuni and singleshothardening routinely usedare scan, continuous orprogressive, static, using inductionhardening (Fig.1).Four inductionmethods components withcomplex shapesare surface hardened changes, undercuts, teeth, splines,andmore. Manyofthese or transverse holes,grooves, shoulders, flanges, diameter ing incomplex geometries containing longitudinal and/ componentNew designsinvolve material removal result *Member ofASMInternational with large shoulders, multiple liquation, andcracking. For example, scan hardening shafts distortion, undesirable microstructures, grain boundary perature hotandcold deviations, spots,excessive shape netic fieldgenerated by aninductor, whichcan cause tem Inductor configuration dependsonfactors suchas Steel shaftsandshaft-like components are traditionally Irregularities incomponent geometry distort themag Zhichao (Charlie)Li*andB.Lynn Ferguson, federal Corporate Average Fuel Economy regulations. ing initiatives invehicle designto meet more stringent he automotive isimplementinglightweight industry Collin Russell*andValery Rudnev, FASM,* Inductoheat Inc.,MadisonHeights,Mich. Computer modelingisusedininductionhardening process designto improve component HARDENING OFAPOWER TRANSMISSIONSHAFT COMPUTER MODELINGSINGLE-SHOT INDUCTION quality includinghardness, beneficialstress distributions,andreduced distortion. typically control hardness pattern and [1] . diameter changes FEATURE of apprecia------FASM,* Dante and SolutionsInc.,Cleveland, to coil profile. Single shot hardening isalsothepreferred densities, and workpiece positioning is critical with respect care infabrication because itusuallyoperates athighpower part to beheated. Thistypeofinductor requires themost machined from solidcopper to conform to thearea ofthe inductor profile mightbecumbersome andtime-consuming. inductor-to-workpiece gap. Determining theappropriate tor section,applyingfluxconcentrators, andby varying the adjusting thecurrent-carrying face oftheappropriate induc heating. Required heat source control can by beachieved produce heat surplusesand/or heat deficitsuponinduction into account thetendency ofcertain geometrical features to tinely inductionhardened. Fig. 1— For critical applications, inductors single-shot are CNC Variety ofcomplex components geometry thatare rou-

- 63 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 13 . - - - - - [3]

(b) ), finish tem ), martensite s FEATURE ), transformation strain, and coefficients of ther and coefficients strain, ), transformation f (a) perature (M perature mal expansion (CTE) for austenite and martensite. Because and martensite. austenite for (CTE) mal expansion in diameter. Phase transformations occur during induction occur Phase transformations in diameter. trans of the part quenching. The surface and spray heating forms to austenite during heating, and during quenching, during heating, austenite to forms or mar bainite, pearlite, ferrite, to transform can austenite descriptions Accurate rate. depending on the cooling tensite of properties and mechanical of phase transformations analysis thermal stress for required individual phases are Figure 2(a) shows the TTT diagram of 4140 generated from of 4140 generated TTT diagram the 2(a) shows Figure is not used in Dante The TTT diagram database. the Dante phase transformation analytical the but models directly, information. TTT diagram all contain models and database curve during marten strain a dilatometry 2(b) shows Figure The curve provides cooling. under continuous formation site (M temperature start the martensite Finite element models: (a) electromagnetic model used element models: (a) electromagnetic Fig. 3 — Finite model used by Dante. and (b) 2D axisymmetric by Flux-3D, (b) - - - - -

. [2] austenitization is complete, or after a short delay. delay. a short or after is complete, austenitization Consider a case study of induction hardening of an AISI of induction hardening study Consider a case Today, most software programs are not capable of not capable are programs most software Today, The current production environment does not allownot does environment production current The 4140 alloy steel shaft with shoulders and numerous changes and numerous shaft with shoulders steel 4140 alloy suming, and difficult or impossible to resolve experimentally. experimentally. resolve suming, and difficult or impossible to interrelated different of how Simulation enables prediction and final the transitional impact could factors and nonlinear It also helps component. of the heated thermal conditions process improve to must be accomplished what determine rec process the most appropriate establish to effectiveness when factor comfort a provides modeling Computer ipes. short surprises, unpleasant avoids designing newsystems, development time. curve,ens the learning and reduces FEA software However, modeling single shot hardening. propri with Solutions in combination Dante developed by Inductoheat developed by Flux-3D for subroutines etary of the features all critical consideration into enable taking process induction hardening the luxury of process design via trial and error. Computer error. and trial via design luxurythe process of quickly specialists to simulation enables induction heating time con be costly, which could details, process determine MODELING INDUCTION HARDENING OF A STEEL SHAFT OF A STEEL COMPUTER MODELING SPECIFICS after ately a of a fraction from range of quench delay can The duration of the depending on the geometry seconds a few to second hardnessand composition, chemical material component, specification. pattern (a) database. Dante from generated AISI 4140 for curve transformation (a) and dilatometry strain (b) of martensite Fig. 2 — TTT diagram are rates production times/high heat shorter when choice but is seconds, be as short as two time can Heating desired. is critical Sufficient rotation eight seconds. to four typically per rotations 10 full design; at least with single-shot inductor immedi begin quenching can Spray cycle is desired. heat 64 14 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 MODELING USINGDANTE STRESS ANDPHASE TRANSFORMATION MAPPING FROM FLUX-3DTO DANTE meshes were usedfor theFluxandDante models. using apolymersolutionwithoutdelay. Different finite element Fig. 3(b).After inductionheating, theshaftwas spray quenched mation, andstress analyses;theDante meshisshown in mapped into theDante modelfor thermal,phasetransfor Calculated power distribution from the Flux-3D model was heating stages. Thefinite elementmodelisshown inFig.3(a). and 3Dheat source distributionwas obtained atdifferent transformation inthisstudy isaustenite to martensite. the cooling rate duringspray quenchingissevere, themain radial displacement, andhoopstress distributionsafter two and Dante reveals good correlation (Fig.4). A comparison oftemperature profiles projected by Flux-3D element mesheswere usedintheFlux-3D andDante models. mapping subroutine was because developed different finite was mappedinto theDante heat treatment model.Aspecial Power distribution in terms of time predicted by Flux-3D tion, andstress duringheating evolution andquenching. used inDante to modeltemperature, phasetransforma circumferentially a2Daxisymmetric intheshaft, modelwas 25 full rotations duringtheheating cycle. a total heating timeoffive seconds, whichtranslates into inductor witharotation rate offive rotations/second, and the hardening process, theshaftwas positionedinsidethe determined to address changes inshaftgeometry. During appropriate locations for magnetic fluxconcentrators were Using Flux-3D, theelectromagnetic problem was solved Temperature, austenite pattern, axial displacement, Copper inductor profiling was optimized andthemost Because temperature distributionisrelatively uniform Fig. 4—Predicted temperature distributionsbetween Flux-3D and Dante during inductionheating at2s(a)and 5s(b). (a) FEATURE

- -

(b) ual stress distributionaffects shaftfatigue performance. after theshaftcools to room temperature (Fig.9).Resid +450 MPa atthecase-core location, and+150MPa inthecore Hoopstresses arein theshaft. −700MPa atthesurface, pleted hasasignificant effect onthechange instresses compression of-80MPa. under theaustenitized layer, andthecore isunderslight compression, atensile stress of about390MPa isobserved 306°C. Hoopstress onthesurface isabout−310MPa under temperature isabout70°Candcore temperature isabout austenite layer transforms to martensite (Fig.8).Thesurface formation. thermal shrinkage caused by quenchingpriorto martensite nies martensite formation. Surface stress istensile dueto compression dueto thevolume expansion thataccompa on thesurface (Fig.7).Surface stress shiftsfrom tension to 15 KW/(m using a6%polymersolution;convection coefficient of radial displacement oftheheated region isabout0.2mm. 5 mmdeep. Surface temperature isabout1100°C,andthe seconds ofheating; theaustenite layer isapproximately in thecore to balance thestress. austenite layer dueto thermal expansion, with tensile stress a magnitude close to neutral. Compression occurs under the the surface transforms to austenite, thestress decreases to face isundercompression dueto thermalexpansion. After heating before thesurface transforms to austenite, thesur seconds ofheating are shown inFig.5.At theearly stage of M ing, surface temperature isabout204 to represent thespray quench.After two seconds ofquench s (320°C)of AISI 4140,and martensite formation started Cooling ofthecore after phasetransformation iscom At about10.4seconds ofquenching,almost allofthe After heating iscomplete, theshaftisspray quenched Figure 6shows predicted results attheendoffive 2 K) isappliedontheshaftsurface oftheFEAmodel °C, which is below the °C, whichisbelow the - - - - -

65 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 15

(e) (e) (d) (d) FEATURE (c) (c) (b) (b) (a) (a) (a) Temperature, (b) austenite phase, (c) axial displacement, (d) radial displacement, and (e) hoop stress distributions at displacement, and (e) hoop stress phase, (c) axial displacement, (d) radial (b) austenite (a) Temperature, Fig. 6 — 2 s of heating. (a) Temperature, (b) austenite phase, (c) axial displacement, (d) radial displacement, and (e) hoop stress distributions at displacement, hoop stress and (e) phase, (c) axial displacement, (d) radial (b) austenite Fig. 5 — (a) Temperature, 5 s of heating. 66 16 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 10.4 s of quenching. 10.4 sofquenching. Fig. 8—(a)Temperature, (b)austenite phase,(c)martensite and (e)hoopstress phase,(d)axialdisplacement, distributionsat 2 sofquenching. Fig. 7—(a)Temperature, (b)austenite phase,(c)martensite and(e)hoopstress phase,(d)axialdisplacement, distributionsat (a) (a) FEATURE (b) (b) (c) (c) (d) (d) (e) (e)

67 ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 17

(e) (440) 234-8477, charlie.li@ (d) FEATURE References Hand - ASM 4C, , Vol 1. Induction Heating and Heat Treating eds., ASM Intl., 2014. Rudnev G. Totten, and book, V. al., Development of a Carburizing and 2. D. Bammann, et Carbu- Model for A Material Quenching Simulation Tool: Proc. Phase Transformations, Undergoing rizing Steels , of Distortion on Quenching and Control 2nd Intl. Conf. p 367-375, 1996. Needs for Data and A. Freborg, 3. Z. Li, B. Ferguson, MS&T Proc. Parts, of Steel Treatment Modeling Heat , p 219-226, 2004. Conf. Solu- Zhichao (Charlie) Li, Dante information: more For tions Inc., Cleveland, OH 44130, dante-solutions.com, www.dante-solutions.com. dante-solutions.com, (c) - - (b) (a) Years of experience, leveraged by advancements in advancements by leveraged experience, of Years tiveness of applying computer simulation during the design of applying computer tiveness processes. induction hardening for and development stages curve, development the learning reducing This shortens design and process inductor time and enabling accurate ~HTPro optimization. high performance computers, have improved the cost effec the cost improved have computers, high performance end of quenching. CONCLUSION Compressive residual stresses are preferred on the surface. on the surface. preferred are stresses residual Compressive stresses tensile compression, surface balance to However, fail to which may lead the core, or at under the case exist (a) Temperature, (b) austenite phase, (c) martensite phase, (d) axial displacement, and (e) hoop stress distributions at the phase, (d) axial displacement, stress and (e) hoop phase, (c) martensite (b) austenite Fig. 9 — (a) Temperature, metallurgical exhibits locations those at material the if ures or is not clean) (e.g., material irregularities or microstructural on based optimization high. Process is too if the applied load the stress optimize to factor modeling is a critical computer distribution in specific applications. and hardness ECM TREATED GEARS DRIVE THE WORLD Low Pressure Vacuum Carburizing Systems

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73 Shipley Jur Dennies Demarest Lundquist the News Members in Members

Dupont Firrao Dalley Knauss Holdford

73 the News Chapters in Chapters Akyuz Ulvan Parrington Hartfield Subramanian Ross Lane Mueller Wang Vanderlinde 72

- - Committee Volunteerism Volunteerism Tim Lundquist, Ted William Vander Cheryl Hartfield,

NEWS 71 manager– Erhan Ulvan,

Women in Women in Engineering and Canada) | F 440.338.4634 | E [email protected] | W asminternational.org and Canada) | F 440.338.4634 | E [email protected] Submit news of ASM and its members, chapters, and affiliate societies to Frances Richards, editor, ASM News | ASM International ASM News | ASM International editor, Richards, Frances to societies and affiliate chapters, Submit news of ASM and its members, OH 44073 | P 440.338.5151 ext. 5563 | F 440.338.4634 | E [email protected] Park, | Materials 9639 Kinsman Road in U.S. OH 44073 | P 440.338.5151 ext. free 0 or 800.336.5152 ext. 0 (toll Park, Materials Road, at 9639 Kinsman ASM International Contact

account manager–industry, Schaeffler manager–industry, account

- transi chief–technology FASM, Knauss, Lee 69 ASM

senior member of technical staff, staff, senior member of technical Sam Subramanian, team lead–metallurgy and failure anal- and failure lead–metallurgy Akyuz, team Burak failure analyst, failure Holdford, Rebecca Donato are positions member board to Appointed executive director, Maxim Integrated, Integrated, Maxim director, executive Wang, Zhiyong ASM Affiliate Board Members Board - ASM Affili five with their Rules of Governance, n accordance and officers their elections for completed have Societies ate the welcoming join us in 2016. Please for members board NEW OFFICERS AND BOARD MEMBERS AND BOARD OFFICERS NEW ASM AFFILIATE ANNOUNCE SOCIETIES AFFILIATE ASM ysis, Applied Technical Services Inc., FAS president, and Inc., FAS Services ysis, Applied Technical Dupont, Pierre Belgium, FAS vice president, are pleased to welcome the welcome to pleased president, are vice Belgium, FAS principle engineer, Shipley, Roch Board. FAS inaugural appointed Inc., was Analysis and Consulting Professional Professional engineer, senior Lane, and James F. treasurer Serv secretary. appointed Analysis and Consulting Inc., was succeeds as president of EDFAS while EDFAS of as president succeeds past as immediate on the board CDH Consulting, remains president. Demarest, president, J. James vice elected is IARPA, tion, and officer, finance IBM, is elected E.I.T., Operations, and Secure of Safe director–Office linde, FASM, serve a two-year Officers secretary. is reappointed IARPA, term. a two- for the board to elected was NXP Semiconductors, chair of ISTFA. as general term year is president past ing as immediate Inc. Group Acuren engineering and laboratories, and di Torino Politecnico professor, FASM, Firrao, terms); (one-year ED&T Corp. chief engineer emeritus, Jur, and NTSB, engineer, research materials Erik Mueller, ASM Failure Analysis Society ASM Failure ASM Electronic DeviceASM Electronic Analysis Society Failure following appointments. following In This Issue

manager, Analysis and Test Analysis and Test manager, Ross, and Ryan consultant, elected were Laboratory, Propulsion NASA Jet Laboratory, term. a four-year for board the EDFAS to I 70 HIGHLIGHTS ASM AFFILIATE BOARD MEMBERS

Roger A. Jones, corporate president, Solar Atmo- spheres Inc., remains on the board as immediate past president. Hannah M. Noll, superintendent, Bakers Powder Operations, ATI Specialty Materials, was reappointed young professional board member and Blake M. Whitley, Colo- Grice Kelly Kowalski Oakes rado School of Mines, was appointed student board mem- ber. Both are one-year appointments. ASM International Metallographic Society IMS president Jaret J. Frafjord, laboratory director, IMR Test Labs–Portland, announced the appointment of Mike Keeble, US labs and technology manager, Buehler, as an IMS director for one year, filling an unexpired term. Cryderman Powell Rowan Wingens Rachel Lukas, University of Pittsburgh, was appointed as a student board member for one year. ASM Thermal Spray Society The TSS electorate elected a vice president and three directors to the board; the TSS executive commit- tee appointed two student board members; and the pres- ident-elect appointed a secretary/treasurer. See page 3 of iTSSe in this issue for the full story. Jones Noll Whitley Frafjord ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED Seeking Applicants for SMST Fellowship The International Organization on Shape Memory & Superelastic Technologies (SMST), an affiliate society of ASM International, is seeking applications for the 2017 SMST Fellowship. The intent of the fellowship is to provide a current use gift to a deserving graduate student(s) with the purpose of initiating interest in a unique path of research for Keeble Lukas shape memory materials such as Nitinol. The award, which is financially supported in 2017 by Edwards LifeSciences, includes a stipend up to $50,000. The recipient will present Ron Parrington, FASM, director–industrial services, ESI Inc. research results at the 2019 SMST Conference to be held (two-year terms), and Amber Dalley, director of business in Constance, Germany. Application deadline is January 9, development–materials and environmental, RJ Lee Group, 2017. For more information visit http://bit.ly/29pjIkD or and Daniel P. Dennies, FASM, principal, DMS Inc. (three- contact [email protected]. year terms). Daniel Grice, senior materials engineering, Materials Evaluation and Engineering Inc., was appointed emerging SEEKING NOMINATIONS professional board member and Sean M. Kelly, Worcester FOR NEW EDFAS AWARDS Polytechnic Institute, was appointed student board mem- EDFAS is pleased to announce two new awards to recog- ber. Both are one-year appointments. nize the accomplishments of its members. The awards will be given annually, with the inaugural EDFAS Lifetime Achieve- ASM Heat Treating Society ment Award and the EDFAS Presidents Award being pre- HTS president Stephen G. Kowalski, president, Kow- sented at ISTFA 2017. Deadline for both awards is March 1, alski Heat Treating Co., and HTS vice president, James P. 2017. For more information, visit asminternational.org/web/ vice president business development, Super Sys- Oakes, edfas/societyawards. Nominate a worthy colleague today! tems Inc., welcome the following new members to the HTS board for a three-year term: Robert Cryderman, research EDFAS Lifetime Achievement Award associate professor, Colorado School of Mines; Joseph The EDFAS Lifetime Achievement Award was estab- Powell, president, Akron Steel Treating Co.; Olga Rowan, lished by the EDFAS Board of Directors in 2015 to recognize senior engineer, Caterpillar Inc. Thomas Wingens, director, leaders in the EDFAS community who have devoted their Wingens International Industry Consultancy, was appointed time, knowledge, and abilities to the advancement of the to a one-year term to complete an unexpired term. electronic device failure analysis industry. 71

WOMEN IN ENGINEERING HIGHLIGHTS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

EDFAS President’s Award Annual ASM Award Nominations The EDFAS President’s Award shall recognize excep- due Feb. 1, 2017 tional service to EDFAS and the electronic device failure The deadline for the majority of ASM’s awards is analysis community. Examples of such service include com- February 1, 2017, and we are actively seeking nominations mittee service, service on the board of directors, organiza- for all of these awards, a few of which are listed below: tion of conferences or symposia, development of education • Edward DeMille Campbell Memorial lectureship courses, and student and general public outreach. While • Distinguished Life Membership any member of EDFAS is expected to further the Society’s • William Hunt Eisenman Award goals through service, this award shall recognize those who • Gold Medal provided an exceptional amount of effort in their service • Silver Medal to the Society. For complete rules and nomination forms, • visit edfas.org, click on Membership & Networking and then Bronze Medal Society Awards or contact Joanne Miller at 440.338.5151 • Historical Landmarks ext. 5513, [email protected]. • Honorary Membership Deadline for both awards is March 1, 2017. For • Medal for Advancement of Research more information, visit asminternational.org/web/edfas/ • Allan Ray Putnam Service Award societyawards. • Albert Sauveur Achievement Award • Albert Easton White Distinguished Teacher Award Nominations Due for 2017 • J. Willard Gibbs Phase Equilibria Award ASM Nominating Committee View rules and past recipients at asminternational. ASM International is seeking members to serve on org/membership/awards. To receive a unique nomination the 2017 ASM Nominating Committee. The committee will form link, contact Christine Hoover at christine.hoover@ select a nominee for 2017-2018 vice president (who will asminternational.org. serve as president in 2018-2019) and three nominees for trustee. Committee candidates may only be proposed by a Chapter through its executive committee, an ASM commit- WOMEN IN ENGINEERING tee or council, or an affiliate society board. Nominations This new profile series introduces leading are due December 15. For more information, contact Leslie materials scientists from around the world Taylor at 440.338.5151, ext. 5500, leslie.taylor@asminterna- who happen to be females. Here we speak with tional.org, or visit asminternational.org/about/governance/ Ida Berglund, materials design engineer for nominating-committee. QuesTek Innovations LLC. Berglund Nomination Deadline for 2017 Class of What does your typical workday look like? Fellows is Fast Approaching It starts with a cup of coffee (or three) at my desk while The honor of Fellow of the Society was established to going through emails and outlining my agenda for the day. provide recognition to members for distinguished contribu- There are often one or several internal project meetings tions in the field of materials science and engineering, and during the day to discuss technical work and strategies, and to develop a broadly based forum for technical and profes- the remaining time is spent by the computer on data anal- sional leaders to serve as advisors to the Society. Criteria for ysis, reporting, communication, or doing basic research. the Fellow award include: There is also the daily lunch group effort on solving the Chi- • Outstanding accomplishments in materials science or cago Tribune crossword puzzle. engineering • Broad and productive achievement in production, What’s been your biggest technical challenge? manufacturing, management, design, development, Being able to easily convey scientific concepts, ideas, research, or education and methods to a new audience. Also, despite almost six • Five years of current, continuous ASM membership years in the U.S. I cannot appreciate magnitudes of inches, Deadline for nominations for the class of 2017 is ksi, miles, and such, and find myself having to convert to SI units during conversations and presentations. November 30, 2016. View rules and past recipients at asminternational.org/membership/awards. To receive a What part of your job do you like most? unique nomination form link, contact Christine Hoover at The variety. There is a balanced combination of techni- [email protected]. cal work, meetings, reporting, client or collaborator interac- tions, and proposal writing, as well as travel to conferences or client meetings. Further, QuesTek works with a variety of 72 HIGHLIGHTS VOLUNTEERISM COMMITTEE

alloys, products, customers, and partners, thus the tech- Hobbies? nical work varies significantly, requiring me to constantly Traveling, skiing, dining, baking, and hiking. Basically expand my knowledge in not only alloy design, but in multi- anything involving new experiences or food and drinks. ple fields, which I greatly enjoy. Last book read? What is your engineering background? “Porten mot evigheten” by Ulf Westblom and John Ågren. I started my undergraduate studies in materials design For more information about ASM’s Women in Materials and engineering at the Royal Institute of Technology in Engineering Committee, visit asminternational.org/wime. Stockholm and continued through a master’s program spe- cializing in biomedical engineering while also focusing on metallurgy. This rather unusual combination of design, biol- VOLUNTEERISM ogy, and metallurgy prepared me for an ideal Ph.D. project on biomedical alloy design at University of Florida. COMMITTEE

What are you working on now? Profile of a Volunteer I’m currently involved in seven projects focusing on Beth Matlock, Senior Materials Engi- various classes of alloys or processes for different applica- neer, Technology for Energy Corp. (TEC) tions. While there is a large variety between the projects, When you’re blazing a new trail, it’s the methodologies and tools I use are similar between them good to have help. In the 1970s, Beth Mat- and utilize integrated computational materials engineering, lock was the only woman among 15 class- mates in materials engineering at North with work spanning from alloy design concept generation Matlock to process assessment and property modeling. As an exam- Carolina State University. She started out ple, I’m looking at chemistry modifications of a commercial as a pre-med student, but a chance encounter discussing

ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED alloy and its effect on properties, by modeling the phase super-sharp scissors while working at J.C. Penney led to a evolution with time using thermodynamic and kinetic mod- job in an x-ray diffraction lab and the decision to change her els, and correlating the nano- and microstructure to macro- major. After winning an ASM academic paper contest, she scopic behaviors. The principles are the same whether you was off and running. “It was maybe only $25, but to me that work with turbine blades or gum wrappers. award was huge,” recalls Matlock. “I got support and men- toring from people in the industry.” How many people do you work with? Matlock graduated in 1977 and moved to Lynchburg, QuesTek has 23 fulltime employees. The majority have Va., to work in failure analysis for Babcock and Wilcox. Her Ph.D.s, in materials science, mechanical engineering, or boss made it clear to all employees: “You will be active in physics, and while male dominated, there is a variety of cul- ASM.” Matlock served on the executive committee and tural backgrounds, ages, and personalities among us. The laughs recalling her “greatest contribution:” changing invi- small size of the company makes personal day-to-day inter- tations from “bring your wife” to “bring your spouse.” She actions inevitable, and I’m happy to be around people who and her husband moved to Knoxville, Tenn., in 1982 for his are not only intelligent, but also fun and kind. job and welcomed their first child. Working as a consultant, If a young person approached you for career advice Matlock joined the Oak Ridge Chapter and helped with about pursuing engineering, what would you tell them? membership outreach. Engineering is probably not what you think it is, or Employed by TEC for 32 years, Matlock works in the at least only part of it. Engineering skills can be applied to materials testing division. She’s served in numerous roles almost any field, regardless of discipline. As long as you with the Oak Ridge Chapter including chair in 2010 and enjoy what you do and are willing to learn new things, you marvels at tremendous programs in this active chapter. can make a career out of it. Therefore I would encourage any Her two children attended meetings and both became engineering studies or training. I would further suggest get- engineers. “My son went to more meetings than most ting involved in professional organizations within fields of members!” she says with a smile, remembering topics like interest by attending meetings and networking to get a bet- Cummins Engine Co., the Titanic, and the legend of the ter understanding of the society you’re considering going Damascus sword. into. This could provide a deeper insight than, for example, Matlock is still an active ASM volunteer for member- textbook reading or listening to people’s opinions and expe- ship outreach. She also runs her own beef cattle farm and riences. It could also give you an idea of the structure of the plays piano for her church. “We were put on this earth to community, which could identify paths needed to reach a give back,” she says. “ASM has given much to me. I need to certain position or environment you are interested in. pass that on to young students and engineers.” 73

MEMBERS IN THE NEWS HIGHLIGHTS ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016

CHAPTERS IN THE NEWS Alpha Sigma Mu has since expanded to include all materials disciplines. Oak Ridge Hosts Materials Camp Doll Awarded Visiting Fellowship University of Akron (UA) professor Gary Doll has been awarded a Royal Academy of Engineering Distinguished Visiting Fellowship allowing him to improve his interactions with the UK’s research base in tribology and surface engineering and to facilitate collabora- Doll tive research at The University of Man- chester. “I hope to continue my research on the surface engineering of materials to address friction, wear, and cor- Participants and volunteers of the Oak Ridge Chapter’s 2016 rosion, and lubrication strategies for challenging environ- Materials Camp held this summer at the University of Tennessee ments,” says Doll, Timken Professor of surface engineering in Knoxville. and director of the Timken Engineered Surfaces Laboratory. Seifi named Director of ASTM’s ASM Announces Mexico Chapter Additive Manufacturing Programs ASM welcomed its newest Chapter—Mexico—during ASTM International recently hired September 20-23 at the inaugural Heat Treat Mexico confer- Mohsen Seifi as a technical consultant ence. Bienvenido! See page 3 in HTPro for the full story. in additive manufacturing (AM) to sup- port standards development and related needs. Seifi, a post-doctoral research associate at Case Western Reserve Uni- versity, will serve as director of AM pro- Seifi grams. Seifi is a globally recognized expert in process-structure-property relationships for metal AM. As director, he will track key trends, drivers, and innova- tions while also building relationships with ASTM members, external networks, and professional organizations. Seifi will play a key role in collaborating with ASTM’s Committee on Additive Manufacturing Technologies (F42) as well as other committees interested in AM. Adriana Michaca and Carlos Carrasco.

MEMBERS IN THE NEWS Lampman Named Alpha Sigma Mu Fellow ASM’s very own Steve Lampman was recognized as a Fellow of Alpha Sigma Mu at a ceremony held during October at MS&T16 in Salt Lake City. Lampman has served as an editor of the ASM Handbook series for nearly three decades. Alpha Sigma Mu is the interna- Lampman tional professional honor society dedicated to encouraging and recognizing excellence in the materials engineering field. Members consist of students, alumni, and other pro- fessionals who have demonstrated exceptional academic and professional accomplishments. Founded in 1932, NEW TITLES FROM ASM INTERNATIONAL

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ASM Handbook, Volume 4E: Heat Treating of Nonferrous Alloys Aluminum-Silicon Casting Alloys: Atlas Of Microstructures Editor: George E. Totten Author: Małgorzata Warmuzek Hardcover | Product code: 05444G | ISBN: 978-1-62708-112-2 Hardcover | Product code: 05919G | ISBN: 978-1-62708-108-5

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Advertising closes January 5, 2017 Dictionary of Metals Contact us: by Harold M. Cobb 9639 Kinsman Road Materials Park, OH 44073-0002 Subscriptions/Customer Service: The authoritative reference work for terms and definitions of metals, 440.338.5151 800.336.5152 ext. 0 history, discoverer, naming, meaning, Fax: 440.338.4634 [email protected] applications, significance of the asminternational.org/AMP discovery and physical properties. Also includes a timeline of important events Subscriptions/Customer Service: Sales Staff: in the history of metals and metallurgy. 800.336.5152 ext. 0 AM&P/iTSSe/ASM Web Media [email protected] National Sales Manager Product Code: 05359G Erik Klingerman, Order online at Sales Staff: 440.338.5151 ext. 5574 www.asminternational.org/store Skip Wolfe, Director, Sales and Marketing [email protected] 440.338.5151 ext. 5226 Fax: 440.338.8542 [email protected] Affiliate Sponsorships Metallurgical and Kelly Thomas, CEM.CMP, National Account Manager AD INDEX Materials Transactions E AM&P/ASM Web Media Advertiser Page Advertiser Page Erik Klingerman 440.338.1733 Allied High Tech Products Inc. ThisBC new technicalMTS Systems journal Corp. from ASM and TMS5 is focused on the science of materials applied to National Sales Manager Applied Testing Systems 9 NSL Analytical Services Inc. 28 [email protected] current and emerging energy technologies. 440.338.5151 ext. 5574 AMT AG Access43 the journalOerlikon online Metco now! AG 48 Fax: 440.338.8542 DeWAL Industries Inc. 36 Saint-Gobain Coating 32 [email protected] ECM USA Journals68 CustomerSolutions Service Epsilon Technology Corp. 23325 Spring StreetThermo-Calc Software AB IFC iTSSe/Affiliate Sponsorships Goodfellow Corp. NewIFC York, NYTinius 10013, Olsen USA Inc. 11 Kelly Thomas, CEM.CMP tel: 800/777-4643 Inductoheat Inc. 50 Tungco Inc. 34 fax: 201/348-4505 National Account Manager Westmoreland Mechanical Instron [email protected] 77 440.338.1733 Testing & Research Inc. Ipsen Inc. 55 Fax: 614.948.3090 Master Bond Inc. 9 The ad index is published as a service. Every care Advanced [email protected] Metallizing Equipment Co. is taken to make it accurate, but 37 Materials & Processes assumes no responsibility 74 Pvt.ADVANCED Ltd. MATERIALS & PROCESSESfor errors or •omissions. NOVEMBER-DECEMBER 2014 APRIL 9-12, 2017 CHARLESTON AREA CONVENTION CENTER | CHARLESTON, SOUTH CAROLINA, USA

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POETRY BOOK PUTS THE PEDAL TO THE METAL A new book of poetry coauthored by an ASM Fellow provides a playful glimpse into the complex field of automotive materials. “What’s in Your Car: A Poetic Ride Through the Periodic Table,” by Paul E. Krajewski, FASM, and Matthew N. Topper uses a combina- tion of catchy poems and interesting pictures to explore how elements of the periodic table are used to make a car. Thirty-one elements are shown with images of the raw materials and their applica- tion within a vehicle. Materials are described with simple poems that can serve as a starting point for deeper exploration into the world of materials and automobiles. The book aims to appeal to children of all ages as they learn how different materials come together to create today’s automobiles. Included here are a few excerpts. “What’s in Your Car,” by Paul E. Krajewski and Matthew N. Topper.

Introduction could be used this way. Vanadium The elements are bricks that Aluminum is applied all over the car; Vanadium is found in many construct all things, You could say it’s a lightweight superstar. a mineral and deposit. From magnificent buildings to Wheels are forged and engines cast, The Model T could not have diamond rings. Making cars that are both cool and fast. been made without it. They give objects properties, and Aluminum’s surface refuses to rust, Vanadium makes steel each one has a role It’s a metal for hoods that wear resistant and strong, That can make it unique, or part engineers trust. Creating axles and crankshafts of the whole. that can last long. Shiny or light, heavy or strong, Molybdenum It also helps make battery acid and more, Conductive or bright, you can’t go wrong. Molybdenum’s a tongue twister, like the performance valve This book tells the story of what’s in a car. an out-and-out folly, material Titanium 64. From aluminum to zinc, they help you So most people just use its drive far. nickname, moly. So buckle your belt and adjust your view. Adding it to steel is an absolute must, Here’s a book about elements in a car To make that material more just for you. resistant to rust. Moly and sulfur create a slick actor, Aluminum Making lubes and greases We use aluminum almost every day, for your car or tractor. But I’ll bet you didn’t know it Vanadium is found in ocean algae.

Molybdenum is used as a fertilizer for cauliflower and broccoli.

Aluminum was once viewed as more precious than gold and silver. 80 3D PRINTSHOP

DIGGING UP A NEW material performance and printability printer to operate at different speeds or and validate models to reduce residual installing acoustic and electromagnetic ADDITITVE APPLICATION stress and distortion. ornl.gov. shields. buffalo.edu. Scientists at Oak Ridge National Laboratory (ORNL), Tenn., are design- 3D PRINTERS VULNERABLE COMING TOGETHER IN ing and producing the world’s first TO SMARTPHONE SPIES COLORADO 3D-printed excavator, a prototype that Researchers at the University of A public-private partnership has will leverage large-scale additive manu- Buffalo, N.Y., discovered that 3D printers been established to advance AM meth- facturing (AM) technologies and explore can be hacked with a common smart- ods for Nitinol, a nickel-titanium alloy the feasibility of printing with metal phone, threatening intellectual property. increasingly used in the medical indus- alloys. The scientists are collaborating While many 3D printers have security try. The Colorado School of Mines, Con- with industry partners and student engi- features such as encryption and water- fluent Medical Technologies, and the neers from the University of Illinois at marks designed to foil cyberattacks, Development of Additive Processing Urbana-Champaign who won a design the Buffalo team sidestepped those Technologies (ADAPT) program will join competition for the project. Three exca- safeguards and programmed a smart- forces to optimize the superelastic prop- vator components will be printed at phone’s built-in sensors to measure the erties of AM-synthesized Nitinol, which the DOE’s Manufacturing Demonstra- machine’s electromagnetic energy and exhibits unique shape memory proper- tion Facility at ORNL: the cab, the stick acoustic waves, which allowed them to ties in addition to being superelastic. (a large hydraulically articulated arm), map the print nozzle’s movements as “Over the next few years, we expect and a heat exchanger. The stick will be it printed. The phone, held 20 cm from ADVANCED MATERIALS & PROCESSES | NOVEMBER/DECEMBER 2016 NOVEMBER/DECEMBER | & PROCESSES MATERIALS ADVANCED additive manufacturing technologies fabricated with the Wolf System using the printer, gathered enough data to to have a profound effect on the med- a freeform technique for printing large- replicate a simple object with 94% accu- ical device industry,” says Tom Duerig, scale metal components, and the heat racy. For complex objects such as an founder of Confluent, a contract manu- exchanger will be printed on a Concept automotive part, the accuracy rate was facturer of Nitinol-based medical devices. Laser machine that produces metal parts still above 90%. To counter this vulnera- As part of the collaboration, the com- through a powder-bed-based laser melt- bility, researchers suggest several ways pany established the Confluent Medical ing process. During the nine-month fab- to make 3D printers more secure: Put Postdoctoral Fellowship at the School of rication and assembly period, the team a moat around the printer because the Mines with an initial $100,000 gift. In addi- aims to develop processes to improve ability to obtain accurate data for sim- ple objects diminished to 87% at 30 cm tion, a full-time postdoctoral researcher and 66% at 40 cm; or increase the print was hired for the project by ADAPT, a new speed—emerging materials may enable R&D consortium dedicated to develop- faster printing, reducing the ability to ing next-generation data informatics and track the print nozzle. Other options advanced characterization technologies include using software and hard- for AM. mines.edu, confluentmedical.com, ware-based solutions to program the inside.mines.edu/ADAPT-Home.

3D-printed excavator made of carbon fiber-reinforced ABS plastic. Courtesy of ORNL. Illustration of a smartphone hacking a 3D printer. Powerful Software for Thermodynamic and Diffusion Calculations Changing the Paradigm for Materials Design

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