Celebrating 100 Years

AMERICANa CERAMICting SOCIETY ars Celebr 100 ye

bullemerginge ceramicstin & glass technology MAY 2021 From concept to industry: Ultrafast laser welding

FMEA for spark plug design | MOF–glass composites | Virtual student exchange NEXT GENERATION GLASS RESEARCH for Sustainable Manufacturing

Thanks to a $1.7 million grant through the New York State Department of Environmental Conservation focused on glass recycling and de-carbonization of the glass manufacturing process, Alfred University is excited to announce the launch of the Center for Glass Innovation (CGI).

The CGI is an industry-led research center, with member directed programming and access to:

• Member-Directed Pre-Competitive Research • Self-Directed Funded Research • Collaborative Research • Discounted Analytical Services • Workforce Development Programming, Industry Short-Courses & Subsidized Interns • Intellectual Property

For membership information visit: www.alfred.edu/CACT or Contact Dr. John Simmins at: [email protected] Together creating the future of glass. contents May 2021 • Vol. 100 No.4 feature articles department News & Trends ...... 3 From concept to industry: Ultrafast laser Spotlight ...... 8 20 welding Research Briefs ...... 14 Ultrashort pulse laser welding has the potential to transform optomechanical component manufacturing—and Advances in Nanomaterials . . . . 16 research around the world is helping to move this technique from concept to industry. by Richard M. Carter columns

cover story Business and Market View . . . . . 5 Welding equipment and supplies: Global markets by BCC Publishing Staff Making sense of failure modes and effects 28 analysis: Case study of a spark plug insulator Into the Bulletin Archives— 1950s...... 6 Failure modes and effects analysis (FMEA) is a systematic approach to reduce technical risks of a product or by Lisa McDonald process by identifying all potential failure modes and their causes. Deciphering the Discipline . . . .. 48 Joining of similar and dissimilar materials by William J. Walker, Jr. by Alessandro De Zanet meetings Hybrid composites made from metal- MCARE 2021 combined with the 34 organic framework and inorganic glasses 4th Annual Energy Harvesting Elaborating on the recent discovery of glass formation at Society Meeting (EHS 2021) . . . 38 the phosphate-imidazolate join, we fabricate amorphous organic–inorganic composites using metal-organic frame- Materials Science and Technology works and inorganic glass. (MS&T21) ...... 40

by Courtney Calahoo, Louis Longley, PACRIM 14 including Glass & Thomas D. Bennett, and Lothar Wondraczek Optical Materials Division 2021 Annual Meeting (GOMD 2021). . . 42

Recap of St. Louis Section/Refrac- tory Ceramics Division 56th Sympo- Building bridges in the time of Corona: sium on Refractories...... 43 36 Virtual Student Exchange Program In August 2020, a group of Ph.D. students participated in a two-day Virtual Student Exchange Program, which offered them a way to replicate some of the in-person resources experiences of meetings that are currently unavailable Calendar...... 44 due to the coronavirus pandemic. Classified Advertising...... 45 by Iva Milisavljevic, Jenna Metera, Kana Tomita, Display Ad Index...... 47 and Yiquan Wu

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 1 AMERICAN CERAMIC SOCIETY bulletin online Editorial and Production www.ceramics.org Eileen De Guire, Editor [email protected] Lisa McDonald, Associate Managing Editor May 2021 • Vol. 100 No.4 Michelle Martin, Production Editor Tess Speakman, Senior Graphic Designer Editorial Advisory Board Darryl Butt, University of Utah Michael Cinibulk, Air Force Research Laboratory http://bit.ly/acerstwitter http://bit.ly/acerslink http://bit.ly/acersgplus http://bit.ly/acersfb http://bit.ly/acersrss Michael Hill, Tev Tech Inc . Eliana Muccillo, IPEN-SP, Brazil Oomman Varghese, University of Houston Kelley Wilkerson, Missouri S&T As seen on Ceramic Tech Today... Customer Service/Circulation Mantis shrimp inspire tough compos- ph: 866-721-3322 fx: 240-396-5637 [email protected] ites and sophisticated optical sensors

Advertising Sales Artists and scientists alike find inspiration in nature. But National Sales two recent scientific studies found inspiration in the same Mona Thiel, National Sales Director creature: the mantis shrimp. The creature’s incredibly tough [email protected] materials and complex eyes inspired innovations that ph: 614-794-5834 fx: 614-794-5822 could lead to fracture-resistant biocomposites and highly Europe advanced optical sensors.

Richard Rozelaar Credit: Dorothea OLDANI, Unsplash [email protected] ph: 44-(0)-20-7834-7676 fx: 44-(0)-20-7973-0076 Executive Staff Mark Mecklenborg, Executive Director and Publisher [email protected] Read more at www.ceramics.org/mantis-shrimp Eileen De Guire, Director of Technical Publications and Communications [email protected] Marcus Fish, Development Director Also see our ACerS journals... Ceramic and Glass Industry Foundation Electric field assisted solid‐state interfacial joining of TaC-HfC ceramics without filler [email protected] Michael Johnson, Director of Finance and Operations By A . Nisar, T . Dolmetsch, T . Paul, et al . [email protected] Journal of the American Ceramic Society Mark Kibble, Director of Information Technology [email protected] Laser-induced modification and external pressureless joining Na2FeP2O7 on solid electrolyte Sue LaBute, Human Resources Manager & Exec . Assistant [email protected] By M . Hiratsuka, T . Honma, and T . Komatsu Andrea Ross, Director of Meetings and Marketing International Journal of Ceramic Engineering & Science [email protected] Kevin Thompson, Director of Membership Effect of the thickness of nickel film interlayer on [email protected] direct-bonded aluminum/alumina as substrate in high-power devices Officers Dana Goski, President By W . Chao, C .‐Lin, and K . Lin Elizabeth Dickey, President-Elect International Journal of Applied Ceramic Technology Tatsuki Ohji, Past President Stephen Houseman, Treasurer Investigation of alumina doped 45S5 glass as a Mark Mecklenborg, Secretary bioactive filler for experimental dental composites Board of Directors ByY . B . Elalmis, B . K . Ikizler, S . K . Depren, et al . Mario Affatigato, Director 2018–2021 International Journal of Applied Glass Science Darryl Butt, Director 2020–2023 Helen Chan, Director 2019–2022 Monica Ferraris, Director 2019–2022 William Headrick, Director 2019–2022 Eva Hemmer, Director 2020–2023 John Kieffer, Director 2018–2021 Makio Naito, Director 2020–2023 Jingyang Wang, Director 2018–2021 Read more at www.ceramics.org/journals Stephen Freiman, Parliamentarian

American Ceramic Society Bulletin covers news and activities of the Society and its members, includes items of interest to the ceramics community, and provides the most current information concerning all aspects of ceramic technology, including R&D, manufacturing, engineering, and marketing . The American Ceramic Society is not responsible for the accuracy of information in the editorial, articles, and advertising sections of this publication . Readers should independently evaluate the accuracy of any statement in the editorial, articles, and advertising sections of this publication . American Ceramic Society Bulletin (ISSN No . 0002-7812) . ©2021 . Printed in the United States of America . ACerS Bulletin is published monthly, except for February, July, and November, as a “dual-media” magazine in print and electronic formats (www .ceramics .org) . Editorial and Subscription Offices: 550 Polaris Parkway, Suite 510, Westerville, OH 43082-7045 . Subscription included with The American Ceramic Society membership . Nonmember print subscription rates, including online access: United States and Canada, 1 year $135; international, 1 year $150 .* Rates include shipping charges . International Remail Service is standard outside of the United States and Canada . *International nonmembers also may elect to receive an electronic-only, email delivery subscription for $100 . Single issues, January–October/November: member $6 per issue; nonmember $15 per issue . December issue (ceramicSOURCE): member $20, nonmember $40 . Postage/handling for single issues: United States and Canada, $3 per item; United States and Canada Expedited (UPS 2nd day air), $8 per item; International Standard, $6 per item . POSTMASTER: Please send address changes to American Ceramic Society Bulletin, 550 Polaris Parkway, Suite 510, Westerville, OH 43082-7045 . Periodical postage paid at Westerville, Ohio, and additional mailing offices . Allow six weeks for address changes . ACSBA7, Vol . 100, No . 4, pp 1– 48 . All feature articles are covered in Current Contents .

2 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 news & trends

Endless Frontier Act: Will applied research become a main focus for the National Science Foundation? If you conduct basic science research “From 2000 to 2017, R&D spending is closing fast and that threatens our in the United States, chances are high in the United States grew at an aver- long-term health, economic competi- that you have received funding through age of 4.3% per year, … But spending tiveness, and national security,” writes the National Science Foundation in China grew by more than 17% per Senate Majority Leader Chuck Schumer (NSF). Created by Congress in 1950 “to year during the same period,” a Nature (D-NY) in a statement. “America can- develop and encourage the pursuit of article overviewing the recent “State of not afford to continue our decades-long a national policy for the promotion of U.S. Science and Engineering 2020” underinvestment and expect to lead the basic research and education in the sci- NSF report explains. “The United States world in advanced scientific and techno- ences,” NSF is now the funding source accounted for 25% of the US$2.2 tril- logical research.” for approximately 27% of the total fed- lion spent on R&D worldwide in 2017, These concerns are a major reason eral budget for basic research conducted and China made up 23%.” why, in November 2019, Schumer first at U.S. colleges and universities. These statistics have concerned U.S. spoke publicly about a proposal to have However, in recent years, a push government officials, and the past year the federal government increase support to make NSF a more applied research only heightened the concerns. “The for applied research during a confer- agency has gained steam in Congress coronavirus pandemic has shown the ence organized by the National Security due largely to increased investments science and technology gap between the Commission on Artificial Intelligence. made by China. United States and the rest of the world He said the goal of the proposal was to

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American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 3 news & trends

“I believe it would be a mistake for a technology directorate at NSF to serve as an offset to private funding for commercial innovation and entrepreneurship,” says Arden Bement, who led NSF from 2004 to 2010, in a Science article. “Federal funding for applied technology research and development should be need-based and channeled through mission agencies.” The Endless Frontier Act did not receive a vote before the end of the last Congress. But this February, Schumer announced that he planned to use the Endless Frontier Act as the “centerpiece” of a legislative package aimed at bolstering U.S. competitiveness with China in critical technology sectors. Several former NSF directors and former chairs of the agency’s governing body signed a letter in support of the bill (including Bement, who previously expressed reservations.) “As former NSF directors and National Science Board Chairs with decades of government experience, we are sup-

Credit: Jeff Fitlow, Rice University portive of the spirit of this legislation,” they write. “We note Rice University graduate student Wendy Hu, pictured, is leading that basic research is increasingly coupled to applications that development of a new technique to help clinicians obtain mean- respond to national needs. … The Endless Frontier Act would ingful patient groupings. Research like Hu’s that uses big data position NSF to take up that challenge.” falls under the key technology areas promoted by the Endless Frontier Act. Besides the Endless Frontier Act, there are several other proposals for increasing applied research funding that do create a new research-funding entity provisionally called the not involve drastically reorganizing NSF. For example, “National Science and Technology Foundation” that would Representative Ro Khanna (D-CA) introduced separate legisla- focus on emerging technologies such as artificial intelligence, tion in 2020 to establish a “Federal Institute of Technology” quantum computing, robotics, and 5G telecommunications. that would fund dozens of R&D hubs across the country, At that time, Schumer did not indicate whether the entity while Sen. Mark Warner (D-VA) proposed creating a new divi- would be permanent or if it would expire at the end of a sion in NSF that would fund partnerships between universities suggested five-year funding period. However, it became clear and local workforce organizations. that the initiative was meant to be a permanent change when In addition, the recently released report by the National Schumer and three bipartisan colleagues introduced the Security Commission on Artificial Intelligence recommends Endless Frontier Act in May 2020. establishing a new agency called the National Technology The bill, which is named in reference to the seminal Foundation that “would complement successful existing orga- “Science—The Endless Frontier” report by Vannevar Bush, nizations, such as the NSF and DARPA, by providing the would implement two major changes to NSF. One, the bill means to more aggressively move science into engineering.” would establish a new Directorate for Technology within On March 26, the House Science Committee introduced a NSF, bringing the total numbers of directorates to eight. bipartisan bill that offers an alternative vision for the National Two, NSF would be renamed the National Science and Science Foundation than that of the Endless Frontier Act. Technology Foundation (NSTF) to reflect the addition of the Learn more about their bill at https://bit.ly/3cQtGwj, which technology directorate. proposes to double the National Science Foundation budget “The Directorate for Technology would fund an assort- over five years and add a directorate to the agency focused on ment of university centers, testbeds, fellowships, and technol- “societal challenges.” 10 0 ogy consortiums, with a total recommended budget rising to $35 billion within four years, dwarfing the agency’s current THE AMERICAN CERAMIC SOCIETY $8.3 billion topline. The bill also proposes to create a multi- Website Advertising billion dollar technology hub program within the Commerce Department focused on catalyzing R&D partnerships in areas TARGET YOUR MARKET that are not already leading centers of innovation,” an FYI article on the bill elaborates. ceramics.org While the bill’s sponsors argue this reorganization of NSF is necessary to remain competitive on a global level, some lead- Contact Mona Thiel For Details ers in the science community expressed concerns that it would 614-794-5834 | [email protected] dilute NSF’s purpose.

4 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 business and market view

A regular column featuring excerpts from BCC Research reports on industry sectors involving the ceramic and glass industry.

Welding equipment and supplies: Global markets

By BCC Publishing Staff

he total market arc or arcs, mostly without the application • Other processes: There are many of pressure and with or without the use other welding processes, some of which T for welding-related of filler metal, depending upon the base are used on a selective basis. Others are products is expected to reach plate thickness. Examples: carbon arc in the development stage. Examples: welding, metal inert gas welding, plasma braze or bronze welding, induction weld- $37.2 billion by 2025, with arc welding, stud arc welding. ing, magnetic pulse welding. a compound annual growth • Resistance welding: Resistance The predicted CAGR of 5% for the rate (CAGR) of 5.1% from welding is a welding process wherein arc welding technology segment is the coalescence is produced by heat obtained highest among all the types of welding 2021 to 2025. The growth from the resistance of work to the flow technologies. The CAGR of 2.3% for in the safety and protective of electric current in a circuit of which thermochemical welding technology is the work is a part and by the applications the lowest, as this includes gas welding, equipment segment is expect- of pressure. No filler metal is needed. which is slowly becoming obsolete in ed to be the highest, with a Examples: spot welding, seam welding, many developed countries. CAGR of 7.6% during the projection welding, percussion welding. Various types of electrodes, filler • Solid-state welding: A solid-state rods, wires, fluxes, and gases are used forecast period. welding process produces coalescence in addition to the basic welding equip- Welding is a fabrication process that at temperatures essentially below the ment. These are called “consumables” joins material like metals and thermo- melting point of the base materials because they are consumed during plastics by applying some pressure and being joined without the addition of a welding. The consumables market is either with or without the presence of filler metal. Pressure is always applied. expected to continue increasing in filler material. Advantages of welding as Examples: cold welding, diffusion value and grow at a faster rate than the a joining method include considerable welding, ultrasonic welding, hot pres- equipment market because the market freedom in design, a joined piece that is sure welding. for consumables includes older equip- as strong as the base metal, and general • Thermochemical welding: The ther- ment as well as new equipment. equipment is not costly. Disadvantages mochemical welding process is a fusion The Asia-Pacific region is expected of welding include possible residual welding process in which no outside heat to increase at the highest CAGR of stresses and distortion of the workpieces, is required to melt the workpieces to be 5.4% due to the number of developed edge preparation of the workpiece, and joined. These welding processes involve countries moving their industries to this potential metallurgical changes. exothermic reactions. Examples: gas weld- region. Most of the leading welding tech- Welding processes can be classified ing, plastic welding, thermit welding, nology companies are from the Europe by the method used in producing the atomic hydrogen welding. and North America regions. welding heat and by the way the filler • Radiant energy welding: Radiant About the author material is fed into the weld. Welding energy processes focus an energy beam BCC Publishing Staff provides com- processes are typically classified as: on the workpiece. Heat is generated only prehensive analyses of global market siz- • Arc welding: Arc welding is a group when the energy beam strikes the working, forecasting, and industry intelligence, of welding processes wherein coalescence piece. Examples: electron beam welding, covering markets where advances in sci- is produced by heating with an electric laser beam welding, hybrid laser welding. ence and technology are improving the quality, standard, and sustainability of Table 1. Global market for welding-related products, by type of equipment, through 2025 ($ millions) businesses, economies, and lives. Contact Type of equipment 2019 2020 2021 2025 CAGR% the staff at [email protected]. (2021–2025) Resource Welding equipment and consumables 18,254.2 17,822.2 19,584.6 23,275.1 4.4% BCC Publishing Staff, “Welding Various gases for welding 6,418.8 6,010.8 6,178.1 7,693.7 5.6% Equipment and Supplies: The Global Automated and robotic welding and accessories 3,009.5 2,865.9 3,656.9 4,768.6 6.9% Market” BCC Research Report Safety and protective equipment 1,063.8 1,054.6 1,106.3 1,484.7 7.6% AVM040F, September 2020. Total 28,746.3 27,753.5 30,525.9 37,222.0 5.1% www.bccresearch.com. 10 0

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 5 bulletin timeline By Lisa McDonald

Into the Bulletin Archives—A look back at our 100 years in print

Since May 1922, the ACerS Bulletin has served the ACerS community, providing them updates on member news, Division meetings, and the latest research in ceramics and glass. In celebration of Volume 100 this year, the Bulletin editorial team is running a special column in each issue of the 2021 Bulletin that looks at the history of the Bulletin by decade. This issue highlights the 1950s. We hope you enjoy following the journey of the Bulletin from its early years to today. As an ACerS member, you have access to all 100 years of the Bulletin on the Bulletin Archive Online at https://bulletin-archive.ceramics.org. 10 0

Into the Bulletin Archives—1950s December 4, 1954. The January 1955 From the very first issue of this decade, the 1950s Bulletins took a significant turn in terms issue reported on the event, including of cover art—instead of real-life images, simple hand-drawn illustration were used. While the a quote from ACerS general secretary artwork generally featured machinery and parts, December issues were holiday themed. Charles S. Pearce on how the building For the Society, the 1950s is a significant decade because, for the first time since its came to be. founding, the Society raised enough money to build its own headquarters building in Columbus, Ohio. The building, which was located near the Park of Roses, was dedicated on “…it was back in 1938 that G. G. Hanson of Consolidated • • • • • • • • • • • • • • • • • • • • • • • • Feldspar insisted that The Society should have an office building 1950s of its own, a ceramic structure of which it could be justly proud, and presented his check for $10 to start the building fund. This first contribution was carried on the books for 12 years before it had company and the action that ACerS Bulletin (January 1955) Vol. 34 Iss. 1, p. 19 culminated in the new building

Credit: got under way.” ▲ The rst Society-owned headquarters building was considered “a true –ACerS Bulletin, Vol. 34., ceramic show place,” being made from brick, terra cotta, glazed tiles, and more. • Iss. 1., January 1955 The Society added two Divisions during the 1950s. Basic Science was announced in the March 1951 issue as being “composed of those members who are interested in the fundamental facts,

(December 1956) Vol. 35 Iss. 12, front cover front 12, Iss. 35 Vol. 1956) (December principles, and theories that underlie

the various manufacturing processes of

(December 1956) Vol. 35 Iss. 12, front cover front 12, Iss. 35 Vol. 1956) (December Bulletin ACerS ACerS Bulletin ACerS the ceramic industry.” Electronics was

ACerS Bulletin (July 1957) Vol. 36 Iss. 7, p. 283 Credit: Credit: Credit: Credit: announced in January 1958, and in Credit: the following February issue, a couple ▲ ACerS held its rst ceramographic exhibit in 1957 ▲ The cover of Bulletin December issues during the 59th Annual Meeting in Dallas, Texas. Opinion of corporate members expressed their in the 1950s were holiday themed, like surveys on the event unanimously recommended that it be approval of the new Division, such as this one from 1956. continued annually. Pictured is one of the entries: an elec- A. J. “Jo” Gitter of Whittaker, Clark & tron micrograph showing the nature of the surface structure Daniels, Inc. development of a barium titanate dielectric material. • • • • • • • • • • • • • • 6 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 DIVISIONS OF THE SOCIETY During the 1950s, the Society had nine Divisions.

• Basic Science (new) • Materials and Equipment • Design • Refractories • • • • • • • • • • • • • • • • • • • • • Electronics (new) • Structural Clay • Enamel “In my opinion, this is a forward about Ceramics Monthly and explore recent Products • Glass moving step. In the past several years issues at http://bit.ly/CeramicsMonthly. • White Wares I have had many, many contacts with the electronic industry and increasingly I felt that somewhere it would have to ‘hone’ for certain types of components with which the electrical engineering field are not really familiar.” –ACerS Bulletin, Vol. 37., Iss. 2., February 1958

In contrast to the approval surrounding the new Electronics Division, another member felt quite differently about the existing Design Division. “After 25 years closely associated with the art movement in ceramics, … I am still thoroughly convinced that the weakest link in American ceramics today is Design,” William Manker wrote in a December 1951 letter. “What we are lacking and that which we are primarily interested in—the Design Division—should and must continue to be an integrated part of The American Ceramic Society.” Manker offered several suggestions that he believed would help the Design Division flourish, and in January 1953, some of his suggestions were fulfilled when members Spencer Davis and Louis G. Farber launched a new magazine called Ceramics Monthly.

“The idea for a magazine devot- ed exclusively to the total ceramic art and craft field did not originate entirely in the minds of the publish- ers. The actions and comments of the thousands of active but much neglected ceramists stimulated the idea. … Here then is the line of communication so obviously needed by individuals from all walks of ceramic life.” –Ceramics Monthly, Vol. 1., Iss. 1., January 1953

Over 40 years later, in 1996, the Society • • • • • • • • • • • • • • would acquire Ceramics Monthly. Learn more • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 7 acers spotlight

SOCIETY Welcome new ACerS Corporate Partners ACerS is pleased to welcome its newest Corporate Partner: DIVISION – Uncountable SECTION

CHAPTER To learn about the benefits of ACerS corporate partnership, contact Kevin Thompson, membership NEWS director, at (614) 794-5894 or [email protected]. 10 0 Find the materials and supplies you need in ceramicSOURCE With more than 80 pages of listings, ACerS’ annual buyer’s guide ceramicSOURCE 2021 is certain to help you find the perfect materials, equipment, consultants, providers, supplies, and more. Whether you are looking for additives, refractories, a new kiln, laboratory services, dinnerware, or glass products—and everything in between—SOURCE has you covered. Be a part of ACerS online resource directory and printed buyer’s guide by adding your company’s free listing at https://ceramicsource.org. ACerS Corporate Partners may enhance their listing by adding logos, white papers, PDFs, and more. 10 0

Ceramic Tech Chat: Yuichi Ikuhara Hosted by ACerS Bulletin editors, ceram c Ceramic Tech Chat talks with ACerS i members to learn about their unique Te c h chat and personal stories of how they found their way to careers in ceramics. New episodes publish the second Wednesday www.ceramics.org/ceramic-tech-chat of each month. In the March episode of Ceramic Tech Chat, Yuichi Ikuhara, professor of engineering innovation at the University of Tokyo, discusses his work using scanning transmission electron microscopy to characterize grain boundaries in ceramics, the recent advances that have greatly improved this technique’s resolution capabilities, and where he sees TEM headed in the future. Check out a preview from his episode, which features Ikuhara discussing the big advances in TEM he has seen over the course of his career. “Previously, we are studying conventional transmission electron microscopy. So, we can observe the microstructure, but not so high resolution. But in this century, we have a very big evolution, that is spherical aberration corrected scanning transmission electron microscopy. This is very powerful technique, and the resolution of Cs-STEM is now less than 1 angstrom. Actually, we have a very high spatial resolution less than 0.5 angstrom. This means that you can even observe the hydrogen columns or lithium columns in materials.” Listen to Ikuhara’s whole interview—and all of our other Ceramic Tech Chat episodes—at http://ceramictechchat.ceramics.org/974767. 10 0

8 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Volunteer spotlight ACerS Volunteer Spotlight profiles a mem- MAY 11 ber who demonstrates outstanding service to 11 AM – 12 PM EST the Society. Hui (Claire) Xiong is Frontiers of Ceramics & associate professor in the Micron School of Glass Webinar Series Materials Science and SPONSORED BY Engineering at Boise State University. Xiong Xiong received her Ph.D. in electroanalytical chemistry from the PRESENTER: University of Pittsburgh. She conduct- WILL TASHMAN Title: Digitalization and the Future of Formulating in Modern R&D Labs ed postdoctoral work at Harvard Cost: Free University and Argonne National ACerS Corporate Partner Uncountable is sponsoring the complimentary webinar Laboratory. Xiong received the NSF “Digitalization and the future of formulating in modern R&D labs” on Tuesday, CAREER Award in 2015. She also is a May 11, 2021. CAES fellow and a Scialog Fellow. The biggest lever that R&D leaders have today is to implement better data tools Xiong is an active member of that make the learning process faster and easier. Will Tashman, co-founder of ACerS and serves as an officer of the Uncountable, will discuss the benefits of implementing a true data infrastructure and Electronics Division. She was one of the challenges that organizations will face along this journey. the lead organizers for the Electronic For more information and to register, visit http://bit.ly/Uncountable. 10 0 Materials and Applications conferences in 2020 and 2021. We extend our deep appreciation to Xiong for her service to our Society! 10 0 ECD seeks secretary A world leader in bioactive and nominations The Engineering Ceramics Division custom glass solutions invites nominations for the incom- ing 2021–2022 Division secretary. Nominations and a short description of the candidate’s qualifications should be Mo-Sci offers a wide variety of custom glass solutions submitted to Surojit Gupta at surojit. and will work with you to create tailored glass [email protected] by July 21, 2021. 10 0 materials to match your application. Contact us today to discuss your next project. mo-sci.com/contact IN MEMORIAM Mark Davis John May Lynn Owen Don Steffen @moscicorp Some detailed obituaries can also be found on the ACerS website, @MoSciCorp www.ceramics.org/in-memoriam. www.mo-sci.com • 573.364.2338 linkedin.com/company/moscicorp ISO 9001:2008 • AS9100C

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 9 acers spotlight ACERS ANNUAL MEETING at Technical Meeting and Exhibition AWARDS MS&T21 AND OCTOER COLUMUS OH DEADLINES MATSCITECH.ORG/MST2021

Society Nomination Contacts Description Awards Deadline

ACerS Fellow Sept. 2, 2021 Erica Zimmerman Elevation to ACerS Fellow [email protected] recognizes outstanding contributions to the ceramic arts or sciences through broad and productive scholarship in ceramic science and technology, by conspicuous achievement in ceramic industry, or by FOR MORE outstanding service to the Society. Visit http://bit.ly/ SocietyFellows to download INFORMATION: the nomination form.

ceramics.org/members/awards Division Award Nomination Deadline Contacts Description

GOMD Alfred R. Cooper May 15 Steve Martin The award recognizes undergraduate students who have demonstrated excellence in Scholars [email protected] research, engineering, and/or study in glass science or technology.

Electronics Edward C. Henry May 15 The award recognizes an outstanding paper reporting original work in the Journal of the Matjaz Spretizer American Ceramic Society or the Bulletin during the previous calendar year on a subject [email protected] related to electronic ceramics.

Electronics Lewis C. Hoffman May 15 Matjaz Spretizer The award recognizes academic interest and excellence among undergraduate students Scholarship [email protected] in the area of ceramics/materials science and engineering. Bioceramics Young Scholar July 1 Julian Jones The award recognizes excellence in research among current degree-seeking graduate [email protected] students and postdoctoral research associates.

Bioceramics Global Young July 1 The award recognizes the outstanding young ceramic engineer or material scientist who Julian Jones Bioceramicist has made significant contributions to the area of bioceramics for human healthcare [email protected] around the globe.

Bioceramics Larry L. Hench July 1 The award is presented to a deserving individual(s) in recognition of lifetime dedication, Lifetime Achievement Julian Jones vision, and accomplishments in advancing the field of bioceramics, particularly toward [email protected] innovation in the field and contribution of that innovation to translation of technology toward clinical use.

Bioceramics Tadashi Kokubo July 1 Julian Jones The award is presented in recognition of outstanding achievements in the field of [email protected] bioceramics research and development.

Engineering Ceramics Jubilee Global Diversity July 1 The award recognizes exceptional early- to mid-career professionals who are women Michael Halbig and/or underrepresented minorities (i.e., based on race, ethnicity, nationality, and/or [email protected] geographic location) in the area of ceramic science and engineering.

10 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Division Award Nomination Deadline Contacts Description

Bioceramics Tadashi Kokubo July 1 Julian Jones The award is presented in recognition of outstanding achievements in the field of [email protected] bioceramics research and development.

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 11 acers spotlight

MS&T21 speakers: You may be eligible for the GEMS award! STUDENTS The Basic Science Division organizes the annual Graduate Excellence in Materials Science (GEMS) awards to recognize the outstanding achievements of graduate AND students in materials science and engineering. The award is open to all graduate students who are making an oral presentation in any symposium or session at the Materials Science & Technology (MS&T) meeting. OUTREACH In addition to their abstract submission, students also must submit a nomination packet to the chair of the GEMS award selection committee, John Blendell, by Sunday, Aug. 15, 2021. For further details, go to www.ceramics.org/GEMS. 10 0 An abundance of student opportunities available at MS&T21 There are many opportunities available at this year’s MS&T. Make sure to sign up for the following student contests: • Undergraduate student poster contest • Undergraduate student speaking contest • Graduate student poster contest • Ceramic mug drop contest • Ceramic disc golf contest • Humanitarian pitch competition • …and MORE! For more information on any of the contests or student activities at MS&T, visit www.matscitech.org/students, or contact Yolanda Natividad, member engagement manager. 10 0 ACerS GGRN for young ceramic and glass researchers Put yourself on the path toward post-graduate success with ACerS Global Graduate Researcher Network. ACerS GGRN network addresses the professional and career development needs of graduate-level research students who have a primary interest in ceramics and glass. GGRN aims to help graduate students • Engage with The American Ceramic Society, • Build a network of peers and contacts within the ceramic and glass community, and • Access professional development tools. Are you a current graduate student who could benefit from additional networking within the ceramic and glass community? Visit www.ceramics.org/ggrn to learn what GGRN can do for you, or contact Yolanda Natividad, member engagement manager. 10 0 ACerS Associate Membership and Young Professionals Network The American Ceramic Society offers one year of Associate Membership at no charge for recent graduates who have completed their terminal degree. Join today to receive the benefits of membership in the world’s premier membership organization for ceramics and glass professionals. Start your free year-long membership by visiting www.ceramics.org/associate or contact Yolanda Natividad, member engagement manager. FOR MORE Also, consider joining ACerS Young Professionals Network (YPN) once you have become an ACerS member. YPN is designed for members who have completed their INFORMATION: degree and are 25 to 40 years of age. YPN gives young ceramic and glass scientists access to invaluable connections and opportunities. For more information, visit Yolanda Natividad www.ceramics.org/ypn. You may join this growing community by logging in to your [email protected] ACerS Personal Snapshot and marking “Young Professionals Network (YPN)” under the Interest Groups and Communities tab. 10 0

12 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 2020 GRATITUDE REPORT

We thank our generous donors for their support of our programs to attract, inspire, and train the next generation of ceramic and glass professionals. Despite the difficulties encountered due to the pandemic, we are pleased to present to you some highlights of 2020—examples of how your gifts have impacted and motivated students.

CGIF presents 2020 Gratitude Report The Ceramic and Glass Industry Our mission of inspiring and training the We invite you to read more about what your Foundation is pleased to share its 2020 next generation of ceramic and glass donations have done for students who are Gratitude Report—an overview of the professionals is being fulfilled every impacted through the CGIF at http:// year’s highlights presented in apprecia- day because of our donors. Despite foundation.ceramics.org/2020Report. As tion for all of those who have donated to the pandemic, your gifts enabled us to always, we truly appreciate you and your support our endeavors. We know that the launch a new materials science teaching gifts of support. growth of our outreach programs would resource, our Mini Materials Demo Kit, not be possible without our donors, thus a collection of seven simple demonstra- If you would like to provide a gift to the we offer our Gratitude Report to show tions for use by parents, teachers, and CGIF to support our work, please contact what YOU have accomplished with your students who are utilizing online and CGIF development director Marcus Fish at gifts of support. at-home teaching resources. [email protected] or 614-794-5863. You may also donate online at https://myacers. ceramics.org/donate. 10 0

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 13 research briefs

Researchers confirm existence of unique nonlinear optical response in nanocrystal-in-glass composites Researchers in China discovered nanocrystal-in-glass com- available for purchase. These devices mainly use various crystals as posites exhibit a unique nonlinear optical response called the nonlinear material. However, researchers have started explor- transverse second-harmonic generation that would allow for ing the potential of using nanocrystal-in-glass composites instead. the creation of light sources with expanded capabilities. Nanocrystal-in-glass composites are composed of tiny Nonlinear optics refers to the study of a wide range of inter- crystals embedded in a glassy matrix. These composites have esting physical phenomena based on nonlinear relationships. emerged as an alternative to glasses and crystals in display “Nonlinear” means there is not a direct or straight-line rela- applications because of some superior optical properties. For tionship between variables. In other words, nonlinear materi- example, nanocrystal-in-glass composites containing high-quartz als and processes exhibit responses that are disproportionate nanocrystals present zero thermal expansion over a wide tem- compared to the external force(s) triggering it. perature range of 0–50°C, which makes them ideal for use as In the case of nonlinear optics, the nonlinear optical process optical mirror blanks in ultrastable space telescopes. called second-harmonic generation is highly studied because of its Some nanocrystal-in-glass composites, such as those embed-

ability for high-resolution imaging. In this process, which is also ded with LiNbO3 and LiNb0.5Ta0.5O3, are nonlinear materials known as frequency doubling, photons that interact with a non- and so have potential for use in second-harmonic generation linear material will “combine” to form new photons with twice devices. However, the recent study led by professors Shifeng the frequency of the initial photons. This phenomenon allows for Zhou and Huakang Yu from South China University of Tech- the creation of low-power and compact light sources that operate nology reveals these composites may have additional potential in wavelengths typically requiring more power and larger devices. not previously realized. Since second-harmonic generation was identified in 1961, there Originally, their goal was to study the nonlinear optical now are numerous commercial devices based on this phenomenon response of nanocrystal-in-glass composites with different

Optical microscopy (left) and transmission electron microscopy (right) images of a glass composite embedded with

LiNbO3. Researchers in China discovered this composite exhibits a unique nonlinear optical response that is rarely seen in bulk materials. Credit: Shifeng Zhou

Research News

Concrete on the double Scientists obtain high-entropy carbide using electric arc plasma A team of researchers at Oak Ridge National Laboratory and the Scientists at Tomsk Polytechnic University in Russia synthesized a high- University of Tennessee developed a concrete mix that demonstrates entropy carbide consisting of five various metals using a vacuum-free high early strength within six hours of mixing, potentially doubling the electric arc method. High-entropy carbides are a new class of materials production capacity for the precast industry. Quick performing concrete simultaneously consisting of four or more various metals and carbon. shortens manufacturing time for prefabricated assemblies, but these Their main feature lies in the capability to endure high temperatures and early-strength mixes have short setting times and require specific energy flux densities. The high-entropy carbide created by the scientists curing methods. The researchers evaluated commercially available consists of titanium, zirconium, niobium, hafnium, tantalum, and components including steel, glass, and carbon fibers. The result was carbon. They plan to explore synthesizing high-entropy carbides of other a self-compacting mix that not only showed early strength but also chemical compositions using this method as well. For more information, maintained its workability for 30 minutes. For more information, visit visit https://news.tpu.ru/en/news. 10 0 https://www.ornl.gov/news. 10 0

14 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 domain structures in a counter-propagating laser scheme, i.e., a materials—seeing it in bulk nonlinear materials is rare. How- scheme where two laser beams enter the composite from oppo- ever, the fact it was discovered for the first time in a micro- site sides and interact. structured nonlinear photonic glass is exciting because of what While the nonlinear optical response in certain regions it offers in terms of application. of the LiNbO3-embedded composites was as expected, the “Standard second-harmonic generation is usually used for researchers surprisingly observed a local and brighter signal in laser frequency conversion,” Zhou says. In contrast, because an extreme region of the microstructure map—a signal that dis- the transverse second-harmonic generation signal reflects the appeared when either of the two laser beams were blocked. time domain information of the fundamental pulses, “the “It is strange that this brighter signal would vanish while signal can be used for pulse group velocity and pulse width the background second-harmonic generation still existed when measurement of ultrashort optical pulses with femtosecond either individual pulse is blocked,” Zhou explains in an email. time scales.” They realized that the brighter signal must be due to a spe- While this study focused on nanocrystal-in-glass composites cial nonlinear response called transverse second-harmonic gen- embedded with LiNbO3, “It should be noted that the strategy eration. Transverse second-harmonic generation differs from should be universal to a wide category of nanoparticle-in-glass standard second-harmonic generation in two significant ways. composites,” Zhou says. He adds that the researchers are now 1. Phase matching mode: Standard second-harmonic pho- working on developing a novel fabrication strategy to further tons are generated from the same pulse, whereas transverse expand the nanocrystal-in-glass composites to more extreme second-harmonic photons are generated from oppositely regions, and they are exploring the composites’ potential for propagating pulses. other unique properties and new practical applications. 2. Generation condition: The only requirement for achiev- The paper, published in Advanced Materials, is “Manipulating ing standard second-harmonic generation is to fulfill the phase nonlinear optical response via domain control in nanocrystal- matching condition, i.e., minimize mismatch between interact- in-glass composites” (DOI: 10.1002/adma.202006482). 10 0 ing waves along the propagation direction. Transverse second- harmonic generation requires that, in addition to the phase matching condition, overlap of the oppositely propagating pulses in time and space must occur as well. This difference in origin means that standard second-harmonic generation and transverse second-harmonic generation manifest differently as well. While the signal from standard second-harmonic generation can easily be observed at any position where the fundamental pulse passes, the signal from transverse second-harmonic generation can only be observed at the position where oppositely propagating pulses overlap. The discovery of transverse second-harmonic generation in nanocrystal-in-glass composites is surprising because the phenomenon is typically observed in low-dimension nonlinear

Fast p-type oxide semiconductor rolled into life with liquid metal An RMIT-led research team has introduced ultrathin beta-tellurite to the 2D semiconducting material family, providing an answer to the decades-long search for a high mobility p-type oxide. There are two types of semiconducting materials: “n-type,” which have abundant negatively-charged electrons; and “p-type,” which possess plenty of positively-charged holes. A barrier to oxide devices has been that while many high-performance n-type oxides are known, there is a significant lack of high-quality p-type oxides. The new beta-tellurite is a p-type, and the researchers isolated it using a specifically developed synthesis technique that relies on liquid metal chemistry. For more information, visit http://www.fleet.org.au/news. 10 0

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 15 advances in nanomaterials

Researchers demonstrate potential of MXenes as additives in ultrahigh-temperature ceramics Researchers at Indiana University–Purdue University phase transformation process from a 2D flake to a 3D crystal- Indianapolis investigated the phase stability and transforma- line structure when annealed at high temperatures: tion of titanium carbide MXenes at high temperatures to 1. Low-temperature annealing up to 200°C results in loss of better understand its potential as an additive in ultrahigh- water molecules trapped between the MXene layers. temperature ceramics. 2. Medium-temperature annealing causes desorption of

Titanium carbide (Ti3C2Tx) is the most studied layered functional groups. Specifically, temperatures of 300–500°C carbide from the MXene family. It is known to have impres- result in removal of –OH groups, –F groups desorb at 500– sive material properties, including high in-plane mechanical 750°C, and complete desorption of all –F and –OH groups stiffness (330 ± 30 GPa), high electrical conductivity (10,000– occurs above 800°C. 20,000 S•cm–1), and high temperature phase stability (up to 3. High-temperature annealing above 800°C causes partial

800°C under inert environments). phase transformation to cubic TiCy, while full transformation Recently, researchers have investigated using titanium car- occurs at temperatures above 1,200°C. bide MXenes as additives in metal and ceramic matrix compos- Processing at temperatures above 800°C is required for ites to endow the composites with improved in-matrix mechan- many metal and ceramic matrix composites, yet detailed char- ical and electrical properties. However, this application faces a acterization of the phase transformations at these temperatures slight obstacle—these composites require processing at relatively is not complete. Fortunately, the new study led by Anasori high temperatures, and titanium carbide MXenes exhibit vari- looks to fill this gap in knowledge. able rates of oxidation and degradation when exposed to high The researchers explain that titanium carbide MXenes offer temperatures in the presence of oxygen. a unique advantage compared to other 2D materials when it Technically, “all the ultrahigh-temperature ceramics comes to investigating the material properties. “Fundamentally,

(carbides, nitrides, and borides) get oxidized in air. But Ti3C2Tx is a nano-lamellar titanium carbide, which means that the oxide shell is too thin (at relatively low temperatures) Ti3C2Tx has compositional similarity to the bulk crystalline that we don’t discuss them,” explains Babak Anasori, assis- three-dimensional (3D) nano-lamellar transition metal carbides tant professor at Indiana University–Purdue University that have been studied for the past >50 years,” they write. As Indianapolis, in an email. “But if we make UHTCs at 1-nm such, “We can use previously established literature on the size [as is the case with MXenes], then oxidation becomes a bulk carbides as a guide on the potential phase transformation major issue.” behavior of Ti3C2Tx during high-temperature annealing.” Processing in low-oxygen environments offers a partial solu- Based on what is known about bulk carbides, the research- tion, but researchers still need to consider the possible effect ers hypothesized that titanium carbide MXenes would have of high temperatures on the MXene’s electrical, catalytic, and two main ranges of phase transition: mechanical properties. In particular, early studies have estab- 1. Low-temperature phase transition to a mix of 3D crystal- lished that titanium carbide MXenes undergo a three-stage line Ti2C + TiCy at temperatures of 700–1,000°C. Credit: Babak Anasori, Indiana University–Purdue University Indianapolis Researchers at Indiana University–Purdue University Indianapolis showed titanium carbide MXene flakes undergo a phase transformation upon sintering to become a stable, bulk 3D crystal.

16 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 R R Starbar and Moly-D elements are made in the U.S.A. with a focus on providing

2. High-temperature phase transition to purely TiCy at tem- the highest quality heating elements peratures above 1,000°C. and service to the global market. The researchers used wet chemical selective etching to syn- thesize two different forms of titanium carbide MXene films for their experiments: nondelaminated multilayer stacks (clay) and delaminated single-to-few layers of flakes (single-flake). Then, they investigated the phase transformations using in- situ heated X-ray diffraction paired with a 2D detector (up to 1,000°C) and ex-situ methods using tube furnace and spark plasma sintering for high-temperature annealing (up to 1,500°C). The results confirmed their original hypothesis. In particular, they found that the titanium carbide MXene keeps its 2D layered structure up to 600°C, after which stable 3D crystal-

line phases of Ti2C and TiCy are formed. These phases remain stable up to annealing temperatures of 1,000°C in both single- flake films and multi-layer clay films, after which there is a sub- 56 years of service and reliability

sequent transition to cubic TiCy above 1,000°C. In an email, Ph.D. student Brian Wyatt explains why con- I Squared R Element Co., Inc. firmation of this transition from a 2D to 3D crystalline phase Phone: (716)542-5511 is an important finding. Generally, the layers of 2D materials Email: [email protected] are held together by weak van der Waals forces. For 2D materials such as graphene or hexagonal boron nitride, the van der www.isquaredrelement.com Waals bonds can become weak spots in the composites. “In contrast, we can turn MXenes’ inter-flake van der

Waals bonds to primary bonds through high-temperature GLOBAL SUPPORT TEAM sintering,” Wyatt says. This transformation will allow the ON-SITE SERVICE MXene to “behave as a type of ‘glue’ within UHTCs to improve the bonding between ceramic grains, and thus form fracture and thermal shock resistance UHTCs with improved Engineered Solutions oxidation properties.” FOR POWDER COMPACTION Anasori’s group is already working on forming MXene UHTC composites using different ceramic materials and exploring their mechanical and oxidation properties. “We CNC HYDRAULIC AND believe MXenes for the extreme environment will become a ELECTRIC PRESSES new and fast-growing research area,” Ph.D. student S. Kartik Easy to Setup and Flexible for Simple to Complex Parts Nemani says in an email. The paper, published in Journal of Physics: Condensed Matter, is “High-temperature stability and phase transformations of

titanium carbide (Ti3C2Tx) MXene” (DOI: 10.1088/1361- 648X/abe793). 10 0 HIGH SPEED PTX PRESSES Repeatable. Reliable. Precise. find your COLD ISOSTATIC PRESSES vendors with Featuring Dry Bag Pressing ceramicSOURCE 814.371.3015 ceramicsource.org [email protected] www.gasbarre.com POWDER COMPACTION SOLUTIONS

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 17 advances in nanomaterials

Hydrogenation stabilizes borophene for practical use Researchers led by Northwestern Hydrogenation, or reaction with hydro- “This oxidation peak is clearly smaller University researchers, along with col- gen, is one type of passivation process than that of the borophene sample after leagues from the University of Florida that first-principles calculations suggest 1 hour of ambient exposure, indicating and Argonne National Laboratory, could be used to stabilize borophene that the oxidation rate is reduced by experimentally investigated the hydroge- and suppress ambient oxidation. more than two orders of magnitude,” nation of borophene to see how well it While theoretical explorations of they write. These findings show “that stabilizes the material for practical use. hydrogenated borophene, or “boro- diverse hydrogen-bonding motifs on Borophene, a 2D sheet of boron phane,” have taken place, “atomically borophene impart ambient stability.” atoms, was first theorized in the 1990s well-defined synthesis and characteriza- In addition to providing ambient and experimentally confirmed in 2015. tion of borophane polymorphs have stability on the order of days, which is a Much like graphene, borophene is flexi- not yet been achieved,” the researchers sufficient time window for most ambient ble, strong, and lightweight. It also forms explain in the paper. So, their aim was characterization and processing meth- in several different crystal structures to investigate this synthesis. ods, the researchers also found that the (polymorphs), so structural manipula- To create borophane, they exposed hydrogenation of borophene was revers- tion of borophene is easier than it is for borophene to atomic hydrogen in ible using thermal annealing. graphene. For these reasons, some feel ultrahigh-vacuum conditions. Then, they “Specifically, borophane samples borophene may serve certain applica- extensively studied the bonding structure could be recovered to pristine boro- tions such as wearable device applica- and properties by combining scanning phene without apparent degradation tions better than graphene. tunneling microscopy and spectroscopy, after annealing the sample to ~300°C,” However, borophene rapidly oxidizes inelastic electron tunneling spectroscopy, they write. This finding is significant in air, which means integrating boro- and density functional theory. because it means pristine borophene can phene into practical devices is difficult. Similar to the high degree of poly- be regained once ambient processing is To date, experimental characterization morphism in borophene, the research- complete or robust encapsulation layers of borophene has required ultrahigh- ers observed eight different borophane are applied. vacuum conditions to avoid unwanted polymorphs. All of the polymorphs dem- In a Northwestern University press reactions with air. onstrated markedly improved chemical release, senior author and Walter P. Fortunately, passivation may address and morphological stability in ambient Murphy Professor of Materials Science borophene’s volatility. Passivation conditions. In particular, degradation in and Engineering Mark C. Hersam says refers to processes used to reduce borophane was only detected after 1 week their findings will allow researchers to the chemical reactivity of a material. of ambient exposure. more rapidly explore borophane’s properties and its potential applications. The paper, published in Science, is “Synthesis of borophane polymorphs through hydrogenation of borophene” (DOI: 10.1126/science.abg1874). 10 0

LIVE VIRTUAL CONFERENCE July 19–22, 2021 MATERIALS CHALLENGES IN ALTERNATIVE AND RENEWABLE ENERGY 2021 (MCARE 2021) 4TH ANNUAL ENERGY HARVESTING SOCIETY Credit: Mark Hersam, Northwestern University Hydrogenating the 2D material borophene offers a way to stabilize it against ambi- MEETING (EHS 2021) ent oxidation. In this image, grayish teal balls represent boron and red balls represent hydrogen.

18 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 THERE’S ALWAYS SOMETHING NEW TO LEARN IN ACERS LEARNING CENTER. CerSONLINE UPCOMING LEARNINGCenter ceramics.org/onlinecourses

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From concept to industry: Ultrafast laser welding

By Richard M. Carter hen manufacturing optomechanical Wcomponents, one of the more problematic steps is bonding the optical components to a structural body. Such optical components can include a whole variety of glass and crystal materials, but these materials are normally chosen for Ultrashort pulse laser welding has the potential to their optical properties rather than their structural transform optomechanical component manufacturing or mechanical performance. Because it usually is —and research around the world is helping to move inadvisable to manufacture the structural chassis this technique from concept to industry. from similar (i.e., glass) materials, this decision inevitably leads to a significant mismatch between the properties of the optic and its mount, most significantly in their thermal properties. There are essentially two options when joining dissimilar materials. The first option involves using some form of clamp or mechanical fix- ing. In this case, the mismatch in thermal properties is less of an issue; however, such an approach requires additional design engineering and several manufacturing steps. Thus cost, mass, volume, and scope for mis- alignment can all increase, which can significantly impact applications. The other option is to use some form of bonding interlayer. This interlayer can take the form of an adhesive, frit, or solder, for example, depending on the precise materials involved. However, creating a reproducible manufacturing process with these materials is rarely as simple as one might wish. For example, issues in the use of adhesives for high-precision optics are well known and can be attested to by

20 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Capsule summary A SHORT HISTORY BROAD POTENTIAL BUDDING INDUSTRY Since researchers at Osaka University (Japan) The applicability of the technique is very A few companies have adopted ultrashort published a paper in 2005 showing that ultra- broad, from the types of materials welded pulse laser welding as an industrial process short laser pulses could weld transparent mate- together to the wavelength of laser used, thus because, despite the high cost, this technique rials together, a substantial amount of research giving laser manufacturers the ability to offer offers the key advantages of a limited ther- worldwide has demonstrated new material a suitable system provided they have suf- mally affected zone, the ability to join a range combinations as well as generated knowledge ficient knowhow of the focusing and material of materials, and the ability to do so without on fundamental laser–material interactions. handling requirements. introducing an interlayer.

anyone who has attempted to develop a optical and mechanical components as “ultrashort” pulsed laser is required, one reproducible high-precision adhesive pro- these materials can differ in expansion which produces laser pulses in the order cess. Therefore, in general, considerable rates by an order of magnitude or more. of pico- to femtoseconds (10–12 to 10–15 s). time and money usually are needed to Because joining of dissimilar materi- Over these extremely short timescales, develop sufficient art for a reliable, high- als is still fundamentally desired, the the laser–material interactions take precision process. trick would seem to be to minimize the on some features that can be benefi- Furthermore, these bonding processes volume of material that needs to be cially exploited, which can be further fundamentally rely on the introduction heated, thus reducing the total amount enhanced by focusing the laser into a of an interlayer in some form, which of thermal stress introduced. Minimizing very small area. First, the duration of often generates its own problems. A the volume of heated material can be any individual pulse is sufficiently short common manifestation is creep, or part best achieved by limiting the total ther- so there is no time for heat to dissipate movement during curing. But often mal energy introduced around the weld through thermal conduction. Hence, the more problematic is material aging per- zone, i.e., to use a very focused source of thermal energy will, for a short time, be formance, with outgassing a particularly heat. The laser is an ideal tool for local- just as concentrated as the laser energy. significant issue for systems where strict ized heating because the energy can be Second, while the pulses contain a low atmospheric control needs to be main- deposited exactly where it is required by amount of energy (10–15 µJ is typical), tained to avoid reducing system lifetimes focusing and scanning the beam across the combination of temporal and spatial and/or performances (e.g., vacuum sys- the material interface. concentration—typically the pulses are tems and some lasers). Of course, the use of lasers for welding focused into spots of 1–4 µm diameter Because of these limitations, an alter- is not at all new. But there is a significant for this type of welding—results in truly native, direct joining technique would difference in capabilities depending on enormous energy densities, typically in be preferred. The obvious solution there- what type of laser is used. In general, the order of MW of peak power and fore would be to directly weld the two lasers can be divided into two broad GWcm–2 in intensity. This amount of components together. categories. The first is “continuous wave energy is more than enough to not only Be it a torch, arc, friction, or laser, lasers.” As the name suggests, these lasers melt but also vaporize material. welding relies on a source of thermal provide a continuous beam of light. If The combined effect is that there is energy to locally melt material over directed onto a material, it provides a a highly concentrated thermal gradient. a scale of millimeters to centimeters. continuous thermal input very much like The area of the weld zone is molten—as Depending on the technique, the weld- a welding torch and so is not terribly well is required for welding—but the bulk of ing process may also involve adding a suited to preventing thermal expansion the material experiences almost no tem- “filler” material to bridge a gap between issues during welding. perature rise. Furthermore, the thermally the parts. The materials then will mix in The alternative is to pulse the output affected zone, defined here as the zone a liquid state, potentially combine chem- of the laser because it is then possible which has seen sufficient temperature to ically, and cool to form a welded bond. to separate the peak intensity in the melt, is strictly limited in size to only a When dealing with broadly similar pulse from the average power delivered few 100 µm around the focus. It is this materials, this process generally works by temporally concentrating the energy. concentration of the temperature gradi- extremely well, with the welded material The pulse duration and the repetition ent that allows for welding of dissimilar often stronger than the bulk. However, rate are thus both key factors in how the materials without excess thermal stress this process breaks down when consider- laser–material interaction will work—and because the total volume of heated mate- ing dissimilar material welding, largely thus key to controlling the thermal pro- rial is strictly limited. due to differences in thermal expan- file during welding. For most industrial However, the extreme thermal gradi- sion—when a material begins to solidify, laser processes, pulse durations are in ent presents a new issue to the welding thermal stresses accumulate and result in the order of milli- to nanoseconds (10–3 process—material at the focus of the an almost immediate failure of the weld. to 10–9 s). While short, this duration laser beam will be not only melted but Thermal stresses can be problematic does not provide a sufficiently high local- also vaporized (in fact, a plasma will be when considering two different metals, ization of thermal energy to allow for formed). This area essentially becomes but the issue is even more extreme for dissimilar material welding. Instead, an a small pocket of high-pressure gas and,

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 21 From concept to industry: Ultrafast laser welding

chemicals, enabling selective etching). However, its potential to applications of laser welding was not appreciated until relatively recently.

A brief history of ultrashort pulse laser welding The story of ultrashort pulse laser welding starts in 2005 at Osaka University (Japan) with a paper demonstrating that it was possible to not only modify transparent material using an ultrashort laser pulse but also possible 1 Credit: Carter to weld them together. In this paper, Figure 1. Schematic illustration of ultrashort pulse laser welding. The incident laser is they focused a femtosecond laser on focused through the glass onto the metal surface. By translating the laser along the the interface region between two glass interface, a weld is formed from an inner plasma affected region and an outer heat- plates in intimate contact, fusing them affected zone (HAZ). into a weld. The importance of this result was clearly well appreciated by depending on the precise dynamics of atoms. Light is composed of individual the team at Osaka because they were the laser used, may be surrounded by a photons, where each photon has a spe- careful to obtain a patent within Japan region of melted material. Thus, if a weld cific amount of energy that is related before publishing. is attempted on the edge of the parts, this to the wavelength. At 1,000 nm, glass Further publications from Osaka— gas will escape as a jet, carrying off much is transparent because the photons do including joint publications with of the melt volume with it and resulting not have the correct energy to inter- RWTH-Aachen University (Germany) in ablation rather than welding. This phe- act with the atoms within the glass. and IMRA American Inc. (a Michigan- nomenon limits the technique to a lap However, if several photons arrive at based U.S. laser company)—expanded weld, where the laser is focused through a single atom at essentially the same the understanding of the process and one of the two materials (Figure 1). In time, their combined energy will be the range of glasses demonstrated, and this way, the gas is confined until it can enough to trigger absorption. also further reinforced the copywrite cool and form a bond. Under normal circumstances, the protection with additional patents in There clearly is a limit to the materi- probability of photon absorption hap- Germany, Japan, the U.S., and world- als that can be welded with this tech- pening is essentially zero, but a focused wide. However, the process they dem- nique as at least one must be transpar- ultrashort laser pulse has such extreme onstrated relies on the formation of ent to the laser. Typically, these types of photon density that the probability a fusion filament, a feature particular lasers operate at a wavelength of around becomes not only nonzero but quite to femtosecond lasers, and it was only 1,000 nm (in the near infrared part likely. The net result is that it is possible applied to transparent (i.e., broadly simi- of the spectrum), although there are a to trigger absorption in otherwise trans- lar) materials. range of other wavelengths commonly parent materials but only at the focus of This publication set off a bewildering available. At this wavelength, most an ultrashort laser pulse—nowhere else is array of research worldwide, with many optical glasses and crystals will be trans- the photon density sufficient to permit publications demonstrating new mate- parent but all metals and most semi- this phenomenon. In other words, it is rial combinations as well as in-depth conductor materials will not. Ceramics possible to trigger absorption inside the studies on the fundamental laser–mate- pose an interesting issue as while sev- volume of a transparent material. rial interactions, including development eral ceramics are nominally transparent This ability is extremely powerful of sophisticated theoretical modeling at this wavelength, they often are highly because it allows us to control the energy systems. Readers of the Bulletin may be scattering due to the fine structure and deposition within an otherwise transpar- interested to note that this work has thus may not be suitable for focusing a ent material in three dimensions by care- included welding of transparent ceram- laser beam through. fully positioning the focus using micro- ics,2 but for the purpose of this article The final aspect of laser–material stages or some form of optical scanner. we will concentrate on developments interactions using ultrashort pulses is This effect has been known for some toward dissimilar material welding. the most intriguing: the ability to trig- time and has been exploited in a range It would not be till 2007 that Osaka ger what is referred to as nonlinear of applications to alter the glass proper- published the first paper in the area of absorption. To understand this process ties (e.g., to change its refractive index dissimilar material welding, when they requires some understanding of how and make waveguides; or to change demonstrated glass–silicon welding.3 light behaves and how it is absorbed by the reaction of the glass to etchant This achievement was significant as

22 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 it showed that welding was possible between a transparent and opaque material. However, the chemical compatibility of silicon and glass (essentially silicon dioxide) still left open the question of whether the process could be applied more universally to dissimilar materials. Shortly thereafter, the University of Kassel (Germany) published their own demonstration of silicon–glass welding in early 2008,4 indicating international

interest in this development. Credit: Chen et al., Optics Express Osaka continued to lead in this area, Figure 2. Illustration of the use of a correctly positioned focal point to create a melt providing the next milestone in 2008 volume to bridge a gap, or local roughness, between two materials. Taken from 8 with a publication demonstrating the Chen et al. welding of copper and glass using a fem- between the two materials to prevent binations. In 2020, NASA (U.S.) dem- 5 tosecond laser. This study was a major plasma from escaping—in effect hold- onstrated the bonding of several glasses breakthrough as copper, silicon, and oxy- ing the material together using van der and crystals to metals, including invar, gen have limited chemical interactivity Waal’s force until it can be reinforced titanium, calcium fluoride, and Zerodur and thus limited scope to form a purely into a weld. (a specialist low thermal expansion glass chemical bond. Nevertheless, a bond Higher repetition rate and picosecond from Schott).16 More recently, Jena was indeed demonstrated, and it could laser systems, in comparison, produce a (Germany) made a significant contribu- now be said that truly dissimilar material teardrop-shaped weld feature that typically tion by demonstrating silicon–copper welding was possible. exhibits a small but significant melt vol- welding, where the silicon is the trans- The following years would see surpris- ume. This melt has been demonstrated to parent optical material.17 ingly few publications in this area, as the be useful in assisting confinement of the majority of research seemingly aimed at plasma (Figure 2) and thus in reducing Current capabilities and potential similar material welding. It was not until the requirement for surface contact dur- The range of materials with pub- 2011 that the next novel material dem- ing the bonding process. However, it has lished demonstrations include optical onstration was made: The University the disadvantage that more care needs to glasses, crystals, metals, ceramics, and Laval (Canada) with a paper exhibiting be taken to ensure that the laser focus is semiconductors. Thus, the applicability welding of fused silica to both copper accurately positioned and that increased of the technique is very broad. While 6,7 and tungsten. gaps between materials will result in some material combinations appear to It is worth noting that up to this decreased weld strengths.8 be simpler to weld than others (usually point all dissimilar material welding was In my own research group at Heriot- demonstrated by a wider, more forgiv- carried out using a femtosecond laser. Watt University (Edinburgh, Scotland), ing process parameter space), there is no Although pico- and femtosecond lasers we demonstrated welding using a pico- clear link between material properties are both referred to as ultrashort lasers, second laser with a paper in 2014.9 In and the capability or ease of welding. there are significant differences in the this case, additional proof-of-principle From my own experience, it is pos- way the laser–material interactions occur demonstrations expanded the range of sible to weld almost any two materials and thus their capabilities. As previously materials to include new metals and a provided they can be prepared properly. mentioned, femtosecond lasers are able crystal: aluminum, stainless steel, silicon, All that is required is time, effort, and to generate high aspect ratio filaments and copper welded to glass and sapphire sufficient samples to carry out a study of plasma due to a complex self-focusing (Figure 3). Since 2014, several other uni- of the welding parameter space. Indeed, effect in material, while almost entirely versities have published works demon- the only material we have failed to weld avoiding the generation of molten mate- strating welding of various combinations entirely was not a single material but rial when using a low repetition rate of these materials, indicating a wide- rather a mix of silicon carbide and alu- (typically 1–10 kHz). This situation spread interest in this novel capability, minum with individual grains of each results in an extremely high aspect ratio including the universities of Tampere at multimicrometer sizes. Because these weld structure but one which is generally (Finland),10 Okayama (Japan),11 Nara grains are larger than the laser spot size quite intolerant to any gap between the (Japan),12 Kyiv (Ukraine),13 Guangdong used for welding, the process is not two materials because even a micrometer (China),14 and the Key State Labs in really applied to a single material and level gap will allow the gas to escape. Xian (China).15 However, it is only very hence unsurprising that no single set of As such, submicrometer contact (often recently that there were published welding parameters could be obtained referred to as optical contact) is required demonstrations of further material com- for the combination.

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 23 From concept to industry: Ultrafast laser welding

In terms of suitable optical sources, most work was carried out with lasers operating around 1,000 nm. However, there are examples in the literature from 515–1,558 nm, demonstrating that the precise wavelength (within reason) of the laser is not critical. Pulse durations also seem to widely vary, albeit always within the ultrashort pulse range, with demonstrations from 50–2,000 femtoseconds, which is likely more indicative of available lasers within disparate research labs than any fundamental requirement on pulse duration. Similarly, the repetition rates used vary from 1 kHz to several MHz, although here there seems to be a clear difference between femtosecond filament-based welding at low repetition rates and pico-/femto- processes at repetition rates exceeding 100 kHz, which rely on the formation of a melt volume and are more tolerant to surface roughness. The overall picture, therefore, is that although the welding process requires optimization for each material combination and laser system, the required technical specifications for that laser are quite broad, allowing a wide range of laser manufacturers to be able to offer a suitable system provided they have sufficient knowhow of the focusing and material handling requirements. The quality of bonds is more difficult to assess because the majority of these tests are in a proof-of-principle stage with limited statistical information regarding the strength and yield, among other properties. To the best of my knowledge, the only in-depth analysis looking to optimize a dissimilar welding process was carried out at Heriot-Watt,18 although readers will readily appreciate that this kind of detailed research does not always make it into published papers—particularly where there is a potential for industrial application and new product development. Where the quality of these welds was investigated, they tend to rely on some form of mechanical strength for quantitative evaluation. Typical arrangements involve a pull, shear, or some form of wedge/knife inserted in the gap between the components after welding, with the force required to break the bond being logged. It is prudent to be cautious in directly comparing the absolute values of weld strength between published techniques because the techniques usually are not directly compa- rable to one another and there is as yet no clear ISO standard for evaluating these types of bonds. Nevertheless, such results are suitable for identifying an optimum for a specific welding process and will, at the least, provide a reasonable estimate of expected strength, as can be seen in Figure 4. One of the issues that becomes quickly apparent is in how the welds fail. This failure is almost always in the glass—often with a volume of glass left attached to the structural component after failure—because the welding process creates a defect in the glass. At the boundary of the glass melt zone, there is an abrupt change to the fictive temperature, which manifests as a visual change in refractive index as well as local stress. Credit: Carter et al., Applied Optics Studies indicate it is this line that most often fails (Figure 5).9 Figure 3. Our first of proof-of-principle welds in (A) Al-SiO 2 The glass–metal weld, despite exhibiting complex chemistry, (B) Cu-SiO (C) Stainless steel–BK7 optical glass (D) Si-SiO 2 2 microcracks,19 which in standard welding would all be causes (E) Stainless steel–Sapphire. These 2.5-mm diameter spirals are typical of a “spot weld arrangement.” Note the backlash for concern but is not normally the source of failure. in our stage control—we have come quite a way since these Thus, in almost every case it is the optical component that samples! Taken from Carter et al.9 fails first. Because the optical component usually is a brittle material, the difficulty then is that the “weld” failure is brittle

24 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 as well—with all the accompanying statistical variation this failure implies. To obtain reliable data on the strength of the bonds, it is thus not only necessary to carefully design a measurement technique but also to measure a large number of components to build up a statistically meaningful set of data. Nevertheless, results from across the published record suggest bonds that are at least as strong as equivalent adhesives and, in some cases, more than ten times stronger—certainly sufficient for current applications. It is crucial to note that these studies reveal that both the strength and the reliability (yield) is tightly inter- twined with material preparation. As mentioned, to obtain a strong, reliable bond, the materials should ideally be placed in intimate, optical contact before Credit: Carter et al., Applied Optics welding. This placement is clearly more Figure 4. Example of weld strength statistics for Al–BK7 bonding. In this case, 20 sam- readily achieved with materials that are ples for each of two processing parameters (average power and focal position) were extremely flat, smooth, and clean. While tested. The bonds here are single 2.5-mm diameter spot welds and are required to sus- tain only 7 N of shear force for this application. Taken from Carter et al.9 easily achieved in optical components (as these are already prepared to high exposed as curved or recessed surfaces high-quality machined or ground surface. specifications with sub micrometer or (both often desired for optical mounts) However, care still is required so that even 10s of nanometer roughness and are out of the question. While other the surface preparation method does not flatness), preparing structural materials polishing techniques may be applicable detrimentally affect the welding because to the same specification is a nontrivial (e.g., chemical, laser) it has yet to be yields varying between 80–97% have problem that scales with the required demonstrated that both the required been obtained for different preparations contact area. level of flatness and roughness can be methods of what is nominally the same The common option at present is achieved in a reliable fashion. surface finish. to polish the material to an essentially The alternative technique, which Thus strengths, yields, and mate- mirror finish via lapping, thus provid- Heriot-Watt has developed extensively, is rial combinations are appropriate for ing both the required roughness and to use the melt generated in a 100s kHz a wide range of applications where flatness. This process is both slow and process to fill the gap between the two a mechanical bond is required. But expensive, but with the right equipment materials, thus relaxing the requirement what of applications where more and expertise, it is reliable for most to polish the metal surface. To date we than a purely mechanical attachment materials (aluminum being a key excep- have successfully welded surfaces with is required? Hermeticity has been tion). Unfortunately, lapping requires SA roughness in the order of approxi- demonstrated in glass–glass and glass– the target surface to be both flat and mately 1 µm, which is consistent with a silicon welding, but it remains to be Credit: Carter et al., Applied Optics Figure 5. Illustration of the weld failure mechanism for a glass–metal bond. Both images are taken side on with a reflection of the weld and the metal surface visible toward the bottom of the images. Image (a) is an untested example. Image (b) was taken part- way through the welding process, and a crack in the glass has developed. Adapted from Carter et al.9

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 25 From concept to industry: Ultrafast laser welding

available, information suggests they offer only similar material (glass–glass) weld- (a) ing as a process. A second early entry came in the form of a Finnish company, Primoceler Oy. This company appears to have been a spin out from the collaborative work between Osaka and Tampere around 2013.10,11 Initially aimed at glass– glass welding, the company also offered glass–silicon welding as part of an all- glass or silicon–glass packaging capability. In 2018, Primoceler was acquired by Schott AG (who also holds an Osaka patent), who now offers glass–glass and glass–silicon welding. Trumpf (a German laser systems company) also is known to be active in this (b) area, with joint publications with the Universities of Jena and Aachen.20,21 For the most part, this research seems to be in the area of glass–glass welding (including as part of its own production process for optical fiber end caps), although in (c) the last few years Trumpf showed glass– metal optical mounds with welds at exhi- bitions, which seems to be as far as the company has taken such applications. The most recent entry into the field Credit: Oxford Lasers is Oxford Lasers (U.K.). They, in collaboration with Heriot-Watt University, (d) developed a prototype laser welding system for glass–metal welding, includ- Figure 6. (a) Photograph ing demonstrations of aluminum–BK7 of an Oxford Lasers C-Series and quartz–stainless steel. Importantly, laser micromachining station. Images of example laser welded this prototype is a fully integrated plat- parts: (b) One-inch, 4-mm thick quartz waveplate form based on a standard turnkey laser welded to stainless steel, (c) Fused silica plate micromachining platform (Figure 6), the welded to the end of a 40-mm diameter alumi- general form of which will be familiar num tube, (d) BK7 prism (18-mm height) welded to industrial laser uses. Therefore, it to a mounting plate. Images courtesy of Oxford includes the expected capacity to, among Lasers. www.oxfordlasers.com. other things, generate user-defined laser beam toolpaths and correct for working demonstrated if this is the case more of small spot welds, thus limiting the distances and aberrations in optics, but generally—although it would certainly issue, but for a hermetic seal a continu- also an adjustable laser amplifier allow- be extremely surprising given the weld ous perimeter weld will be required ing for both a pico- and femtosecond cross-sections studied thus far to find which, by necessity, will cover a longer welding on demand. that it is not. However, a point to con- line and larger area, thus giving larger The key advantages in ultrashort laser sider is that thermal expansion is still expansion stresses. welding are the limited thermally affect- an issue for the assembled component. ed zone, the ability to join a range of Using an ultrashort laser pulse allows Industrial availability and materials, and the ability to do so with- the materials to be bonded but does applications out introducing an interlayer. However, not change the fundamental fact that An early adopter of an industrial the cost of an ultrashort laser system two dissimilar materials will expand process was IMRA American Inc. (from is currently in the order of more than at differing rates. A purely mechanical at least 2006). Although they currently $100k, suggesting applications either bond can be achieved using a series hold some of the key patents publicly require economy of scale or high-value

26 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 products. From the current industrial 7D. Hélie, F. Lacroix, and R. Vallée, Bonding um pulsed picosecond laser welds,” Materials players, this suggestion would seem to of optical materials by femtosecond laser welding Characterization, vol. 120, pp. 53–62, 2016. bear out because, although there are for aerospace and high power laser applications 20S. Richter et al., “Laser welding of glasses few public examples to draw on. Schott (Photonics North 2012). SPIE, 2012, vol. at high repetition rates – fundamentals and 8412. seems to have taken aim at semiconduc- prospects,” Optics & Laser Technology, vol. 83, 8 tor device packaging while Trumpf and J. Chen, R. M. Carter, R. R. Thomson, and pp. 59–66, 2016. Oxford Lasers appear to be well set up to D. P. Hand, “Avoiding the requirement for 21F. Zimmermann et al., Advanced welding of pre-existing optical contact during picosecond cater to high-value optical, optomechani- transparent materials by ultrashort laser pulses laser glass-to-glass welding,” Optics express, vol. (SPIE LAMOM). SPIE, 2019, vol. 10519. 10 0 cal, and aerospace device fabrication. 23, no. 14, pp. 18645–18657, 2015. In truth, while high-value manufactur- 9R. M. Carter, J. Chen, J. D. Shephard, R. R. ing has led the way, the range of potential Thomson, and D. P. Hand, “Picosecond laser applications is truly staggering because welding of similar and dissimilar materials,” dissimilar material bonding is an issue in Applied optics, vol. 53, no. 19, pp. 4233–4238, almost all areas of manufacturing, from 2014. DOWNLOAD A microdevices up to building-scale applica- 10I. Miyamoto, Y. Okamoto, A. Hansen, J. FREE DEMO! tions. We have every expectation that this Vihinen, T. Amberla, and J. Kangastupa, technique will rise to its potential and “High speed, high strength microwelding of prove to be a significant new capability. Si/glass using ps-laser pulses,” Optics express, vol. 23, no. 3, pp. 3427–3439, 2015. About the author 11Y. Okamoto, I. Miyamoto, J. Vihinen, and Richard M. Carter holds a Research A. Okada, “Novel micro-welding of silicon Fellowship in Optical Manufacturing and glass by ultrashort pulsed laser,” in from the Institute of Photonics and Materials Science Forum, 2014, vol. 783: Trans Quantum Sciences at Heriot-Watt Tech Publ, pp. 2792–2797. University, Edinburgh, Scotland. 12M. M. Negrub, D. Hélie, I. V. Yurgelevych, Contact Carter at [email protected]. and L. V. Poperenko, “Ellipsometric control of laser welded materials,” in International ACERS – NIST PHASE References Conference on Global Research and Education, EQUILIBRIA DIAGRAMS 2017: Springer, pp. 26–31. NIST STANDARD REFERENCE DATABASE 31 1T. Tamaki, W. Watanabe, J. Nishii, and K. 13 CONTAINING 30,834 DIAGRAMS Itoh, “Welding of transparent materials using J. Zhang et al., “Microwelding of glass to silicon by green ultrafast laser pulses,” femtosecond laser pulses,” Japanese journal of Optics & , vol. 120, p. 105720, 2019. TRUSTED. applied physics, vol. 44, no. 5L, p. L687, 2005. Laser Technology 14 COMPREHENSIVE. 2E. Penilla et al., “Ultrafast laser welding of S. Matsuyoshi, Y. Mizuguchi, A. Muratsugu, H. Yamada, T. Tamaki, and W. Watanabe, ceramics,” Science, vol. 365, no. 6455, pp. CONVENIENT. 803–808, 2019. “Welding of glass and copper with a rough surface using femtosecond fiber laser pulses,” SMART. 3 T. Tamaki, W. Watanabe, and K. Itoh, Journal of Laser Micro Nanoengineering, vol. 13, PORTABLE. “Laser micro-welding of silicon and borosili- no. 1, pp. 21–25, 2018. cate glass using nonlinear absorption effect 15 UNIQUE. induced by 1558-nm femtosecond fiber G. Zhang and G. Cheng, “Direct welding of glass and metal by 1 kHz femtosecond laser laser pulses,” in Commercial and Biomedical UP-TO-DATE. pulses,” Applied optics, vol. 54, no. 30, pp. Applications of Ultrafast Lasers VII, 2007, vol. AFFORDABLE. 6460: International Society for Optics and 8957–8961, 2015. Photonics, p. 646018. 16R. Lafon, S. Li, F. Micalizzi, and S. Lebair, No price increase in 2021 4A. Horn, I. Mingareev, A. Werth, M. Ultrafast laser bonding of glasses and crystals to Kachel, and U. Brenk, “Investigations on metals for epoxy-free optical instruments (SPIE ultrafast welding of glass–glass and glass–sili- LASE). SPIE, 2020, vol. 11261. con,” Applied Physics A, vol. 93, no. 1, p. 171, 17M. Chambonneau et al., “Taming ultrafast 2008. laser filaments for optimized semiconductor- 5Y. Ozeki et al., “Direct welding between cop- metal welding,” Laser & Photonics Reviews, 15, per and glass substrates with femtosecond 2000433, 2021. laser pulses,” Applied physics express, vol. 1, no. 18R. M. Carter et al., “Towards industrial

8, p. 082601, 2008. ultrafast laser microwelding: SiO2 and BK7 to 6F. Lacroix, D. Hélie, and R. Vallée, “Optical aluminum alloy,” Applied optics, vol. 56, no. bonding reinforced by femtosecond laser 16, pp. 4873–4881, 2017. welding,” in Optical Manufacturing and Testing 19O. P. Ciuca, R. M. Carter, P. B. Prangnell, IX, 2011, vol. 8126: International Society for and D. P. Hand, “Characterisation of weld Equilibria Diagrams Optics and Photonics, p. 812612. zone reactions in dissimilar glass-to-alumini- www.ceramics.org/buyphase

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 27 Making sense of failure modes and effects analysis: Case study of a spark plug insulator

By William J. Walker, Jr.

Figure 1. Cross section of a spark plug showing the major components. Spark plug insulators are typically made from 95–96% alumina. Credit: Tenneco

ailure modes and effects analysis (FMEA) is a electrode, which defines the sparking gap. Fsystematic approach to reduce technical risks The spark plug also has an internal resistor of a product or process by identifying all potential failure that suppresses electromagnetic interference. A critical function of the insulator is to modes and their causes. Effective FMEA can anticipate isolate the high voltage. When the dielec- and prevent problems, reduce costs, shorten product tric breakdown strength of the material is exceeded, a pinhole or puncture through development times, and result in safer products and the ceramic is formed and that puncture processes with high reliability. becomes the preferred path for the electric The right time to start a FMEA is during the concept phase of the product life current, which is to say that it sparks through cycle. It could be a new design, a new technology, or a new process, but it also could the puncture instead of firing across the gap, be a new application of an existing design or process. A FMEA is a living document. and the engine misfires. When changes are made to an existing design or process because of new technol- Today’s engines require as much as 45 kV ogy, new requirements, or new knowledge about the product, including experience to create a spark, an increase from 36 kV not gained during the product life cycle, the FMEA needs to be updated. too many years ago. Dielectric breakdown The two most commonly used FMEAs are Design FMEAs and Process strength of the ceramic is a critical property FMEAs. As the names suggest, Design FMEA applies to the design of a prod- to withstand the high voltage without dam- uct, and Process FMEA identifies potential failure modes from manufactur- age. Improvements of existing ceramic mate- ing, assembly, and logistical processes to ensure that the final product meets rials and development of new ceramic materi- the requirements of the design. Design FMEA and Process FMEA are closely als with higher dielectric breakdown strength linked, as the former provides the inputs for the latter. are ongoing efforts. The focus of this article is on Design FMEA for a ceramic material used to The Design FMEA for the insulators will make spark plug insulators. A spark plug, shown in Figure 1, can be seen as an be considered on two different levels: the electrical feed-through that creates a high-energy spark to initiate combustion spark plug, and the ceramic material. The in an internal combustion engine. The ceramic insulator is generally cylindrical methodology for preparing a Design FMEA with a bore along the axis to support the components that transport electrical for a material is not documented in the stan- current from the ignition lead to the gap where the spark is created. The exter- dard FMEA handbooks and thus presents a nal surface is contoured to interlock with the shell that threads into the cylinder challenge. This article describes the approach head of the engine. The shell is electrically grounded and is attached to a ground taken by Tenneco Inc.

28 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 History of FMEA in the automotive industry A seven-step approach The FMEA methodology was first developed in the The automotive industry follows FMEA stan- The new FMEA handbook defines a 1940s by the United States military as “Failure dards developed by the Automotive Industry Ac- a seven-step approach to FMEA (Table I).1 Mode, Effect and Criticality Analysis.” NASA ad- tion Group (a U.S. industry group) and Verband opted it in the early 1960s for the Apollo program. der Automobilindustrie (a European industry Step 1 is planning and preparation, an In the late 1970s, the automotive industry began group). The two organizations recently released important part of which is to define the to use FMEA following the highly publicized safety a joint handbook that reconciles the differ- scope of the FMEA—what it is that is issues with the Ford Pinto. ences that previously existed in order to have being analyzed, and what is outside the a common standard for the global automotive Following the release of the ISO 9000 inter- industry.b scope of the investigation. The scope is national quality management standards in This project was completed before limited to the area of design responsibil- 1988, the U.S. automotive industry developed the new handbook was released and relies ity. Outside that limit, it is someone heavily on the earlier Verband der Automobilin- QS 9000, which included Design and Process c else’s design responsibility and excluded FMEAs as part of advanced product quality dustrie guidelines to meet the requirements of 10 0 from the FMEA. Another part of Step 1 planning. FMEA is now used by a wide range of a customer in Europe. is putting together the team, which needs industries, including software, semiconductors, to be multidisciplinary to get the perspec- food service, and healthcare. tives of all stakeholders. a. United States Military Procedure MIL-P-1629, Procedure for performing a failure mode, effects Step 2 is structure analysis, which and criticality analysis, Nov. 9, 1949, since updated to MIL-STD-1629. identifies the different system elements b. Failure modes and effects analysis—FMEA Handbook, Automotive Industry Action Group and that go into the product and how these Verband der Automobilindustrie, First Edition, 2019. components are interrelated (for example, c. Verband der Automobilindustrie, “Product and Process FMEA,” Quality Management in the Automotive Industry Volume 4, Second Edition, 2012. the mating of parts and the interfaces where matter or energy is transferred In Step 4, failure analysis, all possible Step 6, optimization, addresses the areas between system elements). System ele- failure modes are listed for each system of highest risk by identifying actions nec- ments include assemblies, subassemblies, element. The failure modes may be the essary to reduce the risk and evaluating components, and characteristics. By loss of function, which can occur sud- the effectiveness of those actions. breaking the system up into separate sys- denly, intermittently, or as a degradation Once these steps are all completed, tem elements, each of the elements can over time. A failure mode also may be Step 7 is results documentation, which cov- be treated as individual focus elements performance outside of the specified ers documenting and communicating the that are analyzed in terms of each one’s range. Once failures are identified, they results. The complete FMEA form can be function and failure. One way to perform are linked based on cause and effect. quite extensive, and includes the function structure analysis is using a structure tree, The failure effect is the consequence of analysis, failure analysis, risk analysis, and which shows how the system elements go the failure mode and occurs at the next optimization in a single document that is together to form the overall system. level up. The failure cause is the reason organized according to the structure analy- Step 3 is function analysis, which (in the next level down) why the failure sis. Historically, the completed FMEA assigns functions to the system ele- mode occurred. The way the failures are was a paper document in the form of an ments and links the functions based on linked usually follows the function tree. FMEA table. However, it has become com- cause and effect. (Functions should be Step 5, risk analysis, assigns risk to mon for the FMEA to be documented in described in terms of what the system each identified failure mode based on electronic format using FMEA software, element does in relation to the next severity, occurrence, and detection. The which allows the data to be presented in higher level on the structure analysis.) FMEA handbook has established guide- multiple formats, including the FMEA With a good function analysis, Step 4, lines for rating these risks (Table II),1 form, the structure tree, and the function failure analysis, can be done in a very sys- which run on a scale of 1 to 10. and failure nets. The software also simpli- tematic manner, which helps to ensure thoroughness of the process. Table II. Criteria for severity, occurrence, and detection ratings.* Rating Effect Severity Occurrence Detection Table I. Seven-step process for conducting failure modes and 10 Very High Safety, regulatory New technology Test method to be effects analysis. 9 developed System analysis Step 1. Planning and preparation - Product identification and boundaries 8 High Loss or degradation New design based - Assemble a cross-functional team 7 of primary function on similar technology Unproven test method Step 2. Structure analysis 6 Step 3. Function analysis 5 Moderate Loss or degradation Detail changes to 4 of secondary function previous design Failure analysis and risk mitigation Step 4. Failure analysis 3 Low Step 5. Risk analysis 2 Objectionable effect Mature technology Proven test method Risk communication Step 6. Optimization on function Step 7. Results documentation 1 Very Low No discernable effect Failure not possible Failure always detected *Adapted from the AIAG & VDA FMEA Handbook.1

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 29 Making sense of failure modes and effects analysis: Case study of a spark plug

Figure 2. Tree diagram showing structure analysis for a spark plug. Structure analysis identifies the different system elements that go into the product and how these components are interrelated. Credit: Walker, Jr.

Figure 3. Tree diagram with addition of one function and one failure at each level for the insulator. Function analysis assigns functions and specific requirements to the system elements from the structure analysis, and links the functions based on cause and effect. Failure analysis identifies the failure to meet the requirements (loss of function) and links the failures. With the addition of all functions and all failures, the function analysis and failure analysis can

Credit: Walker, Jr. become quite complex. fies integration of multiple FMEAs to inputs to an (internal or external) suppli- The next step is function analysis. In describe an entire product or system. er’s FMEA in the form of specifications the simplified example shown in Figure 3, The results of the Design FMEA are and drawings. only one function for the spark plug and the basis for product drawings and design one function for the insulator are con- specifications and are used as the inputs Applying FMEA to a spark plug sidered, but in fact most system elements to the Process FMEA. The Design FMEA The structure analysis for a spark plug will have a number of functions. also will identify certain special character- (Figure 2) shows that the spark plug is In addition to the functions, there are istics, which can be directly responsible made up of a number of different com- specific requirements, such as to form a for the failure of a product and require ponents. Each of these components is spark at the firing tip. This requirement special attention for process control. made of some material and has some comes from the design of the engine. It is For a complex system such as an particular geometry, so at the lower level, outside of the design responsibility of the automobile, FMEAs will be developed there are geometrical characteristics of spark plug designer; it is specified by the on several different levels; together, they the component and the material char- customer. It is one of the inputs into the provide a complete description of the acteristics of the component. The scope Design FMEA. Looking at the insulator, system. Within a single organization, of the FMEA is limited to the area of its function is to isolate the high voltage multiple FMEAs may be integrated into design responsibility. The spark plug so the current can be delivered to the fir- a larger FMEA, but between companies designer specifies a geometry and a mate- ing tip with a requirement to withstand they typically remain separate. In either rial for each of the components. The the voltage needed to form the spark. case, the outputs of an (internal or details of why the material has the prop- The next level down from the insu- external) customer’s FMEA become the erties that it does are not necessary. lator is the system element “Material

30 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Credit: Walker, Jr.

Figure 4. Structure analysis of the ceramic material with functions and characteristics identified for selected system elements. characteristics of the insulator,” which is the set of properties that are needed to (a) meet the performance requirements of the insulator. To withstand the voltage requirement, the key property is dielectric breakdown strength. In Step 4, failure analysis, all possible failures are listed for each system element. In the Figure 3 example, the failure mode is that the insulator does not isolate the high voltage because of a dielectric failure. The failure effect, on the spark plug level, is a spark is not created at the firing tip. The failure cause is the dielectric breakdown strength of (b) the ceramic is too low. Because this is a Design FMEA, it might be better to say the ceramic material was incorrectly specified with insufficient dielectric breakdown strength.

Applying FMEA to a ceramic material As we develop a Design FMEA for the ceramic material—which on the spark plug FMEA is the box marked as “Material characteristics of the insulator”—we need Figure 5. Examples of tree diagrams showing a portion of (a) the function analysis and to think about what the system elements (b) the failure analysis, with fired density as the focus element. are. In other words, we need to consider Credit: Walker, Jr. the components of the material that give basis for developing the Design FMEA Material characteristics are physical us the set of properties that are handed to for the ceramic material. and chemical aspects that fully describe us in the form of a materials specification Performance of a material is its response the material—the structure and the from the spark plug designer. to a complex set of conditions. A material composition. The National Academy The well-known relationships between property is the response to a single well- of Sciences Materials Advisory Board performance, properties, characteristics defined energy field. Examples include defined characteristics as “those fea- (or structure), and processing that are the mechanical strength, dielectric breakdown tures of the composition and structure foundation of materials science were the strength, and thermal conductivity. (including defects) of a material that

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 31 Making sense of failure modes and effects analysis: Case study of a spark plug are significant for a particular prepara- In the structure analysis for the ceramic raw material that go into the formula- tion, study of properties, or use, and material (Figure 4), the highest level is the tion, the particle size after milling, the suffice for reproduction of the mate- fired ceramic. The ceramic is the product spray dried granule size, and so on. rial.”2,3 Characteristics can be considered that is being designed. The requirements These characteristics are inputs into the as intrinsic properties—they are not of the fired ceramic material are the prop- Process FMEA. The characteristics of the response to an external stimulus. erties from the spark plug Design FMEA. the raw materials are the specifications Examples include density, grain size, The next level is the characteristics of the that are given to the suppliers. For cal- pores size, and defect structure. fired ceramic, and one more level down cined alumina, the specifications are the Processing is the path taken to obtain includes the characteristics of the raw ultimate crystal size, the specific surface the desired characteristics. From an engi- materials that go into the ceramic and area, and chemical composition. neering perspective, the performance of also the characteristics of the ceramic mix, Once all of the functions and charac- the material depends on its properties, which is the characteristics of the feed- teristics are assigned, the next step is to the properties depend on the character- stock used to make the ceramic. link functions based on cause and effect. istics, and the characteristics depend on Functions of selected system ele- The function net for fired density is the processing. A scientific understand- ments are included in Figure 4. The shown in Figure 5a. Dielectric strength ing of cause and effect goes in the other functions for the fired ceramic are the is dependent on fired density, and fired direction. The processing defines the properties from the spark plug Design density is dependent of several factors characteristics, the characteristics control FMEA, such as dielectric breakdown at the characteristic level. But dielectric the properties, and the properties work strength and mechanical strength. The breakdown strength is not the only prop- together to determine the performance. characteristics of the fired ceramic are erty that is influenced by fired density. In FMEA language, the term charac- those features of the composition and Others include mechanical strength, teristics is used to broadly describe the structure (including defects) that fully chemical resistance, and thermal con- requirements of the material. In materi- describe this material: the fired density, ductivity. Because each characteristic of als language, these requirements are the amount of porosity, the size of the the fired ceramic can influence several better described as properties. For the pores, the size of the grains, the size of properties, and because each character- ceramic material FMEA, properties and any defects, and the chemical and phase istic of the fired ceramic can depend on characteristics were separated into differ- compositions. The characteristics of the several characteristics of the raw materi- ent system elements on different levels. ceramic mix are the amounts of each als and of the ceramic mix, the function

Table III. Completed FMEA System Element: Characteristics of the fired insulator Function: Fired density Requirement: Density specification Risk Responsibility Action Results Potential Potential Potential Current Current Priority Action Recommend- and Target Severity Occurrence Detection Risk Action Failure Severity Failure Failure Preventive Occurrence Detection Detection Number Priority ed Actions Completion Priority Priority Effect Mode Cause Control Controls Date Number Dielectric 8 Fired Milled DOE on 2 Laser 2 32 Low None – all strength Density Particle particle Scattering current is too low is too Size is size Method design low too large Prototype controls are Testing adequate.

Calcined DOE on 2 Chemical 2 32 Low None – all alumina ceramic Analysis current concentra-- composi- by XRF design tion is tion Prototype controls are too low Testing adequate.

Calcined DOE on 2 2 32 Low None – all alumina raw BET current specific materials method design surface controls are area is Prototype adequate. too low Testing

Calcined DOE on 2 Laser 2 32 Low None – all alumina raw Scattering current ultimate materials Method design crystal size Prototype controls are is too large Testing adequate.

32 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 analysis becomes a complex network of prototype testing has been conducted, can anticipate and prevent problems, causes and effects. FMEA software, such including building spark plugs and put- save money, and provide a guide to a as APIS4 or Q-SYS,5 provide a tool for ting them in engines. Therefore, a prob- safer, more reliable product or process. navigating these complex networks of lem with the design would be detected, The steps to performing Design interactions. Once the function analysis and detection gets a rating of 2. FMEA are first to define the boundar- is completed, the FMEA software will The severity, occurrence, and detec- ies of the system and then to develop show any system element and all other tion ratings are combined to determine the structure analysis, which shows how system elements that are linked to it. the areas of highest risk—the weaknesses the different components of the system The next step is failure analysis. of the design. Earlier FMEA methodol- interact. Next, functions are assigned Figure 5b shows the failure net corre- ogy by the Automotive Industry Action to each element of the system and the sponding to Figure 5a. One failure mode Group, a U.S. industry group, used a functions are linked based on cause and is that the fired density is too low, or risk priority number (RPN), which was effect. Failures are then assigned to each more specifically, the specification for calculated by multiplying the three rat- function and the failures are linked, fired density is too low. One effect of ings, and the areas with highest RPN again based on cause and effect. Risk is this failure mode is that the dielectric were identified as needing improvement. assigned to each failure mode and the strength is too low, which would lead Some companies would set a threshold areas of highest risk are identified in to an increased likelihood of dielectric value for RPN (such as >100 or >150) order to optimize the product and reduce failure. Low fired density also results in where improvements would be required. the overall risk. Finally, the results are degradation of other properties: mechan- For this example, the RPN = 8 x 2 x 2 = documented and communicated. ical strength, chemical resistance, and 32, which is well below the more strin- The FMEA is a living document and thermal conductivity. The failure causes gent threshold of 100, hence no further needs to be updated over the life cycle for low density are not enough calcined action is required. A weakness with the of the product as more information alumina in the mix, milled particle size RPN is that it assumes equal weighting becomes available or as changes are too large, and the raw material being of severity, occurrence, and detection. implemented. For a ceramic material, improperly specified. The current joint methodology by the the well-known relationships between The tree structure is valuable for visu- Automotive Industry Action Group and performance, properties, characteristics alizing all of the relationships between Verband der Automobilindustrie (see (structure and chemistry), and process- the different elements. However, for sidebar: “History of FMEA…”) uses an ing of materials were used to establish risk analysis, optimization, and results action priority, which is a more complex the cause and effects relationships of the documentation, visualization is easier function of severity, occurrence, and Design FMEA. with a table. The table is considered to detection, that places the highest weight be the standard format for documenting on severity and the least weight on About the authors the completed FMEA, with groupings of detection. In the example in Table III, William J. Walker, Jr. is manager of columns containing the structure analy- the action priority (determined from materials engineering for the ignition sis, function analysis, failure analysis, the FMEA Handbook) is low, so no products group at Tenneco Inc. Contact risk analysis, and optimization for each further action is required. If, however, Walker at [email protected]. focus element. With FMEA software, the action priority was high, counter- it is easy to shift between the tree struc- measures would be needed to lower the References ture and the tabular format. In fact, action priority, which is Step 6, optimi- 1Failure modes and effects analysis—FMEA the software is necessary to develop the zation. In the automotive industry, the Handbook, Automotive Industry Action complete FMEA and to integrate it with severity is inherited from the customer Group and Verband der Automobilindustrie, the FMEAs for all of the other systems requirements, and therefore cannot be First Edition, 2019. and subsystems that make up a complex changed. The emphasis for optimiza- 2National Academy of Sciences Materials product, such as an automobile. tion should first be on reducing the Advisory Board MAB-229-M, March 1967. In Step 5, risk analysis, dielectric fail- occurrence of the failure, and second 3J.W. McCauley, “Materials characteris- ure in a spark plug is very severe, so it has on improving the detection. Reducing tics: Definition, philosophy and overview a rating of 8, corresponding to loss of pri- the occurrence is preferred because it of conference,” pp. 1–11 in Materials mary function. For prevention of this fail- involves the process of engineering the Characterization for Systems Performance and ure mode (specifying the density too low), problem out of the product, while detec- Reliability, Edited by J.W. McCauley and V. Weiss, Plenum Press, New York (1986). there is a long history of working with tion merely contains the problem. 4 similar materials and experimental work APIS IQ-Software, APIS Informationstechnologies GmbH. conducted as a “design of experiments” Summary 5 in the lab, which sets forth confidence in FMEA is a systematic method to QSys FMEA, ib seteq GmbH. 10 0 the specification. Therefore, occurrence identify weaknesses with a design or a will be low, with a rating of 2. A lot of process. When done properly, an FMEA

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 33 Hybrid composites made from metal-organic framework and inorganic glasses

By Courtney Calahoo, Louis Longley, Thomas D. Bennett, and Lothar Wondraczek

norganic glasses are a long-studied Iclass of materials, usually obtained through quenching from a liquid phase at sufficient speeds to avoid recrystallisation. The variety of glasses is vast; it comprises many subfamilies with very distinct optical, electronic, and mechanical properties. In contrast, metal-organic frameworks (MOFs) are a relatively new class of materials. They are comprised of inorganic nodes joined by organic linkers, and in their crystalline state, these materials typically display high porosity. Despite their compara- tive novelty, over 80,000 distinct crystal structures are recorded in the literature. A handful of these MOFs are shown to melt when heated in inert atmospheres, and they form glasses upon cooling.1 Albeit still small in variety, researchers have demonstrated already that this new class of MOF-derived glasses exhibit unique properties, such as the persistence of porosity in the liq- 2

uid and quenched states. Credit: Longley et al., Nature Communications Recent work shows that similar hybrid glasses also can be Figure 1. Structural chemistries. (a) Representative atomistic formed through a combination of phosphate chains and imid- structure of ZIF-62, showing ZnN4 tetrahedra connected by azolate linkers.3 Elaborating on this discovery of glass formation imidazolate (Im) and benzimidazolate (bIm) organic ligands. (b) Local structure of (1−x)([Na O] [P O ])–x([Al O ][AlF ] ) at the phosphate-imidazolate join, we fabricated amorphous 2 1.6 2 5 2 3 3 y organic–inorganic composites.4 These composites were prepared glass series. Key: N – light blue, Zn – purple, C – dark grey, P –blue, O – red, Al – light grey, F – orange, Na – green, H – by combining crystalline ZIF-62 (Zn(Im) (bIm) ) (Figure 1a), 1.75 0.25 omitted for clarity. Glass flow. Top-lit and side-lit z-scan digital which is a zinc imidazolate framework, with a variety of sodium microscopy images of the (agZIF-62)0.5(inorganic glass)0.5 com- fluoroaluminophosphate glass powders, (1–x)([Na2O]z[P2O5])– posites heat treated for 1 minute (c–d) and 30 minutes (e–f). x([AlO3/2][AlF3]y) (Figure 1b), in equal mass amounts and then Reproduced with adaptions from Ref. 4 under CC-BY license. heating both components into the liquid state. Isothermal treatment was conducted to investigate the impact of liquid phase glass transitions, identified as due to the inorganic and ZIF mixing on composite properties. glass components, in each of the composite samples. Thermogravimetric analysis, 1H nuclear magnetic resonance Electron, optical, and laser scanning microscopy revealed (NMR) spectroscopy, and Fourier transform infrared spectros- that longer isothermal heat treatments and lower inorganic copy confirmed that the integrity of the organic linkers in the glass transition temperatures produced more homogenous MOF remains unchanged on composite formation; this finding consolidated microstructures with fewer remnant particles. is in line with results observed on single phase MOF glasses.1 This finding is attributed to the increased degree of liquid PXRD results also confirmed that the composites are mainly flow allowed by less viscous (lower glass transition tempera- amorphous, though a small degree of recrystallization of a ture) melts and longer heat treatment times. In line with this dense ZIF-zni (Zn(Im)2) phase was observed, the extent of which observation, the densities of the composites fell between the depended both on treatment time and inorganic glass composi- values of the two end-members and longer heat times results tion. Differential scanning calorimetry revealed two separate in higher densities. Clear evidence of flow can be observed

34 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 a b in the side-lit images (Figure 1c–f), with bubbles, islands, and surface droplets being found in the composites. Structural studies via Raman spectroscopy and solid state 31P NMR shed light on generation of interfacial bonds between the two phases (Figure 2a). Specifically, Raman spectroscopy revealed new Na—N bonding, while solid-state nuclear magnetic resonance found evidence of organic protons in close proximity to phosphorus atoms, likely Credit: Longley et al., Nature Communications due to P—N bonding. Pair distribution Figure 2. Interface and microstructure. (a) Representation of the MOF glass—inorganic function studies confirmed that the glass interface derived from spectroscopic investigations. (b) Domain structure of the com- short-range order of both glassy phases posite as measured by energy-dispersive X-ray spectroscopy. Reproduced with adaptions remains intact on composite formation. from Ref. 4 under CC-BY license. A differential pair distribution function materials depend on the degree of mix- ability and formability of functional treatment also was used to investigate the ing in the liquid phase and therefore materials. However, the results presented atomic scale structure of the composite the degree of consolidation observed in this work indicate there also is great samples;5 however, this investigation did in the material formed on cooling. potential for new materials discovery. not reveal any unambiguous evidence of Additionally, the observation of a small new bonding in the bulk of the compos- degree of ZIF-zni recrystallisation, an About the authors ites. Energy-dispersive X-ray spectroscopy effect not previously observed in ZIF-62 Courtney Calahoo and Lothar shows clear domains originating from the liquids,1 indicates broader interactivity Wondraczek are post-doctoral fellow inorganic glass (phosphorus, aluminum) of the MOF and inorganic glass compo- and professor, respectively, at the Otto and those originating from the MOF nents at elevated temperatures. Schott Institute of Materials Research glass (zinc) (Figure 2b). As previously stated, composite for- at the University of Jena, Germany. Nanoindentation mapping revealed mation has the ability to produce new Louis Longley and Thomas D. Bennett clear separate regions of low hardness classes of materials with advantageous are Ph.D. student and Royal Society and stiffness (agZIF-62) and high hardness properties above and beyond those of University Research Fellow, respectively, and stiffness (inorganic), while much of the end-members. However, creating in the Department of Materials Science the composite material had mechanical a strong bond between materials with and Metallurgy at the University of properties between the endpoint materi- substantially different chemical, thermal, Cambridge, U.K. Contact Wondraczek at als. Longer heat treatment of 30 minutes and mechanical properties presents a [email protected]. resulted in smaller inorganic regions, challenge. Nature in her inventive par- perhaps indicating a finer grain composite simony often extracts the benefits of References and larger interfacial volume. Scratch test- composite formation in spite of these 1T. D. Bennett et al., “Melt-quenched glasses ing also confirmed the fabrication of a issues, through combining materials with of metal-organic frameworks,” J. Am. Chem. true composite material with chemically very different properties, i.e., small inor- Soc., vol. 138, no. 10, pp. 3484–3492, 2016. bonded components, with the scratch resis- ganic crystallites in an organic polymeric 2A. W. Thornton et al., “Porosity in metal- tance, i.e., indenter displacement and work protein matrix in constructions, such organic framework glasses,” Chem. Commun., of deformation, of the composite material as nacre, eggshell, or bones. Beyond the vol. 52, no. 19, pp. 3750–3753, 2016. being between the organic and inorganic benefits of a soft matrix, proteins often 3D. Umeyama, S. Horike, M. Inukai, T. component. The variable temperature Na+ provide necessary scaffolding to pro- Itakura, and S. Kitagawa, “Reversible solid- ionic conductivity of some of the compos- mote the ideal crystal growth and habit. to-liquid phase transition of coordination ite samples was investigated as well. The Clearly, emulation of this practice in polymer crystals,” J. Am. Chem. Soc., vol. 137, ionic conductivity and activation energy man-made materials such as the compos- no. 2, pp. 864–870, 2015. of the composites were found between the ites produced in this work can lead to 4L. Longley et al., “Metal-organic frame- values measured for inorganic glass and val- the discovery of useful materials. work and inorganic glass composites,” Nat. ues measured for other similar MOFs.6 Much work is yet to be done in Commun., vol. 11, no. 1, pp. 1–12, 2020. Taken together, these results indicate overcoming the issues with composite 5W. A. Sławiúski, “Calculation of pair distribu- the formation of a class of composite formation in man-made materials with tion functions for multiphase systems,” J. Appl. materials that are formed of distinct glass drastically different end-members. As Crystallogr., vol. 51, no. 3, pp. 919–923, 2018. domains originating from the inorganic indicated by Umeyama et al.,3 more sys- 6V. Nozari et al., “Sodium ion conductivity and ZIF glasses, which are bonded at tematic exploration of the design space, in superionic IL-impregnated metal-organic the interface. The nanoindentation and e.g., through creation of phase diagrams, frameworks: Enhancing stability through conductivity measurements indicate that are needed for inorganic–organic hybrid structural disorder,” Sci. Rep., vol. 10, no. 1, the functional properties of this class of materials in order to optimize process- pp. 1–9, 2020. 10 0

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 35 Figure 1. Participants in the Virtual Student Exchange Program. Top from left to right: Iva Milisavljevic (Alfred Univ., USA); Jenna Metera (UC San Diego, USA); Kana Tomita (Tokyo Inst of Tech, Japan); Amanda Bellafatto (Colorado School of Mines, USA) Middle from left to right: Rohit Malik (Univ of Seoul, Korea); Haoming Luo (Shanghai Inst Ceramics, China); Gillian Micale (MIT, USA); Yuuki Kitagawa (Kyoto Univ, Japan) Bottom from left to right: Tun Wang (Shanghai Univ, China); Tea-Hyung Kim (Seoul National Univ, Korea); Meir Sharchar (UC San Diego, USA); Chao Wang (Tsinghua Univ, China)

Building bridges in the time

tudent exchange programs represent a of Corona: Sunique opportunity for students to gain valuable research and cultural experiences, knowl- Virtual Student edge, and connections within the scientific community. Overall, these programs make a positive impact on the professional and personal develop- Exchange Program ment of every young researcher. Unfortunately, most of the funded projects and limited school funding that support graduate studies do not include or are insuffi- By Iva Milisavljevic, Jenna Metera, Kana Tomita, cient to provide opportunities for student exchange. Moreover, amid and Yiquan Wu COVID-19 and all the restrictions and travel bans that exist, engaging in exchange programs has become even more challenging. Fortunately, virtual platforms offer a way to replicate some of the in-person experiences of meetings that students currently lack. In August 2020, a group of Ph.D. students participated in a two- day virtual event called the Virtual Student Exchange Program. Alfred University professor Yiquan Wu organized this student networking event as a part of his National Science Foundation project on Collaborative Exchange Research and Materials In Ceramic Sciences (CERAMICS) program. The CERAMICS program was established by Wu with his NSF CAREER award, which is funded by the NSF Division of Materials Research Ceramics Program. Goals of the CERAMICS program include drawing more students to study ceramic

36 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 materials in the pursuit of advanced degrees, better preparing them for their future careers, and training them to be capable of performing in an international research environment at the forefront of science and engineering. During the Virtual

Student Exchange Credit: Wu group Program,12 Ph.D. students Figure 2. SEM images of (a) undoped and (b) 5 at% Nd3+ doped YAG single crystals grown using solid- from four countries gave state single crystal growth (SSCG) method. The SSCG method enables the growth of a single crystal by talks (Figure 1). These converting polycrystalline ceramics. student speakers came from the United States (5), China (3), thoughts on their experiences with dedicated to finding other people Japan (2), and South Korea (2). They student exchange programs, their and beginning collaborations for all presented to the attendees some interest- opinion on the topic, and the future future collaborations and student ing facts about their graduate research of student exchange. exchange opportunities. “I guess that institutions, university culture, research “Overall, student exchange allows the could be a cross between LinkedIn and environment, as well as some of their students to learn to think in different ResearchGate,” explains Metera. research interests and past and current ways, which is the thing that really aids in If there is something to be learned projects. For example, Iva Milisavljevic better research skills,” says Metera, who is from this whole pandemic situation, it from Alfred University presented her currently a Ph.D. student at the University is that we need to reimagine our ways of research on the potential of a novel solid- of California, San Diego. Tomita from communicating and value the potential of sate single crystal growth technique devel- Japan had a similar experience, saying, online networking more. Moreover, for oped in her lab to fabricate high-quality “In my opinion, constant lab student us to collaborate and, therefore, grow on single crystals (Figure 2). exchange is preferable. In that way, mutu- a personal and professional level, we need Participation in the Virtual Student al understanding of both the culture and to develop a positive attitude toward the Exchange Program was a worthwhile expe- research topic gets much deeper.” growth itself and open our minds to new rience for all of the students and, in a way, Concerning the current status ideas and life-long learning. their first link in a network of new connec- and availability of student exchange With that being said, we conclude with tions to share common ideas that could programs, the situation varies from a comment from one of the speakers, support the long-term partnership between institution to institution. According to Gillian Micale from the Massachusetts other researchers and their institutions. Metera’s experience, most collabora- Institute of Technology: “After this Even more importantly, the Virtual tions are organized between principal exchange program, I now believe the Student Exchange Program enabled them investigators at the university and with great barrier to collaboration is the sheer to share not only the exciting results of other institutions; students can fos- wealth of research which exists today. their research but also a piece of their ter relationships as well, but they do For collaboration to occur, we must over- lives outside the research environment. so more easily within the university. come unknown unknowns and find one As Jenna Metera, one of the speakers, Spending some time abroad, on the another in a vast world of information. says, “I feel that researchers and especially other hand, is highly encouraged at This is one of the most beautiful aspects grad students, in general, get lost in their Tomita’s university. However, many of science: by working together, we inspire work and truly identify with it. However, graduate students do not have access growth in countless ways.” the work is not our whole life, and I gen- to travel funds in their institutions, uinely enjoyed learning about the other which lowers their chances of landing About the authors aspects of the other students’ lives at their a student exchange opportunity or Iva Milisavljevic is a Ph.D. student at universities.” Learning about other cul- means they may have to look for such Alfred University. Jenna Metera is a Ph.D. tures and lifestyles of other people is one opportunities elsewhere. In that case, student at the University of California, of the most rewarding aspects of exchange a suggestion from Metera may be the San Diego. Kana Tomita is a Ph.D. stu- programs, which enrich students’ lives answer to the existing situation, espe- dent at the Tokyo Institute of Technology, and support their personal growth. cially nowadays when we are all highly Japan. Yiquan Wu is professor of ceramic After the Virtual Student Exchange engaged in different social media engineering at Alfred University. Contact 10 0 Program ended, Metera and another platforms. Metera suggests establishing Wu at [email protected]. speaker Kana Tomita shared some a centralized area or message board

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 37 LIVE VIRTUAL CONFERENCE

Materials Challenges in Alternative and Renewable Energy 2021 (MCARE 2021) 4th Annual Energy Harvesting Society Meeting (EHS 2021)

MATERIALS CHALLENGES IN ALTERNATIVE AND RENEWABLE ENERGY (MCARE 2021) Organized by The American Ceramic Society and its new Energy Materials and Systems Division, MCARE 2021 is a premier forum to address opportunities of emerging materials technologies that support sustainability of a global society. This conference brings together leading global experts from universities, industry, research and development laboratories, and government agencies to collaboratively interact and communicate materials technologies that address development of affordable, sustainable, environmentally friendly, and renewable energy conversion technologies. If your research seeks sustainable energy solutions on a global scale, you should attend MCARE 2021. This cutting-edge international conference features plenary and invited talks, thematically focused technical sessions, and poster presentations, enabling participants to network and exchange ideas with professional peers and acclaimed experts. The conference atmosphere engages and promotes the participation of scientists and engineers of all ages to include students and early-stage researchers.

MCARE 2021 ORGANIZING CO-CHAIRS

Eva Hemmer Gabrielle Steven C. Tidrow Sanjay Mathur Yoon-Bong Hahn (lead organizer) Gaustad Alfred University, U.S.A. University of Cologne, Germany Jeonbuk National University, Korea University of Ottawa, Canada Alfred University, U.S.A. [email protected] [email protected] [email protected] [email protected] [email protected]

MCARE 2021 TECHNICAL PROGRAM S10: Lifecycle Impacts of Clean Energy Materials S1: Materials for Solar Fuel Production and Applications S11: Materials for Super Ultra-Low Energy and Emission Vehicles S2: Advanced Materials for Energy Storage S3: Joint with EHS Symposium 4: Challenges in Thermal-to- S13: Theory and Experiment Meeting in Energy Materials Electrical Energy Conversion Technology for Innovative Research Novel Applications S14: Chemical and Biological Sensors: Materials, Devices S4: Advanced Materials for Perovskite and Next Generation and Systems Solar Cells S15: Young Scientists Forum on Future Energy Materials S5: Spectral Conversion Materials for Energy Applications and Devices S6: Joint with EHS Symposium 1: Materials, Components and Devices for Self-powered Electronics HONORARY SYMPOSIUM S7: Advanced Materials & Nanodevices for Sustainable and Frontiers of Solar Energy Harvesting and Functional Eco-Friendly Applications Nanomaterials: New Materials for Photovoltaics, Solar Fuels and Multifunctional Optoelectronic Devices S8: Advanced Materials for Fuel Cells and High Temperature Electrolysis (Special symposium in honor of Prof. Yoon-Bong Hahn, Jeonbuk National University) S9: Critical Materials for Energy Applications

38 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 LIVE VIRTUAL CONFERENCE SAVE THE DATE July 19–22, 2021 Materials Challenges in Alternative and ceramics.org/mcare2021 Hosted and organized by: Renewable Energy 2021 (MCARE 2021) Energy Materials and Systems Division Also organized by: 4th Annual Energy Harvesting Society Meeting (EHS 2021)

4TH ANNUAL ENERGY HARVESTING SOCIETY MEETING (EHS 2021) Since its inception, the EHS workshop has been highly successful in bringing the academic community from around the world together to openly discuss and exchange ideas about energy harvesting. Those researching energy harvesting know it has become the key to the future of wireless sensor and actuator networks for a variety of applications, including monitoring of temperature, humidity, light, and location of individuals in a building, chemical/gas sensor, structural health monitoring, and more. Join us to share your research in this area and to freely discuss and network with colleagues from around the globe interested in energy harvesting solutions.

This 4th annual meeting will feature plenary lectures, invited talks, and contributed talks within the following topical areas: • Energy harvesting (e.g., piezoelectric, inductive, photovoltaic, thermoelectric, electrostatic, dielectric, radioactive, electrets) • Energy storage (e.g., supercapacitors, batteries, fuel cells, microbial cells) • Applications (e.g., structural and industrial health monitoring, human body network, wireless sensor nodes, telemetry, personal power) • Emerging energy harvesting technologies (e.g., perovskite solar cells, shape memory EHS 2021 TECHNICAL PROGRAM engines, CNT textiles, thermomagnetics, bio-based processes) S1: Joint with MCARE Symposium 6: Materials, • Energy management, transmission, and distribution; energy-efficient electronics for Components and Devices for Self-powered Electronics energy harvesters and distribution S2: Integrated Energy Harvesting and Storage Systems for • Fluid-flow energy harvesting Wearables and IoT • Solar–thermal converters S3: Multi-functional Energy Conversion Materials and • Multi-junction energy harvesting systems Devices for Energy Harvesting and/or Sensing • Wireless power transfer S4: Joint with MCARE Symposium 3: Challenges in Thermal-to-Electrical Energy Conversion Technology EHS 2021 CO-CHAIRS for Innovative Novel Applications S5: Special Symposium — Celebrating 20 years of Energy Harvesting

SYMPOSIUM 6: Special Symposium—European Energy Harvesting Shashank Priya Jungho Ryu Yang Bai Workshop with Special Honor to Professor The Pennsylvania State Yeungnam University, Korea University of Oulu, University, U.S.A. [email protected] Finland Pim W.A. Groen [email protected] [email protected] (by Invitation Only)

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 39 SAVE THE DATE! OCTOBER 17 – 21, 2021

GREATER COLUMBUS CONVENTION CENTER | COLUMBUS, OH, USA

ACerS 123RD ANNUAL MEETING AT MS&T21

IT’S BEEN WE INVITE YOU TO JOIN US IN COLUMBUS, OHIO THIS YEAR AS WE HIGHLIGHT THE LATEST FINDINGS IN MATERIALS SCIENCE, 2 YEARS ENGINEERING, AND APPLICATION. SINCE WE CERAMIC- AND GLASS-FOCUSED SYMPOSIA: MET IN ADDITIVE MANUFACTURING • Additive Manufacturing of Ceramic-based Materials: Process Development, Materials, PERSON Process Optimization and Applications • Additive Manufacturing of High and Ultra-High Temperature Ceramics and Composites: FOR ACerS Processing, Characterization and Testing ARTIFICIAL INTELLIGENCE ANNUAL • Materials Informatics for Images and Multi-dimensional Datasets

MEETING BIOMATERIALS • Porous Materials for Biomedical Applications AT MS&T. • Next Generation Biomaterials

CERAMIC AND GLASS MATERIALS • Engineering Ceramics: Microstructure-Property- Performance Relations and Applications • Glasses and Optical Materials: Current Issues and Functional Applications • Ceramics and Glasses Modeling by Simulations and Machine Learning • Manufacturing and Processing of Advanced Ceramic Materials • Ceramic Matrix Composites • Journal of the American Ceramic Society Awards Symposium • Phase Transformations in Ceramics: Science and Applications • Preceramic Polymers; Synthesis, Processing, Modeling, and Derived Ceramics • Solid-state Optical Materials and Luminescence Properties • Thermal Shock Resistance of Ceramics and Composites

40 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Technical Meeting and Exhibition MS&T21 MATERIALS SCIENCE & TECHNOLOGY MATSCITECH.ORG/MST21

ELECTRONIC AND MAGNETIC MATERIALS SPECIAL TOPICS • Functional Defects in Electroceramic Materials • 50 Years of Characterizing Structural Ceramics and Glasses: Recognizing the Contributions of George Quinn • Advances in Dielectric Materials and Electronic Devices • Edward Orton Jr. Memorial Lecture ENERGY • GOMD Alfred R. Cooper Award session • Energy Materials for Sustainable Development • ACerS Education and Professional Development Symposium • Hybrid Organic-inorganic Materials for Alternative Energy • ACerS Frontiers of Science and Society – Rustum Roy Lecture FUNDAMENTALS AND CHARACTERIZATION • ACerS Richard M. Fulrath Award Session • Emergent Materials under Extremes and Decisive In Situ • ACerS Robert B. Sosman Award Symposium Characterizations • ACerS/EPDC: Arthur L. Friedberg Ceramic Engineering • Grain Boundaries, Interfaces, and Surfaces in Ceramics: Tutorial and Lecture Fundamental Structure-Property-Performance Relationships • Research Lightning Talks • Materials vs. Minerals: Bridging the Gap between Materials Science and Earth and Planetary Science • Online Teaching Best Practices for the COVID Era and Beyond MATERIALS-ENVIRONMENTAL INTERACTIONS • Advanced Materials for Harsh Environments • Coatings to Protect Materials from Extreme Environments • Progressive Solutions to Improve Corrosion Resistance for Nuclear Waste Storage • Thermodynamics of Materials in Extreme Environments

NANOMATERIALS • Controlled Synthesis, Processing, and Applications of Structural and Functional Nanomaterials • Mechanistic Insights into the Synergistic Properties of Nanocomposites • Nanotechnology for Energy, Environment, Electronics, Healthcare and Industry

PROCESSING AND MANUFACTURING • 13th International Symposium on Green and Sustainable Technologies for Materials Manufacturing and Processing

• Processing and Performance of Materials Using Microwaves, Visit www.matscitech.org/MST21 and sign up Electric and Magnetic Fields, Ultrasound, Lasers, and Mechanical Work – Rustum Roy Symposium for updates about registration, • Synthesis, Characterization, Modeling and Applications of programming, hotel and travel, exhibits, Functional Porous Materials student events, and more!

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 41 rld of Scie o nc W e A Submit your abstract before July 31, 2021 ceramics.org/pacrim14 | Dec. 12–17, 2021

TH PACRIM PACIFIC RIM CONFERENCE ON a nd gy Technolo 14CERAMIC AND GLASS TECHNOLOGY including Glass & Optical Materials Division Meeting (GOMD 2021) Hyatt Regency Vancouver | Vancouver, BC, Canada

PACRIM14 will provide a unique forum for knowledge exchange and sharing, and facilitate the establishment of new contacts from all over the world. The technical program will cover a wide range of exciting and emerging topics organized into a seven-track system, which includes 42 symposia planned that will identify global challenges and opportunities for various ceramic technologies. TRACKS Ceramics for Energy Systems Multiscale Modeling, Simulation, and Characterization S24: Solid oxide fuel cells and hydrogen technologies S25: Direct thermal to electrical energy conversion materials, S1: Characterization and modeling of ceramic interfaces: Structure, applications, and thermal energy harnessing challenges bonding, and grain growth S26: Materials for solar thermal energy conversion and storage S2: Frontier of modeling and design of ceramics and composites S27: Advanced materials and technologies for electrochemical energy S3: Advanced structure analysis and characterization of ceramics storage systems Innovative Processing and Manufacturing S28: Atomic structure and electrochemical property diagnosis toward S4: Novel, green, and strategic processing and manufacturing technologies full crystal rechargeable batteries S5: Polymer derived ceramics (PDCs) and composites S29: Ceramics and ceramic matrix composites for next generation S6: Advanced powder processing and manufacturing technologies nuclear energy S7: Synthesis, processing, and microstructural control of materials using S30: High temperature superconductors: Materials, technologies, and electric currents, magnetic fields, and/or pressures systems S8: Porous ceramics: Innovative processing and advanced applications Ceramics for Environmental Systems S9: Additive manufacturing and 3D printing technologies S31: Advanced functional materials, devices, and systems for environ- S10: Sol-gel processing and related liquid-phase synthesis of ceramics mental conservation, pollution control, and critical materials S11: Layered double hydroxides: Science and design of binding field S32: Ceramics for enabling environmental protection: Clean air and water with charged layers S33: Photocatalysts for energy and environmental applications S12: Specific reaction field and material fabrication design S34: Glass and ceramics for nuclear waste treatment and sequestration Nanotechnology and Structural Ceramics Biomaterials, Biotechnologies, and Bioinspired S13: Novel nanocrystal technologies for advanced ceramic materials Materials and devices S35: Advanced additive manufacturing technologies for bio-applications; S14: Functional nanomaterials for energy harvesting and solar fuels materials, processes, and systems S15: Engineering ceramics and ceramic matrix composites: Design, S36: Advanced multifunctional bioceramics and clinical applications development, and applications S37: Material and technology needs for medical devices, sensors, and S16: Advanced structural ceramics for extreme environments tissue regeneration S17: Multifunctional coatings for structural, energy, and environmental S38: Nanotechnology in medicine applications S39: Biomimetics and bioinspired processing of advanced materials S18: Advanced wear resistant materials: Tribology and reliability S19: Geopolymers: Low energy and environmentally friendly ceramics Special Topics S40: 6th International Richard M. Fulrath Symposium, “Frontiers of Multifunctional Materials and Systems ceramics for a sustainable society” S20: Multiferroic materials, devices, and applications S41: Advancing the global ceramics community: fostering diversity in an S21: Crystalline materials for electrical, optical, and medical applications ever-changing world S22: Microwave dielectric materials and their applications S42: Young Investigator Forum: Next-generation materials for multifunc- S23: Transparent ceramic materials and devices tional applications and sustainable development, and concurrent societal challenges in the new millennium 42 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 ACerS meeting highlights

56th Refractories Symposium honors Richard C. Bradt despite pandemic

Credit all images: ACerS he emerging coronavirus pandemic forced cancellation in March 2020 Tof the 56th Annual St. Louis Section/ Refractory Ceramic Division Refractories Symposium. Unfortunately, the pandemic situation precluded an in-person gather- ing in 2021, too, prompting organizers to proceed with the symposium in an online virtual format on March 24–25, 2021. “Even though we couldn’t be in person this year, the Refractories family still reunited for a fun two days. Each speaker is a famil- Jeff Smith (left) introduces 2020 Theodore Planje Award winner, Tom Vert, who is displaying his award. iar face for most of the attendees, which I president of UNITECR 2021 (now 2022), gave in the January 2018 issue of JACerS (pp. believe helped the audience stay focused the 2020 Planje Award lecture. His engaging 4171-4183). and connected to the virtual meeting,” says talk, titled “Top ten things they don’t tell you Next year, the 57th Refractories Symposium co-organizer Kelley Wilkerson, assistant in university about the refractory industry,” will be held in conjunction with UNITECR in teaching professor at the Missouri Univer- noted that “what happens in the lab and Chicago, Ill., March 15–18, 2022 (originally sity of Science and Technology. in the steel plant are two different things.” scheduled for Sept. 14–17, 2021). The 56th symposium honored the late Rich- His tips covered a wide range, including “Missing the symposium in 2020 meant we ard Bradt, one of the great luminaries in the that customers can be grumpy, never check had a lot to do this year, and it was amazing refractories industry. Speakers reflected on luggage, teamwork is essential, there are no to work with the Society, PCSA, and Bravura the impact he had on them personally and friends during breakout investigation, and to make it happen. I am so thankful for his tremendous global influence. Bradt was lifelong friendships are inevitable. everyone’s hard work to make this event a an ACerS Distinguished Life Member and The 2021 Planje Award winner, Ruth Engel, success, and I can’t wait to see everyone in Fellow of The American Ceramic Society. Refractory Consulting Services, also worked person again soon,” says Wilkerson. 10 0 Charles Semler of Semler Materials in the steel industry. Her talk, “The path to Services spoke about Bradt’s “early” career planning is SERENDIP- years, comprising the first 30 or so years ITY,” highlighted key nodes and of his career. From the beginning, Bradt’s lessons from her 25-year career research focused on structure–property as a refractories engineer with relationships with an emphasis on mechan- Armco/AK Steel. She says, “One ical properties, especially the application thing that has never changed of fracture mechanics to brittle materials. is that refractories are always He applied rigorous quantitative methods, blamed for the operations used statistics, looked for correlations, and problems. When you have a adopted modeling and visual imaging to refractory problem, the opera- improve understanding of refractories. tion stops.” “Dick was highly instrumental in pushing our RCD also presented its Allen industry into the modern era,” says Semler. Award to Bruno Luchini, Joern Grabenhorst, Jens Fruhstor- Despite being online, nearly 180 people fer, Victor C. Pandolfelli, and registered for the event to hear 19 talks over Christos G., Aneziris for their two days. Highlights included the presen- paper, “On the nonlinear tation of the St. Louis Section’s Theodore behavior of Young’s modulus Planje Award for 2020 and 2021. Tom Vert, of carbon-bonded alumina at Ruth Engel’s first hardhat. Engel was the 2021 St. Louis Section Theodore retired from Dofasco/Arcelor Mittal and high temperatures,” published Planje Award winner.

American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 43 resources

Calendar of events

April 2021 October 2021 23–28 46th International Conference and Expo on Advanced Ceramics and 25–30 International Congress 12–15 International Research Composites (ICACC2022) – Hilton on Ceramics (ICC8) – Bexco, Busan, Conference on Structure and Daytona Beach Oceanfront Resort, Korea; www.iccs.org Thermodynamics of Oxides/carbides/ nitrides/borides at High Temperature Daytona Beach, Fla.; (STOHT) – Arizona State University, https://ceramics.org/icacc2022 27–28 Glass International Ariz.; https://mccormacklab.engineering. Digital Forum – VIRTUAL ucdavis.edu/events/structure-and-ther- March 2022 EVENT ONLY; modynamics-oxidescarbidesnitridesbo- https://www.glass-international.com/ rides-high-temperatures-stoht2020 15–18 17th Biennial Worldwide glass-international-digital-forum Congress Unified International 17–21 ACerS 123rd Annual Meeting Technical Conference on Refractories – May 2021 with Materials Science & Technology Hilton Chicago, Chicago, Ill.; 2021 – Greater Columbus Convention 3–7 th https://ceramics.org/unitecr2021 6 International Conference on Center, Columbus, Ohio; Competitive Materials and Technology https://ceramics.org/mst21 Processes (ic-cmtp6) – Hunguest Hotel May 2022 Palota, Miskolc-Lillafüred, Hungary; 20–21 ceramitec conference 2021 – 22–26 Glass and Optical Materials www.ic-cmtp6.eu Messe München; Munich, Germany; Division Annual Meeting (GOMD 2022) 16–19 https://www.ceramitec.com/en/ – Hyatt Regency Baltimore, Baltimore, Ultra-high Temperature trade-fair/ceramitec-conference Md.; https://bit.ly/3ftnJqI Ceramics: Materials for Extreme – Environment Applications V The 18–20 Flourine Forum 2021 – Pan June 2022 Lodge at Snowbird, Snowbird, Utah; Pacific Hanoi, Vietnam; 22–26 ACerS 2022 Structural Clay http://bit.ly/5thUHTC http://imformed.com/get-imformed/ Products Division & Southwest forums/fluorine-forum-2020 June 2021 Section Meeting in conjunction with the National Brick Research Center 25–27 China Refractory Minerals 21–24 The NSMMS & CRASTE Meeting – Omni Charlotte Hotel, Forum 2021 – InterContinental, Joint Symposia – Bethesda North Charlotte, N.C.; https://bit.ly/31zyfob Dalian, China; http://imformed.com/ Marriott Hotel & Conference Center, get-imformed/forums/china-refractory- Rockville, Md.; https://www. July 2022 minerals-forum-2020 usasymposium.com/space/default.php 24–28 Pan American Ceramics 28–30 MagForum 2021: Magnesium November 2021 Congress and Ferroelectrics Meeting Minerals and Markets Conference – 1–4 82nd Conference on Glass of Americas (PACC-FMAs 2022) – Grand Hotel Huis ter Duin, Noordwijk, Problems – Greater Columbus Hilton Panama, Panama City, Panama; Amsterdam; http://imformed.com/get- Convention Center, Columbus, Ohio; https://ceramics.org/PACCFMAs imformed/forums/magforum-2020 http://glassproblemsconference.org July 2024 July 2021 December 2021 14–19 International Congress 12–17 th 19–22 Materials Challenges 14 Pacific Rim Conference on Ceramics – Hotel Bonaventure, in Alternative & Renewable on Ceramic and Glass Technology Montreal, Canada; www.ceramics.org Energy 2021 (MCARE 2021) (PACRIM 14) – Hyatt Regency th Vancouver, Vancouver, British Columbia, combined with the 4 Annual Energy Dates in RED denote new event in Canada; www.ceramics.org/PACRIM14 Harvesting Society Meeting (EHS this issue. 2021) – VIRTUAL EVENT ONLY; Entries in BLUE denote ACerS https://ceramics.org/mcare2021 January 2022 events. 18–21 Electronic Materials and August 2021 Applications 2022 (EMA 2022) – denotes meetings that ACerS cosponsors, endorses, or other- 31–Sept 1 th DoubleTree by Hilton Orlando at Sea 6 Ceramics Expo – wise cooperates in organizing. Cleveland, Ohio; https://ceramics.org/ World Conference Hotel, Orlando, Fla.; https://ceramics.org/ema2022 event/6th-ceramics-expo denotes virtual meeting

44 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 PROOF of your advertisement for insertion in the FEBRUARY issue

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46 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Call for contributing MAY 2021 editors for ACerS-NIST ADINDEX Phase Equilibria ‡Find us in ceramicSOURCE 2021 Buyer’s Guide AMERICAN CERAMIC SOCIETY Diagrams Program bulletin Professors, researchers, retirees, post-docs, and graduate students ...

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American Ceramic Society Bulletin, Vol. 100, No. 4 | www.ceramics.org Celebrating 100 years 47 deciphering the discipline Alessandro De Zanet A regular column offering the student perspective of the next generation of ceramic and glass Guest columnist scientists, organized by the ACerS Presidents Council of Student Advisors.

Joining of similar and dissimilar materials

An oft-cited adage in industry is “whenever possible, avoid joining.” Often the discontinuity formed in a component during joining results in the creation of a weaker area, leading

to lower performances there compared Credit: De Zanet to the surrounding material. However, Surface of a carbon fiber reinforced silicon carbide (C/SiC) specimen before the joints often cannot be avoided, and so atmospheric-pressure plasma jet treatment (left) and after the treatment (right). different strategies must be proposed. performance of joints. Glass-ceramics inexpensive, and it can be applied to It is possible to choose between provide the advantage of offering the large components and/or large batches. mechanical joining, such as clasps and desired properties for the application, To date, we have worked on carbon latches; direct joining, i.e., welding; though achieving this benefit requires fiber reinforced carbon and carbon fiber or indirect joining, such as brazing or designing an appropriate chemical com- reinforced silicon carbide, obtaining adhesive joints. Any of these techniques position and choosing a proper devitri- good results both in term of selective can be used to join similar or dissimilar fication process. For dissimilar joints, removal and increment of the surface materials, but when the latter are bond- the joining material must provide a well- area (Figure 1). Future activities will focus ed together, some additional challenges bonded interface on both materials and on assessing the effectiveness of this treat- arise because of their different physical should minimize the difference of the ment as joint strength enhancer when and/or chemical properties. coefficient of thermal expansion, thus brazing alloys are used as joining materials. Technical ceramics often need to be reducing detrimental residual stresses. joined with themselves or integrated For more than 25 years, my research References with other materials to develop devices group has actively researched join- 1M. Ferraris, V. Casalegno, F. Smeacetto, M. that operate in challenging environ- ing solutions for ceramics. We have Salvo. “Glass as a joining material for ceramic ments. Their intrinsic brittleness makes developed a strong knowledge on glass- matrix composites: 25 years of research at the process of preparing them for ceramics as joining materials1 and have Politecnico di Torino,” Int. J. Appl. Glas. Sci. mechanical joining complex; further- designed new joining processes, for 11 (2020) 569–576. https://doi.org/10.1111/ more, this choice would not be effective example, the refractory metals-wrap tech- ijag.15032. if sealing is required by the application. nique, which provides a joining material 2P.K. Gianchandani, V. Casalegno, M. Salvo, Few solutions for direct joining of that consists of a silicon matrix dispersed M. Ferraris, I. Dlouhý. “‘Refractory metal, technical ceramics exist. One option with reaction-derived silicide particles.2 RM – wrap’: A tailorable, pressure-less join- is to carry out direct bonding, but this As a second-year Ph.D. student, my ing technology,” Ceram. Int. 45 (2019) 4824– 4834. https://doi.org/10.1016/ option involves solid-state diffusion. For doctoral research activity focuses on sur- j.ceramint.2018.11.178. ceramics, solid-state diffusion requires face modification of ceramic matrix com- 3 high temperatures and pressures plus posites (CMCs) and ceramics to enhance F. Valenza, V. Casalegno, S. Gambaro, M.L. Muolo, A. Passerone, M. Salvo, M. Ferraris, extended times, making the process the joint strength. Concerning CMCs, the “Surface engineering of SiC f /SiC compos- unaffordable. Some works on laser weld- objective is to induce a selective removal ites by selective thermal removal,” Int. J. Appl. ing of ceramics have been recently pub- of fibers, creating a brush-like structure on Ceram. Technol. 14 (2017) 287–294. lished, but large-scale industrialization of the surface. In a previous work,3 this type https://doi.org/10.1111/ijac.12618. this process is not yet achieved. of structure was generated through a ther- Indirect joining is a common choice mal treatment, but a detrimental effect on Alessandro De Zanet is a Ph.D. stu- for joining ceramics and ceramic-based mechanical properties was reported. dent in materials science and technology materials. Glue can be a solution for To prevent negative effects on at Politecnico di Torino, Italy. His acti- low-temperature applications; for high- mechanical properties, we now are vities are carried out under the direction temperature applications, brazing alloys exploiting atmospheric-pressure plasma of professors Valentina Casalegno and or glass-ceramics should be considered. jet (APPJ) to confine the treatment Milena Salvo. In his spare time, he enjoys Reactive brazing alloys lead to the forma- only to the surface. Furthermore, this reading nonfiction books on social scien- tion of a reaction layer at the ceramic- technique is more ecofriendly compared ces and innovation, playing boardgames, alloy interface, which improves the with other traditional techniques, quite and walking. 10 0

48 Celebrating 100 years www.ceramics.org | American Ceramic Society Bulletin, Vol. 100, No. 4 Your kiln, Like no other.

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Your kiln Ad.indd 1 6/30/20 7:55 AM yttrium iron garnet glassy carbon photonics fused quartz beamsplitters piezoceramics europium phosphors additive manufacturing III-IV semiconductors ITO 1 1 2 2 H He 1.00794 4.002602 Hydrogen transparent conductive oxides sol-gel process bioimplants Helium YSZ 3 2 4 2 5 2 6 2 7 2 8 2 9 2 10 2 1 2 3 4 5 6 7 8 Li Be B C N O F Ne 6.941 9.012182 10.811 12.0107 14.0067 15.9994 18.9984032 20.1797 zeolites Lithium Beryllium raman substrates barium uoride Boron Carbon Nitrogen Oxygen FluorinenanoNeon ribbons 11 2 12 2 13 2 14 2 15 2 16 2 17 2 18 2 8 8 8 8 8 8 8 8 1 2 3 4 5 6 7 8 Na Mg Al Si P S Cl Ar 22.98976928 24.305 26.9815386 28.0855 30.973762 32.065 35.453 39.948 anode Sodium Magnesium sapphire windows anti-ballistic ceramicsAluminum Silicon Phosphorus Sulfur Chlorine Argon silicates 19 2 20 2 21 2 22 2 23 2 24 2 25 2 26 2 27 2 28 2 29 2 30 2 31 2 32 2 33 2 34 2 35 2 36 2 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 10 11 13 13 14 15 16 18 18 18 18 18 18 18 18 K 1 Ca 2 Sc 2 Ti 2 V 2 Cr 1 Mn 2 Fe 2 Co 2 Ni 2 Cu 1 Zn 2 Ga 3 Ge 4 As 5 Se 6 Br 7 Kr 8 39.0983 40.078 44.955912 47.867 50.9415 51.9961 54.938045 55.845 58.933195 58.6934 63.546 65.38 69.723 72.64 74.9216 78.96 79.904 83.798 oxides Potassium Calcium Scandium Titanium Vanadium Chromium Manganese Iron Cobalt Nickel Copper Zinc Gallium Germanium Arsenic Selenium Bromine Krypton cermet 37 2 38 2 39 2 40 2 41 2 42 2 43 2 44 2 45 2 46 2 47 2 48 2 49 2 50 2 51 2 52 2 53 2 54 2 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 8 8 9 10 12 13 13 15 16 18 18 18 18 18 18 18 18 18 Rb 1 Sr 2 Y 2 Zr 2 Nb 1 Mo 1 Tc 2 Ru 1 Rh 1 Pd Ag 1 Cd 2 In 3 Sn 4 Sb 5 Te 6 I 7 Xe 8 85.4678 87.62 88.90585 91.224 92.90638 95.96 (98.0) 101.07 102.9055 106.42 107.8682 112.411 114.818 118.71 121.76 127.6 126.90447 131.293 Rubidium Strontium Yttrium Zirconium Niobium Molybdenum Technetium Ruthenium Rhodium Palladium Silver Cadmium Indium Tin Antimony Tellurium Iodine Xenon

TiCN 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 h-BN 55 56 57 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 8 8 9 10 11 12 13 14 15 17 18 18 18 18 18 18 18 18 Cs 1 Ba 2 La 2 Hf 2 Ta 2 W 2 Re 2 Os 2 Ir 2 Pt 1 Au 1 Hg 2 Tl 3 Pb 4 Bi 5 Po 6 At 7 Rn 8 132.9054 137.327 138.90547 178.48 180.9488 183.84 186.207 190.23 192.217 195.084 196.966569 200.59 204.3833 207.2 208.9804 (209) (210) (222) Cesium Barium Lanthanum Hafnium Tantalum Tungsten Rhenium Osmium Iridium Platinum Gold Mercury Thallium Lead Bismuth Polonium Astatine Radon

87 2 88 2 89 2 104 2 105 2 106 2 107 2 108 2 109 2 110 2 111 2 112 2 113 2 114 2 115 2 116 2 117 2 118 2 ZnS 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 InGaAs 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 18 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 18 18 18 32 32 32 32 32 32 32 32 32 32 32 32 32 32 32 8 8 9 10 11 12 13 14 15 17 18 18 Nh 18 18 Mc 18 18 Ts 18 Og 18 Fr 1 Ra 2 Ac 2 Rf 2 Db 2 Sg 2 Bh 2 Hs 2 Mt 2 Ds 1 Rg 1 Cn 2 3 Fl 4 5 Lv 6 7 8 (223) (226) (227) (267) (268) (271) (272) (270) (276) (281) (280) (285) (284) (289) (288) (293) (294) (294) Francium Radium Actinium Rutherfordium Dubnium Seaborgium Bohrium Hassium Meitnerium Darmstadtium Roentgenium Copernicium Nihonium Flerovium Moscovium Livermorium Tennessine Oganesson Si3N4 epitaxial crystal growth cerium oxide polishing powder rutile 58 2 59 2 60 2 61 2 62 2 63 2 64 2 65 2 66 2 67 2 68 2 69 2 70 2 71 2 8 8 8 8 8 8 8 8 8 8 8 8 8 8 18 18 18 18 18 18 18 18 18 18 18 18 18 18 19 21 22 23 24 25 25 27 28 29 30 31 32 32 9 8 8 8 8 8 9 8 8 8 8 8 8 9 Ce 2 Pr 2 Nd 2 Pm 2 Sm 2 Eu 2 Gd 2 Tb 2 Dy 2 Ho 2 Er 2 Tm 2 Yb 2 Lu 2 140.116 140.90765 144.242 (145) 150.36 151.964 157.25 158.92535 162.5 164.93032 167.259 168.93421 173.054 174.9668 quantum dots Cerium Praseodymium Neodymium Promethium Samarium Europium Gadolinium Terbium Dysprosium Holmium Erbium Thulium Ytterbium Lutetium spintronics 90 2 91 2 92 2 93 2 94 2 95 2 96 2 97 2 98 2 99 2 100 2 101 2 102 2 103 2 8 8 8 8 8 8 8 8 8 8 8 8 8 8 18 18 18 18 18 18 18 18 18 18 18 18 18 18 32 32 32 32 32 32 32 32 32 32 32 32 32 32 18 20 21 22 24 25 25 27 28 29 30 31 32 32 10 9 9 9 8 8 9 8 8 8 8 8 8 8 Th 2 Pa 2 U 2 Np 2 Pu 2 Am 2 Cm 2 Bk 2 Cf 2 Es 2 Fm 2 Md 2 No 2 Lr 3 SiALON 232.03806 231.03588 238.02891 (237) (244) (243) (247) (247) (251) (252) (257) (258) (259) (262) YBCO Thorium Protactinium Uranium Neptunium Plutonium Americium Curium Berkelium Californium Einsteinium Fermium Mendelevium Nobelium Lawrencium GDC transparent ceramics chalcogenides nanodispersions perovskites scintillation Ce:YAG superconductors fuel cell materials laser crystals sputtering targets TM CVD precursors deposition slugs Now Invent. silicon carbide MBE grade materials beta-barium borate alumina substrates solar energy The Next Generation of Material Science Catalogs lithium niobate photovoltaics Over 15,000 certi ed high purity laboratory chemicals, metals, & advanced materials and a magnesia state-of-the-art Research Center. Printable GHS-compliant Safety Data Sheets. Thousands of ber optics new products. And much more. All on a secure multi-language "Mobile Responsive” platform. thin lm MgF2 dialectric coatings ultra high purity materials borosilicate glass metamaterials

American Elements opens a world of possibilities so you can Now Invent! superconductors www.americanelements.com indium tin oxide