PIM International Vol 8 No 1 March 2014

in this issue Company visit: Ortho Organizers HIP of MIM components Profile: Centorr Vacuum Industries

Published by Inovar Communications Ltd www.pim-international.com

MIM in China Publisher & editorial offices Inovar Communications Ltd 2 The Rural Enterprise Centre Battlefield Enterprise Park Shrewsbury SY1 3FE, United Kingdom Tel: +44 (0)1743 454990 Fax: +44 (0)1743 469909 Email: [email protected] Web: www.pim-international.com

Managing Director and Editor Nick Williams Tel: +44 (0)1743 454991 For the metal, ceramic and carbide injection moulding industries Email: [email protected]

Publishing Director Paul Whittaker Tel: +44 (0)1743 454992 Email: [email protected] New opportunities

Consulting Editors Professor Randall M German in established markets Associate Dean of Engineering, Professor of Mechanical Engineering, San Diego State University, USA Welcome to the first issue ofPIM International for 2014. With the Dr Yoshiyuki Kato PM World Congress scheduled for May 2014, those in our industry Kato Professional Engineer Office, Yokohama, Japan will once again have an unmissable opportunity to get together Dr Professor Frank Petzoldt Deputy Director, Fraunhofer IFAM, Bremen, Germany with parts producers, industry suppliers and leading researchers Bernard Williams from around the world to share information and discover new Consultant, Shrewsbury, UK opportunities. We look forward to exhibiting at PM2014 Orlando in May and hope to see you in the exhibit hall. Advertising Jon Craxford, Advertising Director Tel: +44 (0) 207 1939 749 This issue of PIM International features two reports on PIM in the Fax: +44 (0) 1743 469 909 dental sector, one of the most important markets for PIM globally, E-mail: [email protected] but particularly in North America. “PIM in the dental sector: From

Subscriptions orthodontic components to implants” reviews the growth of this Powder Injection Moulding International is published sector and the new opportunities for the future (page 33), whilst on a quarterly basis. The annual subscription charge our report on a visit to Ortho Organizers provides real insight into for four issues is £135.00 including shipping. Rates in € and US$ are available on application. the use of MIM at a captive facility (page 38).

Accuracy of contents We also review the use of Hot Isostatic Pressing (HIP) for the Whilst every effort has been made to ensure the processing of MIM parts to full density. As our report reveals, accuracy of the information in this publication, there are many reasons to consider the HIP process, however the publisher accepts no responsibility for errors or omissions or for any consequences arising there are also several important considerations to bear in mind in there from. Inovar Communications Ltd cannot be order to gain the desired benefits page( 43). held responsible for views or claims expressed by contributors or advertisers, which are not necessarily As our industry continues to grow many part producers are those of the publisher. feeling real pressure on their production capacity. The potential Advertisements for investments in new furnaces is therefore generating a lot of Although all advertising material is expected to interest in the industry from furnace manufacturers. We profile conform to ethical standards, inclusion in this publication does not constitute a guarantee or Centorr Vacuum Industries, one of North America’s longest endorsement of the quality or value of such product established suppliers of high temperature vacuum furnaces, or of the claims made by its manufacturer. and review their experiences of the MIM industry and recent Reproduction, storage and usage commercial successes (page 51). Single photocopies of articles may be made for personal use in accordance with national copyright Looking to Asia, the recent and highly successful APMA 2013 laws. Permission of the publisher and payment of conference attracted a truly international audience and we fees may be required for all other photocopying. All rights reserved. Except as outlined above, no present a report on some MIM related highlights (page 73). We part of this publication may be reproduced, stored in also publish a paper from Zhuzhou, China’s hardmetal capital, on a retrieval system, or transmitted in any form or by the injection moulding of hardmetal cutting tool inserts (page 73). any means, electronic, photocopying or otherwise, Worldwide without prior permission of the publisher and Nick Williams copyright owner. Global manufacturer of nodular and spherical aluminum powders, Managing Director and Editor pre-alloyed aluminum powders, and aluminum premixes for PM Design and production Inovar Communications Ltd www.ampal-inc.com www.poudres-hermillon.com Printed by In the Americas Cambrian Printers, Aberystwyth, United Kingdom Supplier of carbonyl iron and atomized stainless steel powders for ISSN 1753-1497 the MIM and PM industries Vol. 8, No. 1 March 2014 Cover image © 2014 Inovar Communications Ltd A Carriere Distalizer™ appliance United States Metal Powders, Incorporated manufactured by Ortho Organizers 408 U.S. Highway 202, Flemington, New Jersey 08822 USA Tel: +1 (908) 782 5454 Fax: +1 (908) 782 3489 email: [email protected] March 2014 Powder Injection Moulding International 1 | contents page | news | events | advertisers’ index | email | | contents page | news | events | advertisers’ index | email | March 2014

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In this issue

33 PIM in the dental sector: From orthodontic 58 APMA 2013 conference: Advances in MIM components to implants applications and materials presented in Xiamen The dental sector has for many decades been an APMA 2013, the 2nd International Conference on PM in important market for the PIM industry, accounting for Asia, took place in Xiamen, China, November 3-6, 2013. around 16% of global MIM sales by value. Prof Randall Lin Dongguo and Seong Jin Park report on a number of German looks at the sector’s history and opportunities. presentations relating to MIM applications and materials.

38 Ortho Organizers: A global leader in the 67 Advances in PIM process simulation speed up development and manufacture of MIM the development of micro parts orthodontic products Simulation technology for the PIM process has advanced Ortho Organizers, Inc. supplies orthodontic products rapidly in recent years. Experts from Karlsruhe Institute to the worldwide dental market and its in-house MIM of Technology (KIT) and SIGMA Engineering GmbH operation enables the company to remain at the forefront present an overview developments that illustrate how of the manufacture of innovative orthodontic products. simulation can support mould design and quality control Prof Randall German reports on a recent visit. in micro-PIM applications.

43 An introduction to the Hot Isostatic Pressing

(HIP) of MIM components Technical paper

Using HIP to achieve full density MIM products offers a wide range of benefits. As Dr Stephen J Mashl explains, 73 The structure and performance of WC-10%Co there are however a number of considerations to bear in Cemented Carbide inserts made by PIM mind when considering the HIP of MIM parts. She Q Wang, Sunhe Liu, Wen Guanghua

51 Centorr Vacuum Industries: Celebrating 60 years of innovation in vacuum furnace Regular features production Centorr Vacuum Industries is one of North America’s 5 Industry news largest manufacturers of high temperature vacuum 72 Global PIM patents furnaces. We report on the company’s history and long association with global MIM industry. 80 Events guide, Advertisers’ index

Catamold® Imagination is the only limit! Industry News To submit news for inclusion in Powder Injection Moulding International please contact Nick Williams [email protected]

[ Catamold® – Inject your ideas ] ARC Group expansion New to the school this year is a course on the company’s 3D printing capabilities. Through the launch and MIM school dates of ARC’s new division, 3D Material Technologies (3DMT), announced ARC has been building up capital equipment of the newest models of metal and plastic 3D printers. 3DMT is housing ARC Group Worldwide, Inc., based in Longmont, Colorado, its 3D printers in Colorado, as well as ARC’s other facili- USA, announced in December 2013 that Advanced Forming ties. The new 3D course will allow students the unique Technology, Inc. (AFT), a division of the company’s Preci- opportunity to get hands-on experience with a number of sion Components Group, has begun expanding its opera- new 3D printing technologies. tional capabilities at its Colorado location. The 2014 classes are free to attend for registered Commenting on the expansion, Jedidiah Rust, Director applicants only, and will be held on the following of Operations for AFT Colorado, stated, “AFT continues dates from February 19-20, May 21-22, August 20-21 to experience growth within our major market segments, and November 12-13. For more information email demonstrating the quality of our products and services, [email protected]. The company states that and necessitating the need for additional capacity.” spaces are only for qualified attendees and are limited. AFT currently services five growth industries, including www.arcgroupworldwide.com automotive, medical, aerospace, firearms and consumer. Rust further commented, “In order to continue to meet our customers’ high demand, AFT has taken the initiative BASF SE GBU Carbonyl Iron Powder to increase output through infrastructure investment and and Metal Systems lean manufacturing initiatives.” Expansion completed Powder Injection Molding to-date represents the first of several phases, with the G-CA/MI – J513 planned expansion expected to be complete by December 67056 Ludwigshafen, Germany 2014. Phone: +49 621 60 52835 Thomas K Houck, Vice President of US Metal Injection E-mail: [email protected] Molding Operations, stated, “This capital expansion and Internet: www.basf.de/catamold infrastructure upgrade will enable us to meet current demand and grow our business for the future. Our continued focus on operational excellence will provide the company with the strengthened ability to expand volumes, provide additional value added processes to our customers and increase our 3D printing capabilities/services. These initiatives, combined with our expected growth, should position the company for continued success with a diverse, Discover the amazing possibilities of metal and ceramic components captivated customer base, innovative technology solutions, manufacturing using Power Injection Molding with Catamold® and BASF. and increased shareholder value.”

With Catamold®, conventional injection molding machines can be used to Schedule for AFT’s “MIM School” seminars announced produce geometrically demanding components economically. You can do injection molding of metal and ceramic feedstock as easily as plastic. AFT’s MIM School, started in 2005, is a two day training And this opens up new means of producing complex components that seminar for new and existing ARC customers, vendors provide economic and technical beneﬁ ts in sectors ranging from Automotive, and shareholders wishing to learn more about the MIM Consumer Products, and Mechanical Engineering to Medical Products and process. Since the start of the school, AFT has trained Communications/Electronics. over 250 students on MIM technology. The seminar walks students through the technical aspects of MIM, Take advantage of the new diversity in Powder Injection Molding with Catamold®. Get in touch with us – we’ll be glad to help you on the road to success. from the materials technology of metal powders, to the compounding and secondary processes, through the use

®= registered trademark of BASF SE of both classroom and hands-on training on the manufacturing floor.

Arcam acquires MIM titanium powder the existing management team. “With this deal we will be a manufacturer AP&C from Raymor part of the leading company in Industries 3D-printing in metals. Because of our long term close cooperation Sweden’s Arcam AB has signed an Magnus René, President and CEO of with Arcam we know that this deal agreement to acquire the AP&C Arcam. will give us a very good platform division from Raymor Industries for a AP&C uses proprietary plasma for continued growth in the total of $35 million Canadian dollars. atomisation technology to produce 3D-printing industry. Being part The move will see Arcam secure its metal powders, with titanium alloy of a larger group will also help supply of titanium powder used in powder being the largest product. A in accelerating growth to better the production of components via the significant part of AP&C sales is to service the overall metal powder company’s Additive Manufacturing the 3D-Printing industry with other market”, stated Jacques Mallette, process. markets including Metal Injection President of Raymor Industries and AP&C is a global manufacturer of Moulding (MIM), powders for spray future President of Arcam’s powder high quality metal powders and has coatings as well as powders for business. been a supplier of titanium powders HIPed components. Arcam and the The total purchase price Choose the best in sintering. to Arcam since 2006. Titanium team at AP&C intend to continue amounts to CAD$35 million where powder is an important part of to expand the powder business and a cash payment amounting to Arcam’s offering to its customers. advance the plasma atomisation CAD$20 million will be paid on “With this acquisition Arcam technology. closing and the remaining part as secures access to the optimum The AP&C division is expected to two instalments to be made in 2015 production of high grade metal generate CAD$6.5 million of revenue and 2016 subject to certain targets powders for our customers and we during 2013 with an EBITDA result being met. Closing of the acquisition also add technology and expertise of around CAD$1.5 M. The acquired is subject to customary closing Achieving part purity in powder metal production for business, which currently employees conditions and is expected to take 3D-printing in general and other 29, will become a subsidiary of place in the first quarter 2014. through vacuum sintering. advanced applications,” stated Arcam and continue operating with www.arcam.com

When processing powder metal components, completely removing all binders and contaminants from the hot Advanced Metalworking Practices zone during the debinding process can be challenging. If not done correctly, furnace performance and part quality can be adversely affected, driving up the costs per part. The Forerunner in Powder Injection TITAN® DS is specially designed Vacuum furnace technology now exists to debind and for applications in the Powder Molding Feedstock sinter in one process cycle, not only saving heat treaters Metallurgy industry. Feedstock for Metal Injection Molding time and money, but also resulting in superior, more consistent part quality. • Precise process control for Application specific customized consistent part quality feedstocks for metals and ceramics AMP was the first to offer commercially At Advanced Metalworking Practices feedstock production is our only business. • Enhanced technical features Our products are used widely for applications in industries such as medical and available PIM feedstock. PIM feedstock orthodontic, electronics, hardware and sporting goodsSix. commercially available wax/ for high-quantity MIM polymer binder variations production is our only business. We offer full ISO 9001:2008 certified Contacts: and PM applications ® William R. Mossner R&D capabilities including trial size batches, Supplier of quality feedstock ADVAMET Dwight Webster For more information on sintering, Feedstock production from 25 lb to 1700 lb in onFeedstocke batch production batches Advanced Metalworking • Reduced door-to-door cycle Can supply customers with lower cost, off-the-shelf, Practices, LLC capillary rheometery, molding test bars, available from 10 to 770 kg 401 Industrial Drive standard 4605 Alloy Steel and 17-4 PH Stainless visit www.IpsenUSA.com/Sintering. time Carmel, IN 46032, USA debinding and sintering. Supplier of Customized feedstock made from numerous e-mail: [email protected] ferrous and non-ferrous metals and alloys. Phone: +1 317 843 1499 Fax: +1 317 843 9359 • Standardized system for use High Quality Feedstocks since 1988 Advanced Metalworking Practices, LLC around the world - longer than any other supplier 4511 West 99th Street Phone: +1 317 337 0441 www.advancedmetalworking.com Carmel [email protected] IN 46032 [email protected] ISO 9001:2008 Certified USA www.amp-llc.net

EPSON ATMIX CORPORATION New cooling system from Hasco Medical/dental prevents hot spots in injection moulding ceramics market

Hasco Hasenclever GmbH of Lüden- cross each other on the same plane, to grow to $2.3 scheid, Germany, a supplier of metric making it possible to incorporate billion by 2018 mould plates, mould components and small plate thicknesses and inex- hot runner systems, has introduced pensive accessory components in the NanoMarkets, of Glen Allen, Virginia, its new CoolCross Z99 cooling system mould design. By reducing the plate USA, has published its report “World- for injection moulds. The system thickness, use can be made of shorter wide Medical Ceramics Markets: makes possible, for the first time, to nozzles, guidance and attachment 2013” providing a detailed analysis of have cooling channels crossing each elements. emerging medical and dental market other on the same plane in a flexible Hasco states that the number of opportunities for alumina, zirconia, manner without any major outlay on cooling channels can be reduced, since silicon ceramics, hydroxyapatite, production. it is no longer necessary to have a bioglass, piezoceramics, nanoce- CoolCross permits a homogeneous cooling channel in an additional plane. ramics and other materials. The temperature distribution at the core If the CoolCross is used in thicker company forecasts worldwide or insert, as well as constant cavity plates, the installation depth can medical ceramics to grow from $1.1 cooling on all four sides for the full be selected on a variable basis. “By billion in 2013 to $2.3 billion in 2018. Finer Powder Production duration of the injection moulding employing the innovative CoolCross Ceramics are widely used in medical cycle, states Hasco. The system also Z99, which is available exclusively and dental applications including hip leaner Powder Production prevents hot spots. It also provides from Hasco for the cooling circuits and knee implants; crowns, bridges C protection against rotation, which is in injection moulds, it is possible to and other dental implants; surgical achieved through a locking mecha- achieve time and cost savings for both and diagnostic tools, implantable Shape Control of Powders nism, and prevents the unintended the mould unit and the accessory electronic implants and regenerative closure of the cooling channels. components,” the company stated. medicine. Different independent cooling circuits www.hasco.com www.nanomarkets.net

• Low Alloy Steel • High Alloy Steel • Stainless Steel • Magnetic Materials • Granulated Powder

JAPAN Mr. Numasawa, Ryo [email protected] U.S.A and SOUTH AMERICA Mr. Pelletiers, Tom ASIA and OCEANIA [email protected] Mr. Yoshida, Shunsuke [email protected] EU Dr. Pyrasch, Dieter CHINA Dieter.Pyrasch@thyssenkrupp.com Mr. Ota, Arata

Cremer_1213_Anzeige_210x148_Gelb_V2 [email protected] KOREA Mittwoch, 22. Januar 2014 14:32:56 Mr. Yun, John 8 Powder Injection Moulding International March 2014 © 2014 Inovar Communications Ltd Vol. 8 No. 1 Vol. 8 No. 1 © 2014 Inovar Communications Ltd March 2014 Powder Injection Moulding International 9 [email protected] RAI-116 PIM AD:Layout 1 8/28/12 8:24 AM Page 1

Your Premier Source for Milestone passed Amedica signs agreement with Kyocera Hydride–Dehydride (HDH) in PM scientific for silicon nitride medical devices publishing Amedica Corp, Salt Lake City, Utah, Amedica’s FDA approved spinal USA, a biomaterials company using interbody devices. and Plasma Spheroidized (PS) In early January silicon nitride ceramics for application Silicon nitride devices have been of this year in a broad range of medical devices, shown to help promote bone growth Professor Titanium Powders. has announced that it will collaborate and have anti-infective properties. Randall German, with Kyocera Industrial Ceramics They are also semi-radiolucent with Associate Dean Corp. to manufacture medical devices clearly visible boundaries enabling for Engineering using Amedica’s silicon nitride. The an exact view of intra-operative Research at silicon nitride components will be placement and post-operative fusion San Diego State produced at Kyocera’s Vancouver, assessment via common imaging University, Washington, facility and will include modalities. California, USA, passed a milestone with his 1000th AMETEK Specialty Metal Products – Reading Alloys is a leader in PS Powders: Free Flowing scientific publication. producing specialty alloys and fine powders. The company uses a • Available in CP Ti, Ti-6AL-4V Standard (Grade 5) & ELI (Grade 23) The specific article was a variety of manufacturing processes to produce titanium powders • Particle sized from 45 microns (325 mesh) to 500 microns collaborative effort with Jose that meet ISO 9001 / AS 9100 requirements. (35 mesh) Alvarado-Contreras, Eugene Olevsky and Andrey Maximenko entitled “A The company utilizes a new plasma manufacturing method • Spherical morphology, tight PSD, no satellites, agglomerates or entrapped argon continuum approach for modeling which combines an established powder manufacturing process gravitational effects on grain settling with the Plasma Spheroidization (PS) process to offer customers Powder Metallurgy Applications and shape distortion during liquid an alternative high volume, spherical titanium powder production • Plasma Spray/Coating phase sintering of tungsten heavy process. • Cold Isostatic Pressing / Sintering alloys” published in Acta Materialia • Hot Isostatic Presssing (2014, vol. 65, pp. 176-184). It detailed HDH Powders: Greater Control of PSD modelling research in preparation for • Metal Injection Moulding • Available in Ti Sponge, CP Ti, Ti-6AL-4V Standard (Grade 5) experiments to be performed on the • Additive Manufacturing & ELI (Grade 23) International Space Station in 2015. • Particle sized from 45 microns (325 mesh) to 500 microns Markets Served Now, at 1003 published articles, German is also responsible for (35 mesh) • Medical Device • Thin Film (Sputtering Target) • Feedstock fourteen books, five recorded short • Solid, angular, block or sponge morphology • Electronics • Net Shape courses, four market studies, nineteen edited books, and twenty- Morphology: HDH Magnesium Morphology: HDH Sodium Reduced Morphology: PS CP Titanium Powder five issued patents. Reduced Titanium Sponge Powder Titanium Sponge Powder Morphology: HDH CP Titanium Powder (99%+ spherical) His newest book “Sintering: From Empirical Observations to Scientific Principles” is just being released by Elsevier Scientific. His first article was in Metallurgical Transactions in 1972 and with George St. Pierre dealing with the high temperature thermodynamics of nickel-titanium alloys. He has typically aver- aged two to three co-authors per paper, involving more than 300 graduate students and postdoctoral SEM image (x100) of HDH Magnesium SEM image (x100) of HDH Sodium Reduced SEM image (x100) of HDH CP Ti Powder, SEM image (x20) of PS Ti powder, 35 mesh Reduced Ti Sponge Powder, 70 mesh Ti Sponge Powder, 70 mesh (212 m) 70 mesh (212 m) x 100 mesh (150 m) (500 microns ) x 45 mesh (355 microns) researchers working under his µ µ µ (212 m) x 100 mesh (150 m) x 100 mesh (150 m) supervision. µ µ µ

Sandvik Osprey appoints new sales 2014 APMI fellows manager for the Asian market announced

Sandvik Osprey, a leading supplier company but also new business John R Engquist, Consultant, JENS See us at: of gas atomised metal powders for development skills from his time Solutions LLC., a recognised expert the Metal Injection Moulding (MIM) working in the steel industry. We in the PM industry, and Z Zak Fang, PM CHINA industry, based in Neath, South are very excited that he is re-joining University of Utah Metallurgical April 27-29, Shanghai, China Wales, UK, has appointed Dr Paul the team at Sandvik Osprey and Engineering Professor who is a 2014 Davies as Powders Sales Manager look forward to working with him to world-renowned expert in the Booth A091 for the Asian market. grow or activities throughout Asia.” cemented carbides and titanium Davies was formerly Sales & Davies told Powder Injection industries, have been selected to Marketing Manager at Osprey Moulding International, “I am receive the 2014 Fellow Award from from to 2001 to 2008 but has spent delighted to be coming back to APMI International. the past five years working for work at Sandvik Osprey. It’s been The fellowship is APMI’s most Tata Steel Europe managing the great to see the impressive growth prestigious award, recognising development of new advanced that the company has achieved members for their significant materials for the Defence and over the past five years and I look contributions to the goals, purpose Security Industries. forward to contributing to the and mission of the organisation as Dr Martin Kearns, Powders future success of the business. well as for a high level of expertise Group Director at Sandvik Osprey, Asia is a dynamic market with in PM. The recipients will receive told Powder Injection Moulding significant potential both in Metal elevation to Fellow status at the International, “Paul brings with him Injection Moulding as well as PM2014 World Congress in Orlando not only a wealth of knowledge and other advanced Powder Metallurgy during the Industry Luncheon on experience in Powder Metallurgy applications.” May 19, 2014. from his previous time with the www.smt.sandvik.com/osprey www.mpif.org

On the leading edge of metal powder manufacture

With over 35 years’ experience in gas atomisation, Sandvik Osprey offers the world’s widest range of high quality, spherical metal powders for use in Metal Injection Moulding. Our products are used in an increasingly diverse range of applications including automotive, consumer electronics, medical and aerospace.

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on both sides of the fin to create its complex shape. Toler- MIM helps Raytheon improve ances were said to be difficult to maintain from machined product performance and lower part to machined part. Using MIM, the airfoil shape is injection moulded in one manufacturing costs piece (Fig.1 B). Because the hardened steel die cavity used in MIM does not change from shot to shot over a minimum Raytheon Company is an international with some of the latter being difficult if of a quarter of a million shots, tolerances are easily aerospace and defence supplier not impossible to produce using other achieved. After debinding, the fin is sintered at 1260°C, headquartered in Waltham, Massachu- manufacturing methods. Fig.1 Excalibur control fin. The with the sintered part containing less than 2% porosity. setts, USA, with sales exceeding $24.4 One example cited is a control fin machined part (A) and the part The airfoil is then coined to the final shape and attachment Sunrock Ceramics specializes in high billion in 2012. Writing in Raytheon for the Excalibur, a guided artillery manufactured by MIM (B) points are machined to their final dimensions. Final heat alumina industrial ceramics for the Technology Today (2013) Mitchell Gross projectile which provides precision (Courtesy Raytheon Corp) treating is undertaken to attain the strength required. most severe sintering applications stated that Metal Injection Moulding fire at extended ranges for all current Table 1 compares the properties of MIM 17-4PH mate- (MIM) is employed by the company and future 155 mm howitzers. The hardened stainless steel. Machining rial with 17-4PH precipitation hardened stainless steel, of the powder metallurgy and to produce metal structures both original Excalibur control fin (Fig. 1A) was extremely time consuming, showing that they have comparable performance. The cost technical ceramics markets. simple, complex and sophisticated, was composed of 17-4PH precipitation requiring tens of passes with a tool bit of manufacturing the control fin by MIM, however, is said to be only 25% that of the cost using traditional machining Yield Strength Ultimate Tensile Modulus Elasticity Stainless Steel Material Elongation % methods. (ksi) Strength (ksi) (Gsi) The second MIM 17-4PH H1100 138 149 14 37.9 example of a SAE AMS 5604 H1100 115 minimum 140 minimum 5 minimum 28.5 MIM application MIM 17-4PH H1025 139 158 9 42.4 at Raytheon is a radio frequency SAE AMS 5604 H1025 145 minimum 155 minimum 5 minimum 28.5 (RF) housing, MIM 17-4PH H900 164 184 10 32.1 or electronics SAE AMS 5604 H900 170 minimum 190 minimum 5 minimum 28.5 enclosure, which Fig. 2 Metal Injection Moulded RF the company uses Table 1 Properties of MIM 17-4 PH steel in comparison to precipitation hardened 17-4 PH steel (i.e., SAE AMS 5604) for housing (Courtesy Raytheon Corp) in large quantities. different heat treatment conditions (H1100, H1025, H900) MIM is said to be ideally suited to producing the thin walls and unique hole design (Fig. 2). Electronics packages normally require a thermal management system attached with an adhesive bond. The thermal management system is, therefore, limited in its ability to remove heat from the electronics package CM Furnaces, long recognized as an industrial leader in performance-proven, high because of the thermal properties of the adhesive and the temperature fully continuous sintering furnaces for MIM, CIM and traditional press bond thickness. and sinter now OFFERS YOU A CHOICE, for maximum productivity and With MIM, alloy compositions can be adjusted so that the electronics package and the thermal management elimination of costly down time. system can be co-moulded and processed together to Choose one of our exclusive BATCH hydrogen atmosphere Rapid Temp furnaces. achieve higher heat dissipation. Designed for both debinding and sintering, these new furnaces assure economical, Raytheon states the Kovar ratio of iron and nickel can simple and efficient operation. be changed to lower the coefficient of thermal expansion (CTE) of the alloy so the CTE of the alloy is closer to the CTE OR... choose our continuous high temperature sintering furnaces with complete of glass. This lower alloy CTE reduces the probability of automation and low hydrogen consumption. cracking the glass seal around package leads, a common cause for the loss of package hermeticity and of the failure CONTACT US for more information on our full line of furnaces with your of electronic components inside the package. These choice of size, automation, atmosphere capabilities and attributes are said to result in higher-value systems that temperature ranges up to 3100˚F / 1700˚C. have better performance at lower cost. www.raytheon.com

E-Mail: [email protected] FURNACES INC. Submitting News Web Site: 103 Dewey Street Bloomfield, NJ 07003-4237 To submit news to Powder Injection Moulding International http://www.cmfurnaces.com Tel: 973-338-6500 Fax: 973-338-1625 contact Nick Williams: [email protected]

Moulding and Ceramic Injection New report on the global market for Moulding has exhibited spectacular Metal and Ceramic Injection Moulding growth over the last two decades and the trend is expected to continue. BCC Research of Wellesley, Massa- nearly $2.9 billion by 2018 from $1.5 While the market crash in 2008 and chusetts, USA, has released a new billion in 2012 and register a six-year 2009 had its share of repercussions 482 page report (January 2014) compound annual growth rate of in the MIM industry, with automotive reviewing the global MIM and CIM 11.4% from 2012 to 2018. Although sales dropping significantly across components market. In the last BCC the emphasis is mainly on the MIM the world, larger companies have Research report issued in 2009 it put market, the CIM market is also weathered the storm and have grown the market size for MIM to be $985 discussed. stronger and larger in the meantime. million, with expected growth to $1.9 BCC Research stated that the Key to this staying power has been billion by 2014. Now BCC Research global market for components diversification across other applica- projects the global market to grow to manufactured by Metal Injection tions such as medical and dental, aerospace, electronics and communications and luxury products. Growth in the market for cell phones and other handheld products has been a boon to the MIM industry for the last decade and this has also resulted in the industry shifting its base slowly to emerging markets and Asia, where most of the electronics manufacturing takes place. The report discusses various trends in the geographical growth of the industry. Another significant change in the PM China 2014 - Shanghai industry is the size of the largest 27-29 April 2014 companies starting to cross the $50 million sales mark. The first two PM2014 Wold Congress MIM manufacturers to break this Orlando, FL, USA barrier, stated BCC Research, are 18-22 May 2014 visit us at Booth 508 the ARC Group, because of its recent acquisitions, and Indo-US MIM Tec. BCC Research expects that there could be five to ten players crossing the $50 million mark by 2018, with several crossing the $100 million threshold. The final chapter of the report provides detailed profiles of nearly 200 leading companies. On the supply side, several companies are expected to be PM Tooling System enjoying $50 million in purchases from the MIM industry in the next The EROWA PM tooling system is the standard few years. The supply side chapter covers powder manufacturers, feed- interface of the press tools between the stock manufacturers and equipment toolshop and the powder press machine. makers who support the MIM and CIM industry. Application markets Its unrivalled resetting time also enables are analysed in detail, particularly for you to produce small series proﬁ tably. the firearms market. The report, Global Market for Metal and Ceramic Molding, is www.erowa.com available for $6650. www.bccresearch.com

INTRODUCING ELNIK’S Metalysis’ titanium powder used to 3D The Mercury Centre, which sits within the Department of Materials at print automotive parts Sheffield University, used Renishaw’s TM 3D printer to make the parts, demon- Metalysis Ltd, Rotherham, UK, has use of this inexpensive and plentiful strating the feasibility of producing announced that low-cost titanium feedstock for titanium manufacture titanium components using additive powders developed by the company will dramatically reduce the cost layer manufacturing. 3D printing have been used to 3D print automo- of titanium production, allowing its brings further cost benefits by tive parts for the first time. increased use. reducing waste because the current The use of titanium powders in The Metalysis process is radically means of production is subtractive, as 3D printing has been prohibitively cheaper and environmentally benign components are shaped out of metal expensive until now because titanium compared with existing titanium billets, which wastes a huge amount powders currently sell for $200 - $400 production methods, states the of material. Metalysis’ low-cost CUTTING EDGE TECHNOLOGICAL ADVANCES THAT CAN SAVE YOU THOUSANDS $$ per kilogram, states Metalysis. company. Currently, the manufacture titanium powder enables additive Metalysis has developed a new way of of titanium powder involves taking the manufacturing with its metal powder, The Metal Injection Molding process can be both risky and very costly unless you have a company like Elnik Systems producing low-cost titanium powder, metal sponge produced by the Kroll thereby reducing the quantity of which it believes will heralds a new process, which is then processed into material required. working with you. The reason is simple. For over 18 years, Elnik Systems has made technological innovation its era in Additive Manufacturing and see ingot billets, melted into bar form and Dion Vaughan, CEO of Metalysis cornerstone. And innovative thinking leads to smarter MIM performance, we call “MIM-telligenceTM”. greater use of titanium in components finally atomised into powder, resulting added, “Metalysis’ rutile-derived across the automotive, aerospace and in a costly and labour-intensive titanium powder is produced at lower defence industries. four-step process. Metalysis takes cost and is suitable for 3D printing Taking it a step further, once Elnik innovates, extensive ﬁ eld testing is done before their new technology hits the market In a further development, the rutile and transforms it directly into so that manufacturing metal compo- with the help of the full-sized production furnaces at DSH Technologies LLC, a research and development sister titanium powder used to manufac- powdered titanium using electrolysis. nents becomes more economical. The company of Elnik. Elnik also offers free DSH services for one year with the purchase of each new piece of ture the automotive parts is also a The low-cost titanium powder can be Metalysis process could reduce the world-first, as Metalysis has created used in a variety of new applications price of titanium by as much as 75%, their equipment, providing every Elnik customer with additional customized technical support and dependability. titanium from rutile sand, a naturally whereas previously the metal has making titanium almost as cheap as Another Elnik “MIM-telligenceTM” beneﬁ t. occurring titanium ore present in been excessively expensive for use in specialty steels.” beach sands, in one single step. The mass production of lower value items. www.metalysis.com INNOVATIVE SYSTEM FEATURES

 AccuTemp™ proprietary thermocouple control resulting in tight temperature control High Purity Spherical Nickel Powders  Automatic Cleaning Features of binder tailored for MIM trapping components and Dry Vacuum Pump.

 ColdFinger™ Debind Trap forced ﬂ ow enhanced binder trapping.

Tapped Type 4SP nickel powder is a high purity, spherical nickel d10 d50 d90  Gas Tight Retort Design Superior gas control Density powder that is ideal for making powder metal parts SNP-400 4.4 11.4 25.2 5.57 throughout process zone, eliminating escaping where high sintered density and controlled shrinkage are 4SP-10 3.0 6.3 11.2 5.48 gas as compared to competitive designs. important. SNP-20+ 10 7.2 11.4 17.1 5.45 SNP+20 12.6 20.8 34.6 5.37  Laminar Gas Flow efﬁ cient and effective gas management for debinding and sintering. With excellent consistency, narrow PSD and spherical morphology, Type 4SP-10 nickel powder is the ideal choice  Simple Ease of Use PLC controls via Excel for the metal injection molding (MIM) industry. spreadsheet.

Novamet Specialty Products Corp. 681 Lawlins Road, Suite 10 Wyckoff, NJ 07481, USA TEL: +1 201 891 7976 FAX: +1 201 891 9467 EMAIL: [email protected] www.novametcorp.com

Nanostructured powder helps Calado, Chief Technology Officer at Innovnano, stated, “It is important improve the performance of for us to respond to and develop structural ceramics practical solutions to the increasingly demanding applications required Innovnano, a manufacturer of high Innovnano’s nanostructured 3YSZ by the ceramic industry. For this performance ceramic powders is produced via the patented reason, we provide our powders based in Coimbra, Portugal, has Emulsion Detonation Synthesis in a range of formats, enabling produced 3 mol % yttria-stabilised (EDS) manufacturing technology, our customers to explore and take zirconia (3YSZ) for high strength which ensures an even distribution advantage of the enhanced chemical structural ceramics. Manufactured of yttria throughout the zirconia and physical properties offered by to ensure retention of an intrinsic lattice. Importantly, this high a nanostructured material, but with nanostructure, Innovnano’s 3YSZ chemical homogeneity overcomes the handling ease of conventional powder provides the advantageous brittleness and supports a constant microstructured feedstock.” properties associated with small coefficient of thermal expansion, Compared to microstructured grain sizes, including high chemical negating any risk of thermal stress ceramic powders, powders with homogeneity and density. Ideal for and subsequent material fracture for an inherent nanostructure show technical ceramics such as valves and steadfast reliability. Furthermore, with increased chemical activity. process equipment, nanostructured an expansion coefficient similar to Importantly this enables ceramics 3YSZ feedstock translates to ceramic steel, nanostructured 3YSZ is an ideal to be produced at lower sintering components with exceptional bending corrosion-resistant alternative for (processing) temperatures, reducing strength, fracture resistance and traditional steel components. energy costs and minimising tribological performance, to withstand For optimal processability and grain growth. In this way, the the strain and friction that is placed user-handling, Innovnano’s 3YSZ nanostructure is retained, translating FCT Anlagenbau GmbH on moving parts and structural can be supplied in an application- to higher performance ceramic elements for long-term performance. specific form, as a spray-dried parts and increased value of the promote, design, manufacture and sell systems for the development and production of Offering enhanced electrical granulated powder (with or without end-product. heavy-duty material. and thermal insulation properties, binder), suspension or slurry. João www.innovnano-materials.com

Our performance The furnace specialist for  Consulting during the conception of a plant  Vacuum  Gas pressure sintering  Development and design of plants  Hot pressing  Debinding  Manufacturing of plants  Annealing  Tempering  Start-up and After-Sales Service  Sintering  Heat treating  Maintenance and modernisation of existing plants

Applications  Maximum temperature continuous furnaces  Sintering furnaces  Gas pressure sintering furnaces  Vacuum hot presses  Debinding and pyrolysis furnaces  Thermal post combustion  Special plants and manipulating eqiupments  Solvent debinding system

Your Preferred a significant number of MIM parts facturing conference will review recent supply industry, including producers Powder Injection Moulding at will feature as winning components. developments and applications for a of metal powders, lubricants, MIM the PM2014 World Congress, The special session devoted to number of sectors including medical feedstock, tooling, compacting regional reviews of the PM industries devices and implants, aerospace and presses, injection moulding machines, Choice for Orlando in North America, Europe and Asia defence. additive manufacturing equipment, (Wednesday morning, May 21) will Sessions will also cover metal sintering furnaces, furnace belts, The global PIM and PM focus on industry business conditions, powders suitable for AM, equipment powder handling and blending equip- Metal Injection communities will soon technology trends, and markets for PM technology, design and process ment, quality-control and automation come together for the 2014 and particulate materials, including modelling/simulation, and non-powder equipment, particle-size and powder- PM World Congress and Powder Injection Moulding AM technologies. characterization equipment and much, Exhibition, taking place at much more. The team from Powder Molded Parts the Walt Disney Dolphin Inaugural Additive Manufacturing PM2014 Exhibition: Diverse powder Injection Moulding International and Hotel, Orlando, Florida, Conference at PM2014 technologies on offer under one roof Powder Metallurgy Review will be from May 18-21. The various Of interest to the MIM community Bonding all of the diverse powder exhibiting on booth 222. programmes scheduled at from the perspective of producing technologies which will be highlighted A major attraction in the PM2014 the event promise to offer a prototypes will be the inaugural during the PM2014 Powder Metallurgy Exhibition will be the display of all the surfeit of development and conference on ‘Additive Manufacturing World Congress will be the PM2014 entries submitted to the Annual PM technology trends on all with Powder Metallurgy – AM/PM’ Exhibition. This is open from Monday Design Excellence Awards competi- aspects of PM. There are, (May 19-20) which will run alongside morning through to Wednesday tion. Winning parts will be identified however, numerous activities the PM2014 World Congress. afternoon. The PM2014 exhibition following the Awards Luncheon on at PM2014 that will be of Additive Manufacturing (AM) has will be a great opportunity to meet Tuesday, May 20. specific interest to those in made great strides in recent years worldwide MIM and PM colleagues in A buffet lunch will be held in the the PIM community. for the fast production of complex the exhibition hall conveniently located PM2014 exhibition area to promote It is not the first time that the PM World Congress and three dimensional solid objects by, next to the PM2014 Congress at the the location of the following PM World Exhibition has been held in Orlando. Such is the attraction of in most cases, adding successive Walt Disney World Dolphin Hotel. Congress & Exhibition which will be the destination, with its many world class theme parks and laser sintered layers of metal or alloy Some 115 exhibitors are taking over held in Hamburg, Germany, in 2016. recreation activities, it is little wonder that the Metal Powder powder material. The thirteen tech- 150 booths at this year’s World PM www.mpif.org Industry Federation (MPIF) and the American Powder nical sessions at the Additive Manu- Congress from every part of the PM Metallurgy Institute (APMI) decided to return to Orlando for the most important PM event of the year. Even for the most hardworking delegates and exhibitors there will opportunities to enjoy some of the excitement of Orlando at social ISO 9001:2008 Registered events such as the Opening Night Dinner (Sunday, May 19) ® during the International Street Festival and the spectacular EMBEMOULD Megamet Solid Metals, Inc. Epcot Illuminations. The PM2014 Gala Closing Dinner (Wednesday, May 21) promises to be the social highlight of 13748 Shoreline Ct. East the congress. There will also be a specific ‘Metal Injection Earth City, MO 63045 Moulding Industry Event’ (by invitation only) on Tuesday MIM feedstock | MIM & CIM binders evening, May 20.

MIM highlights at PM2014 At eMBe we have the products and services EMBEMOULD® C AND EMBEMOULD® K 83 There are no fewer than ten sessions devoted to MIM as part to help you “shape up” your metal or ceramic MIM and CIM binders for water and solvent debinding

of the large offering of PM technology presentations in the powders, from binders for solvent and catalytic EMBEMOULD® FEEDSTOCK PM2014 technical programme. These sessions will cover debinding to ready-to-mould feedstock. MIM feedstock for solvent or catalytic debinding binder materials, moulding, powder distribution effects in Develop your products with us by using our in- feedstock, magnetic materials, titanium, high temperature house laboratory and extensive experience as EMBELUBE® alloys, and advanced materials and processing. In addition, one of Europe’s leading PM additive suppliers. Poreformers for PIM products with porosity there are three sessions on microPIM and Ceramic Injection Moulding. Our services focus on product development and Running alongside the main PM2014 Technical product innovation to continuously meet our Programme will be a number of Special Interest customers’ evolving needs worldwide. Programmes which, whilst focusing on mainstream PM materials, will also be relevant to the PIM community. These eMBe Products & Service GmbH www.megamet.com include fatigue properties of PM steels, NDT/failure analysis Gemeindewald 7, 86672 Thierhaupten, Germany in PM, machinability of PM components, and technology for Tel.: +49 8271 421988-3 Fax: +49 8271 421988-4 [email protected] growth. [email protected]

There will be a special luncheon during PM2014 314.739.4499 (Tuesday, May 20) at which the MPIF Annual Awards for PM www.embe-products.com Design Excellence will be presented. It is anticipated that Embemould® and Embelube® are registered trademarks. Photo Arburg GmbH & Co KG

New approach to produce high performance MIM heat sinks from copper matrix nanocomposites

Metal Injection Moulding (MIM) is already a proven and well accepted manufacturing process for heat sink devices used in thermal management systems for modern microprocessors, with sintered MIM copper heat sinks often outperforming commercially pure cast copper alloys. However, with the continuing trend towards lower cost and smaller sized high performance electronic devices generating more heat, new thermal management solutions are needed to provide cost Fig. 2 MIM of Cu-MWNTs nanocomposites effective ways of dissipating heat. Responding to these challenges researchers in the PolyMIM GmbH is a manufacturer offering two Mechanical Engineering Department at the University of different binder systems for Metal Injection Molding: Technology Petronas (UTP), Tronoh, Malaysia, have developed a new generation heat sink material made from copper • polyPOM – our catalytic binder system powder reinforced with multiwall carbon nanotubes (MWNTs) • polyMIM – our water soluble binder system using MIM technology. These two binder systems have excellent Ali Samer Muhsan and colleagues have reported on the characteristics during the production process and outcome of their work to develop the new copper matrix/ combine attractive prices with worldwide availability. MWNTs in the open access International Journal of Manu- facturing Engineering (Vol. 2013, 2013, Article ID 386141, 9 Our portfolio covers high-end applications with pages). Key to ensuring a homogeneous dispersion of MWNTs our special alloys as well as the mass production in the copper powder matrix was using a new multilevel requirements seen in the automotive and mixing approach. telecommunications industry, for example. The authors stated that the MWNTs were first purified and Every possible challenge in the Metal Injection Fig. 3 Thermal conductivities of MWNTs/Cu composites functionalised using concentrated acids. Functionalisation Molding process can be overcome with our range of PHOENIX as a function of MWNTs volume fraction with two different was then applied to enhance the dispersion of purified MWNTs products tailored to our customers’ requirements. PH PHOENIX and to create sidewalls groups that have the potential to bind measuring temperatures (25 and 125°C) SCIENTIFIC MWNTs to the Cu matrix. MWNTs were subsequently washed Contact us to find a match for your application! acid) in a Z-blade mixer at 160°C. This step provided a high- with distilled water, dried and mixed with paraffin wax (PW) Phone: +49 6751 85769-0 SCIENTIFIC diluted in heptane solvent along with magnetic stirring. This viscous liquid medium with high shear forces that allowed INDUSTRIES the MWNTs clusters to be properly mixed resulting in uniform Fax: +49 6751 85769-5300 was followed by a sonic agitation process to ensure uniform Mail: [email protected] dispersion in the molten binder system. The copper powder Concept design to dispersion of MWNTs in PW solution. Web: www.polymim.com INDUSTRIES was added gradually during the mixing process to form engineering reality The dried MWNTs/PW mixture was then mixed with the other components of the binder system (polyethylene; stearic Cu-MWNTs-binder feedstock. (Fig. 1) Europe’s specialist engineers Following injection moulding the binder is removed from the Cu-MWNTs matrix by solvent and thermal debinding for design and manufacture of followed by sintering in argon at 950, 1000 and 1050°C. innovative materials processing Microstructural analysis showed that the dispersion of systems MWNTs was significantly improved using the new multilevel

 Atomisers mixing technique, and that there was little mechanical Hot/Cold Gas damage to MWNTs structure. There was good interfacial Water bonding at the Cu/MWNTs interfaces. It was also found that Vacuum Apex Business Park the high-shear forces from the binder system components Gas Recycling Hailsham BN27 3JU, UK during feedstock preparation helped to disperse and exfoliate  Powder Classifiers Tel: +44 (0)1323 449001 the MWNTs clusters into the Cu matrix homogeneously.  Trial Powder Service Fax: +44 (0)1323 449002 The thermal conductivities of Cu-MWNTs nanocomposites [email protected]  Melt Spinners as a function of MWNTs volume fraction with two different www.psiltd.co.uk  Wire Casters measuring temperatures (25 and 125°C) is shown in Fig. 3. T The highest value was recorded at Cu-1 vol.% MWNTs (366.516 W/mK) sintered at 1050°C for 120 minutes. This value corre- sponds to an increase of ~32 W/mK (11.25%) over that of the Fig. 1 Nanoscale dispersion process of MWNTs in Paraffin sintered copper (Cu matrix). Wax (PW) www.utp.edu.my

launched because of Open access book covers Feedstock specialist launches this. Here we see an ‘Some critical issues for new unit for the automatic opportunity to offer attractive, simply Powder Metal Sintering - Brazing - Metal Injection Molding - Hard Metal Reduction - Activated Carbon - Calcining - Annealing injection moulding’ solvent debinding of MIM and made products with low purchase and InTech Europe and InTech CIM parts running costs. We China have made available, PIM binder and feedstock specialist eMBe Products & invite interested as an open-access book, Service GmbH, based in Thierhaupten, Germany, has parties to come and a practical 270 page guide launched a new unit for the automatic solvent debinding test the system in Rotary drum Furnace Multitube-Pusher Furnace to injection moulding. The of MIM and CIM parts. The debinding unit, branded our facility.” Since 1933 ELINO INDUSTRIE-OFENBAU GMBH has been delivering custom-specific heat book, first published in Dee-Solver, is the result of a partnership with Germany’s Commenting on treatment equipment. Elino has delivered more than 4,000 furnaces worldwide, tailor-made hardback form in 2012, is high-tech systems providing renown German quality & reliability. Techtor GmbH. The companies state that this custom the trend towards edited by Dr Jian Wang and manufactured equipment is suitable for all PIM producers solvent debinding, contains individual chapters Elino’s wide product range consist of batch & continuous (gas fired or electrically heated) who are developing and producing parts using a solvent Bayer stated “Solvent furnaces completly “Made in Germany“ written by leading academics Exterior view of the new Dee-Solver debinding process. debinding, in who provide some clear solvent debinding unit from eMBe The Dee-Solver system will be offered in a number of particular ethanol- • with temperatures up to 2.600°C presentations of the injec- Products & Service GmbH • with atmospheres being toxic, aggressive, vacuum, high pressure, flammable, different sizes. The launch model, with a 50 litre capacity, debinding, is a tion moulding process and reducing and neutral works fully automatically with an SPS controller and up method where you do not need additional chemistry such as equipment. The book has the aim of directing people in • with product sizes from nanometers to tons to ten processes can be programmed and stored on a nitric acid, which is strictly regulated by export rules world- plastics and MIM/CIM manufacturing to solve problems touchscreen by the user. The unit contains a programmed wide, and expensive afterburners to deal with formaldehyde Elino’s very well equipped testing laboratory allows for material experimentation and process and avoid costly errors. solvent recovering system, a binder separator and a loaded gas. This solvent is readily available worldwide and validation of in middle-scale furnaces to define relevant application parameters. Together with The first two chapters provide an introduction to customers a huge number of new methods of production as well as new products were deve- vacuum dryer with condenser. A nitrogen flush prevents having it in a DeeSolver system as a debinding medium PVT properties of polymers for injection moulding, loped in the laboratory and successfully brought into the market. dangerous solvent-air mixing. is risk-free. The procedure is as simple as starting a and optimisation of the injection moulding process. Continues MIM pusher Furnace The system, which is designed and manufactured in dishwasher.” For more information contact Michael Bayer, (Made in Germany) The following five chapters are all devoted to Powder Germany, uses solvent-resistant long-life components and email [email protected]. • Elino manufactures continues MIM Injection Moulding. The PIM chapters include a compre- furnaces (approved technology) having meets the most stringent safety and environmental regula- www.embe-products.com low carbon level and complete debinding hensive introduction and review of PIM technology by in stainless steel without water injection system. tions. The same system can be used for water-debinding Joamín González-Gutiérrez and colleagues covering • Elino continues MIM furnaces also consume 3-4 as well. In this process a recovery of the binder is not times less process gas and cost effect worldwide. feedstock preparation, binder formulation, metal and • Best ever corrosion resistance in needed, as the removed biodegradable binder can be put in ceramic powders used including submicron powders, stainless steel parts is achieved by the waste-water. Continues MIM Pusher Furnace Elino pusher MIM furnace worldwide. injection moulding machines, debinding and sintering. Michael Bayer, Managing Director of eMBe Products & Other chapters involving PIM include: ‘Wick ECO-MIM one step debinding batch furnace Service GmbH, told PIM International “The advantage that (Made in Germany) Debinding - An Effective Way of Solving Problems in • One-step complete debinding unit we bring with this product is that it has been developed the Debinding Process of Powder Injection Molding’ by including pre-sintering up to 900°C and manufactured by people who have a deep knowledge • Convection system i.e. temperature Lovro Gorjan; ‘Micro Metal Powder Injection Molding’ homogeneity better than ±5 °C of PIM binder and feedstock compositions. Many small • Special off gas burner unit (environment friendly) by Kazuaki Nishiyabu; ‘Ceramic Injection Molding’ by companies who are interested in PIM are scared when • Changeable process gases Zdravko Stanimirovi and Ivanka Stanimirovi; ‘Optimiza- e.g. H , N , N -H , Ar, Air etc. 2 2 2 2 they receive quotations for capital equipment. PIM is a very tion and Simulation for Ceramic Injection Mould of ZrO2 ECO-MIM one step debinding + pre-sintering expensive technology and many products will never be Fibre Ferrule’ by Bin Lin, et al.

ECO sintering batch furnace (PM/CIM/MIM The remaining chapters review developments in (Made in Germany) microcellular foam injection moulding; insert moulding • up to 1450 °C with temperature accuracy of ±3 °C • Clean sintering i.e. energy/cost saving process employing vapour chamber; thermoplastic • Process gases N , H , Ar, N -H partial pressure 2 2 2 2 matrix reinforced with natural fibres – study of inter- or slight over pressure and vacuum • Vacuum up to 10-5 with Tubular pump facial behaviour; and finally the properties of injection moulded high density polyethylene nanocomposites filled with exfoliated graphene nanoplatelets. ECO-MIM sintering ‘Some Critical Issues for Injection Molding’ , Dr Jian Wang (Ed.), ISBN: 978-953-51-0297-7. www.intechopen.com/books

Submitting News

ELINO INDUSTRIE-OFENBAU GMBH Tel: -+49 (0)2421 - 69020 Fax: +49 (0)2421 - 62979 To submit news to Powder Injection Moulding International Zum Mühlengraben 16-18 [email protected] 52355 Düren - Germany www.elino.de contact Nick Williams: [email protected] Interior view of the new Dee-Solver solvent debinding unit from eMBe Products & Service GmbH

hard material which is deposited in New company created for Thin-film heating technology cuts layers only a few micrometers thick. the 3D printing of functional energy consumption during moulding This extremely thin coating is used to ceramic components heat the forming tool surface to the The Fraunhofer Institute for Fraunhofer researchers teamed up desired temperature. Mechanics of Materials IWM, with Kunststoff Zentrum (Leipzig, Electrical insulation is provided Dutch Ceramic Freiburg, Germany, has developed Germany), which provides consulting by a ceramic layer that shields the Injection Moulding thin-film heating technology which services to injection moulding conductive heating layer from the (CIM) specialist claims to reduce energy consumption professionals, to develop a process steel tool underneath. Fromm stated Formatec Ceramics, in injection moulding by as much that would reduce energy consump- that the challenge of sputtering based in Goirle, as 90% compared with conventional tion by 90% while improving moulded lies not only in producing a perfect the Netherlands, practices. This is achieved by heating part quality. “The thin film heater, in insulating layer so as to avoid any consulting company only the part of the tooling that comes combination with a thin film ther- short circuits, but also in integrating Innotech Europe and into contact with the plastic melt, or mocouple, is able to very accurately a sensor into the thin-film heating Energy Research in the case of PIM, the plasticised regulate the interfacial temperature, layer to measure the temperature Centre Netherlands A selection of printed ceramic feedstock. [thus, increasing] the reproduction of the tool wall and used to regulate (ECN) announced components including gears, Variothermic methods are typically quality of small structures on the the manufacturing process. To in December that filter elements and a watch case used to heat the entire tool during mould surface,” said Fraunhofer’s achieve this, the IWM researchers their research the injection moulding process. In the Alexander Fromm. “It can also lead to set about integrating incredibly fine collaborations have resulted in the foundation of a new case of plastic parts with high end a decrease in cycle time.” thermocouples, made from nickel company, ADMATEC Europe BV. Since spring 2013 the surfaces, the entire forming tool is The process developed involves or nickel-chrome alloy and each just parties worked together to develop a commercially viable heated to around 110°C. Cooling the only heating the thin film surface a few hundred nanometers thick, ceramic printing process for functional ceramic compo- tool sufficiently (to around 20-30°C) of the tool that actually comes into into the insulation layer. Due to their nents. Based on the rapid technical progress and the so that the moulded part can be contact with the plastic melt. The thin extremely low mass, thermocouples solid results, it was stated that founding a new company removed without damage adds time to film coating on the wall of the forming react incredibly fast to the tempera- was the obvious next step. the cycle. By minimising the amount tool is produced using a vacuum- ture changes and make it possible to ADMATEC Europe BV controls the complete printing of tooling surface that must be heated based coating technique known as directly measure the temperature of process in-house, a process named ADMAFLEX. The and cooled during each cycle, signifi- sputtering. The sputtered material the tool wall. ingredients used in the printing material were also cant energy savings can be realised. is a specially designed conductive www.iwm.fraunhofer.de developed in-house and allow for full control of the T & D Molybdenum & Tungsten process. Similarly, the development of the printing equip- Manufacturing LLC ment was undertaken within the group. During the past months the process has been qualified resulting in two validated materials, one for alumina and one for zirconia. The technology’s roots are based on a photosensitive Mo, W and Ta products resin that is homogeneously mixed with ceramic powder. ISO certified The material is then, layer-by-layer, activated through a light source. Following debinding and sintering the part reaches its final properties. • Mo, W, ML plates, sheets annealed for shielding, 24” width In the coming months ADMATEC will focus on realising a diverse range of commercial orders. A wide • Mo, W, Ta, Ta-W heating elements made according to customer drawings range of customers have discovered, through Formatec Ceramics, some unique uses for this new technology. • Spare parts including sheets, ribbon, rods, screw, hex nuts; boats, pins, wires and rivets. Customers are not only based in the high-tech Brainport • Custom made Mo, W, TZM, ML, Ta pieces region near Eindhoven, but also internationally. It was stated that innovations will continue and will most likely • Boats, trays, charge carriers, thermocouple protection tubes, all to customer drawings focus on increasing product sizes whilst retaining a high level of precision. The ADMAFLEX process will also be • W and Mo crucibles tested for printing metals. • Annealing and sintering boats for PM and Michiel de Bruijcker, Managing Director of ADMATEC, MIM told PIM International, “The technical developments have • W, Mo, TZM and Ta hot zones been very rapid over the past year. These results position • Mo, ML or TZM ADMATEC on a unique spot in the rapidly growing market for printing functional components. With a great T & D Molybdenum and Tungsten Manufacturing LLC amount of trust we are looking towards the future, 1101 Sussex Blvd, Suite 2 further enhancing the technology and further market Broomall, PA 19008. USA Tel: +1 484 472 6863 Fax: +1 484 472 6861 developments.” Email: [email protected] www.admatec.nl

was then placed into the mould for injection moulding the Metal plate with internal double sided metal plate from 17-4PH stainless steel feed- Thermoplastic micropart honeycomb structure made stock. The sacrificial insert is removed during debinding moulding market grows and sintering to leave the honeycomb structure between by Metal Injection the metal plates. Each cell, or channel, in the sacrificial According to a recent market report published by Moulding insert was interconnected so as to be removed without Transparency Market Research, the global polymer and air being trapped during debinding and sintering. These thermoplastic micro moulding market was valued at A new Metal Injection Moulding (MIM) process for interconnections would act as channels for fluid applica- $308.0 million in 2012 and is expected to grow to $763 producing double-sided metal plates having an internal tions. Because of the potential deformation of the internal million by 2019, representing CAGR of 14.2% over the honeycomb structure has been developed at the Korea polymer insert during injection of the MIM feedstock, period. Growing demand for micro moulded products Institute of Industrial Technology (KITECH) in Yeonsu-gu, the researchers undertook CAE analysis to predict the from various end use industries such as medical, auto- Incheon. Kwangho Shin and his colleagues reported complex flow behaviour of feedstocks for the production of motive and telecommunications is expected to drive the on their research on the new MIM process in the open a stable part. market over the forecast period. The rapid development of access journal Materials (2013, No. 6, 5878-5892) and The authors stated that the initial design of the micro fluidics and micro optics technologies, mainly in the stated that the rectangular metal plates with the internal finished part was based on a 30 mm square plate having US and Europe, is also expected to augment the market. complex structure are expected to be used under severe a thickness of 2.4 mm, including the polymer sacrificial In addition, the growing number of MIS (Minimally Inva- compressive load conditions with applications including insert of 0.8 mm designed as a honeycomb, with each sive Surgeries), which extensively use micro moulding, insulating panels, pressure vessel chassis and floor metal side also being 0.8 mm thick. It was established is expected to boost the market for thermoplastic micro panels. that for successful processing by Metal Injection Moulding moulding over the forecast period. In the process developed at KITECH one mould was the size of the square plate should be reduced to 22 mm. Medical and healthcare emerged as the leading used to produce the sacrificial polymeric insert which Four holes were added to the insert to prevent movement market for micro moulding and accounted for 35% of within the cavity during injection moulding of the 17-4 PH the total thermoplastic micro moulded products in 2012. feedstock, which had a powder loading of 59% in a wax This is expected to be the fastest growing market for based binder system containing 2% stearic acid (Fig. 1). micro moulded thermoplastics over the forecast period. Side gates were used to fill the metal feedstock for both MicroPIM could benefit from the growth and growing outer plates. The position of the gate was decided and awareness of micro moulding in the plastics sector. made between the shorter sides of the fixing points. The www.transparencymarketresearch.com insert was found to have suitable rigidity to endure the MIM process. Fig. 2 shows the green part and the sintered part, and Fig. 3 shows SEM images for the green part, brown part and sintered part. The shrinkage of the target part during debinding and sintering was about 16.3% in thickness and 15.5% in width direction. The final sintered thickness Fig. 1 Modification for the metal plate with an internal was approximately 2.0 mm. The researchers used an structure (honeycomb): (a) sacrificial polymer insert; and X-ray NDT technique to check the internal structure, and Technical Ceramics (b) sacrificial insert with metal plate it was found that the internal honeycomb structures were well-fabricated. From powder to finished product www.kitech.re.kr

CERAMIC INJECTION DRY MOULDING (CIM) PRESSING

MACHINING Fig. 3 SEM images for AND FINISHING the part at each phase. (a) 6 Chemin des plantes green part; (b) brown part; 70150 MARNAY and (c) sintered part FRANCE Tel: +33 (0)3.84.31.95.40 Fax: +33 (0)3.84.31.95.49 Email: [email protected] www.hardex.fr Fig. 2 Green parts and sintered parts: (a) green part; (b) sintered part; and (c) section view of sintered part

Powder Injection Moulding in the dental sector: From orthodontic components to implants

QUALITY METAL INJECTION MOLDED COMPONENTS The dental sector has for many decades been an important market for the PIM industry, driven initially by the production of small orthodontic brackets. These brackets, often weighing as little as 0.02 g, today account for around 16% of global MIM sales by value. As Prof Randall German, San Diego State University, USA, explains, significant opportunities remain not only in the orthodontics brackets business, but also in the development of metal and ceramic dental implants and dental hand tools.

The dental field always seems to Conceptual framework for Orthodontics, and Minnesota Mining be an add-on in industry reports on dental MIM applications and Manufacturing or 3M. Traction Metal Injection Moulding (MIM). It is arose because MIM offered a lower hardly included in a 2013 report from Dental orthodontic brackets, cost yet higher quality in contrast the Metal Injection Molding Associa- commonly known as braces, remain to investment casting. Nearly thirty tion (MIMA), an association of North an enduring application for MIM. Early years later, the actors have changed, America’s Metal Powder Industries demonstrations arose as MIM devices but MIM dental brackets remain in Federation (MPIF), and likewise is moved into the marketplace guided widespread production. poorly documented in the studies by Johnson & Johnson, American As shown in Fig. 1, orthodontic from other tracking organisations. Orthodontics, Rocky Mountain brackets are small devices (the NOW OFFERING Part of the issue is that most dental MIM is performed by captive operations that choose to remain invisible. Dentistry is a large field with global billing estimated at $120 billion per year; about half of that is in the USA based on approximately 195,000 dentists, some of which are focused on research or teaching. Japan has about half that number of dentists and Europe slightly less than twice that number. THE PREMIER One of the big winners for MIM is in orthodontia, in the form of orthodontic brackets for straightening teeth [1]. This article gives emphasis GLOBAL SOURCE FOR MIM to orthodontic brackets, but it also ponders what is next for MIM in dentistry to identify some growth Fig. 1 Top and bottom pictures of a typical MIM dental bracket, each weighs WWW.ARCMIM.COM opportunities. about 0.04 g ISO 9001 • ISO 13485 • AS9100 • ISO/TS 16949 32 Powder Injection Moulding International March 2014 © 2014 Inovar Communications Ltd Vol. 8 No. 1 Vol. 8 No. 1 © 2014 Inovar Communications Ltd March 2014 Powder Injection Moulding International 33 Opportunities for dental PIM | contents page | news | events | advertisers’ index | email | | contents page | news | events | advertisers’ index | email | Opportunities for dental PIM

pictured brackets have 0.04 g mass and with overhead the MIM industry the spread to other dental products Metric Value each) consisting of various combina- trade price reaches about twice this was slow. The current range of PIM US population 317 million tions of bumps, slots, grooves, holes, or $0.70 each. Of course, when sold products in dentistry includes the posts, logos, and textures, commonly to the patient the price is significantly orthodontic bracket, ultrasonic scaler US dentist population 195,000 with 100 or more geometric higher and some products are report- tip, endodontic abrasive tips, zirconia US orthodontist population 9,500 specifications. Stainless steel dental edly priced at $35 or more. implant posts, titanium implant posts, orthodontic brackets perfectly match and various hand tools [1-9]. These EcoPower US percent of global orthodontia sales 4 % the MIM design window; small mass The production of dental brackets items have been pictured frequently 55 – 300 t Annual growth rate for orthodontia billings 4% at 0.02 to 0.04 g, small sizes in the Dental bracket production was an and are the subject of several reports 2 to 5 mm range, over 75 features, early success for MIM and drove since they significantly challenged Average annual billing per US orthodontist $950,000 production quantity over 200,000 per much interest in the production of the PIM technology. Some examples Number of 12 year olds per year 4 million year, and in some cases reaching fine alloy powders versus mixtures include the following: millions per year. These brackets of iron-nickel-chromium based on all-electric • Ultrasonic cleaner tips fabricated Percentage of youth treated by orthodontist 42% therefore have a high production value carbonyl iron. Experiments using from 17-4 PH (AISI 630) stain- Percentage of orthodontic patients starting as roughly equal to $50,000 per kg, so mixed powders to form stainless 15% less steel. After sintering they adults the powder cost has lower impact steel by diffusional alloying were are coated with titanium nitride, Average number of new starts per orthodontist per on the manufacturing cost. There is successful, but corrosion resistance 220 mass about 1 g, pictured in Fig. 2 year ample room for further products in required long sintering hold times [3,4]. clean Typical treatment time 18 months dental MIM. that were not productive. Thus, early adoption of spherical stainless steel • Microminiature endodontic Typical cost of orthodontic treatment $4,320 A statistical view of US dentistry prealloyed powder was a clear choice abrasives fabricated in a similar manner, with hundreds and even Typical chair time per treatment 13 h We start by reviewing some statistical for this field. profiles on dentistry in the USA. The In visiting some of the early adop- thousands of 20 to 50 µm abra- Typical orthodontist time spent with patient 5 h USA population is approaching 320 ters during 1992, the typical situation sion teeth moulded on the tips as million. This is just 5% of the more was four to twelve moulders, four to pictured in Fig. 3 [5]. Typical orthodontist billing per hour $800 than 7 billion global population. But twelve cavities, and one or two batch • Zirconia tooth implant posts MIM orthodontic bracket market in the US $200 million the USA is disproportionate in dental sintering furnaces. Most of the dental formed using stabilised zirconia care expenditures. About 60 to 70% of firms purchased a license from the with diameters in the 1 to 2 mm Number of orthodontic brackets per year in the US 34 million the population receives regular dental original half dozen technology leaders, range and surface texture for Powder used in the US for orthodontic brackets per 1.5 tonne care provided by a pool of about but generally elected to purchase attachment to bone as pictured in year 195,000 dentists. feedstock since their needs were too Fig. 4 [6]. Table 1 Background statistics on orthodontics in the USA as relevant to the As evident in Table 1, orthodontics modest to justify a mixing facility. • Titanium implant tooth anchors MIM business is a significant MIM evaluation, at Unlike other parts of the MIM generated with two material energy-e cient least in economic value if not in terms industry, the dental firms did not injection moulding to form tissue of powder tonnage. Curiously, dental complain about the cost of powder. attachment core with strength orthodontic brackets account for They were converting gas atomised and elastic modulus matched to about 16% of the MIM global product stainless steel at $60/kg into $50,000 bone, as pictured in Fig. 5 [7,8]. sales based on far less than 0.1% of per kg product. Or as one industry • Distiliser, a longer span combi- the powder sales, and most of this is insider said at an early PIM confer- nation of pad, moveable ball, in the USA. ence in Boulder, Colorado, “… they curved rod, and hook fabricated all-electric. In the USA, about 20 firms are selling a bucket of product for a from zirconia, stainless steel, constitute the MIM production base million dollars.” or nitinol. The distiliser helps to for orthodontic brackets. Depending span large distances for proper energy-efficient. on materials, design, and geography The growth of other PIM dental jaw alignment. the brackets sell for $2 to $70 each, applications with an average price near $5 each. Dental orthodontic brackets were an The largest segments rely on clean. The lower price of $2 each is for large early adopter of MIM, but curiously 17-4 PH (AISI 630) and 316L stain- volume buyers, such as distributors once MIM penetrated that application less steels, with some minor role in international markets for older designs. Because brackets are Yield Strength Tensile Strength Fracture Elongation Alloy produced both in-house by captive MPa MPa % world of innovation facilities and by custom fabricators, www.wittmann-group.com 316L 170 515 50 often the MIM trade price is as low Fig. 2 A picture of the final dental Fig. 3 Endodontic abrasive tip with up as $0.70, so the $2 sale price is 17-4 PH 1050 1185 6 ultrasonic scaler tip after moulding, to 1500 bumps of 20 to 50 µm formed realistic for large volume distributor Headquarters: CP Ti 660 760 13 WITTMANN BATTENFELD GmbH sintering, heat treatment, and by MIM using sintered and heat purchasers [2]. In various reports, the Wiener Neustädter Straße 81|A-2542 Kottingbrunn titanium nitride coating for wear treated stainless steel with titanium direct manufacturing cost of a typical Ti-6Al-6Nb 420 500 20 Tel.: +43 (0) 2252 404-0|Fax.: +43 (0) 2252 404-1062 resistance (Courtesy CetaTech) nitride coating (Courtesy CetaTech) bracket is estimated at $0.35 each, [email protected] Table 2 Typical mechanical properties for MIM dental alloys

where restorations are created. The 10 mm diameter by 16 mm long turbine wheels (about 1.5 mm wall thickness) are driven by air turbines and reach high speeds with low mass, so would require aluminium. Similar to the automotive turbocharger, the geometry is ideal for MIM. Further the ability to hollow out the geometry is a competitive advantage for MIM since it will lower mass to make the turbine more responsive and minimise the Fig. 4 Dental implant from zirconia focused on the Fig. 5 Titanium dental implant with a porous central region potential for soft tissue damage. The moulded bumps to ensure affixation to bone (Courtesy for tissue ingrowth (Courtesy National Research Council of opportunity is in the million units per CetaTech) Canada) year range, ideal for MIM. In other opportunities for MIM, note the distalizer consisting of Fig. 8 Part of a sleep apnea device made by MIM from Ti Grade 4 feedstock ball, rod, pad, and hook has entered (Courtesy OBE GmbH & Co KG) production and is a high value addi- “Critical Issues in Manufacturing M. Uo, H. Matsuno, T. Kawasaki, tion to the MIM portfolio. Additionally, Dental Brackets by Powder Injection “Imaging of Gradient Structure of small MIM components are part of Molding,” International Journal of Titanium/Apatite Functionally Graded new sleep apnea positioner’s designs. Powder Metallurgy, 2012, vol. 48, no. Dental Implant,” Journal of the Japan An example of a titanium MIM 2, pp. 23-29. Institute of Metals, 1998, vol. 62, pp. component in a sleep apnea device is 1095-1101. shown in Fig. 8. [2] B. Williams, “Powder Injection Moulding in the Medical and Dental [8] Y. Thomas, E. Baril, F. Ilinca, J. Sectors,” Powder Injection Moulding F. Hetu, “Development of Titanium Conclusions International, 2007, vol. 1, pp. 12-19. Dental Implant by MIM: Experiments MIM for dental applications was one of [3] C. J. Hwang, Y. B. Ko, H. P. Park, and Simulation,” Advances in Powder Fig. 6 This picture contrasts the translucent dental Fig. 7 Small MIM gears used in an electric toothbrush the first major successes, but generally S. T. Chung, B. O. Rhee, “Computer Metallurgy and Particulate Materials bracket sintered from alumina with the traditional (Courtesy FloMet) has remained hidden. Several signifi- Aided Engineering Design of Powder - 2009, Metal Powder Industries stainless steel sintered brackets, showing the distinct cant opportunities are under discus- Injection Molding Process for a Dental Federation, Princeton, NJ, 2009, pp. aesthetic difference sion, but still stainless steel orthodontic Scaler Tip Mold Design,” Materials 4.81-4.93. from Co-Cr-Mo or other nickel free their own bracket designs. The only In the USA there are about 500,000 brackets remain a mainstay in the USA. Science Forum, 2007, vol. 534, pp. [9] T. Deguchi, M. Ito, A. Obasta, Y. compositions, and small levels of significant challenge remaining new implants installed per year. Since The estimated $200 million in MIM 341-344. Koh, T. Yamagishi, Y. Oshida, “Trial titanium and titanium alloys, including seems to be the fabrication of trans- the implant is not mating with other dental brackets annual sales in the USA [4] S. Ahn, C. J. Hwang, Y. S. Kwon, S. Production of Titanium Orthodontic NiTi (Nitinol). For these applications lucent or transparent brackets, such components, the tolerances are gener- is equal in value (but not tonnage) to the J. Park, R. M. German, “Development Brackets Fabricated by Metal injec- the typical MIM mechanical properties as those shown in Fig. 6. Most of the ally at ± 0.5%, but the size is from 8 to often discussed applications in firearm, of Ultrasonic Dental Tips by Powder tion Molding (MIM) with Sinterings,” are cited in Table 2 [1,2,10]. trials are with alumina or magnesia- 15 mm length and 1 to 5 mm diameter. medical, industrial, and other fields Injection Molding,” International Journal of Dental Research, 1996, vol. alumina spinel sintered in hydrogen combined. Journal of Powder Metallurgy, 2012, 75, pp. 1491-1496. Emerging opportunities in to near optical transparency to form Dental hand tools vol. 48, no. 2, pp. 11-20. [10] R. M. German, “Medical and invisible brackets with good strength Hand tools and even consumer dental MIM Author [5] Y. S. Kwon, S. T. Chung, I. H. Lee, Dental Applications for Micromini- and compatibility [11]. devices are a continuing opportunity S. H. Baek, “Tips for Dental Applica- ature Powder Injection Moulding - A Professor Randall M. German Orthodontic brackets for MIM. Early electric toothbrushes tion by Micro PIM,” Proceedings of a Roadmap for Growth,” Powder Injec- Fellow APMI, ASM, and ACerS Dental orthodontic brackets were Dental implants used small MIM gears to generate Workshop on Medical Applications tion Moulding International, 2009, vol. College of Engineering an early success for MIM, but the Dental implants continue to be the the rotating motion and reportedly for Microminiature Powder Injection 3, no. 2, pp. 21-29. San Diego State University custom industry was small forcing subject of much research, largely at peak production reached 85,000 Molding, R. M. German (ed.), Metal [11] F. Sernetz, “Herstellung San Diego, many of the user firms to integrate because the current machined posts gears per day. Fig. 7 is a picture of Powder Industries Federation, 2009, Orthodontischer Teile aus Metall California, production into their operations. In are priced in the $350 to $450 range. this early product. As dental health on CD. und Keramik mittels MIM und HIP,” the most recent survey of the MIM USA Two target materials are widely education progresses, there are some [6] I. H. Lee, H. C. Kim, S. T. Chung, Powder Metallurgy International, industry, a total of 39 firms claimed to Email [email protected] discussed – titanium and zirconia. opportunities in other consumer hand Y. S. Kwon, S. H. Baek, “Zirconia 1990, vol. 22, no. 3, pp. 69-74. be in production for dental products. The titanium might be treated with tools, for example flossing devices. Post for Dental Application by Micro Of this, over half were captive firms. hydroxyapatite and have a porous Although most of the device will be References PIM,” Proceedings of a Workshop on Besides the USA, they were located in section with 200 µm pores for bone plastic, the critical stress bearing [1] R. K. Enneti, S. J. Park, A. Medical Applications for Micromini- Canada, China, Germany, India, Italy, ingrowth formed using space holder floss support tips will be from metal. Schenck, R. M. German, P. Thomas, ature Powder Injection Molding, R. M. Mexico, and New Zealand. In at least ideas. On the other hand, the zirconia Dental drills are another potential B. Levenfeld, A. Varez, I. O. P. De German (ed.), Metal Powder Indus- one case, the MIM facilities were set is affixed to the bone using threads, for MIM. They are used in the dental Souza, J P. De Souza, A. M. Fuente- tries Federation, 2009, on CD. up by dentists seeking to fabricate posts, bumps, or tapers. office and in the dental laboratory fria, V. P. Onbattuvelli, S. V. Atre, [7] F. Watari, A. Yokoyama, F. Saso,

Vice President of Sales and Marketing with 30 years related marketing and Ortho Organizers: management experience. Mark Payne is Director of Engineering with 21 years of experience in orthodontics. A global leader in the He is responsible for new products and new production processes. Celine Cendras is Director of development and manufacture Marketing with a focus on launching new products and managing the distribution channels for Ortho of MIM orthodontic products Organizers and the recently acquired ClassOne and Masel brands. She has 18 years related experience. Robin Ortho Organizers, Inc., based in Carlsbad, California, USA, provides a Marks is Director of International wide range of orthodontic products to the worldwide dental market. A Sales that now account for over 50% of Ortho Organizers sales via 200 Fig. 2 Students from the SDSU PIM Design course outside the Ortho Organizers part of the orthodontic portfolio of Henry Schein, Inc., Ortho Organizers’ international distributors. facility in Carlsbad, California in-house MIM operation has since 1996 enabled the company to remain As with all firms working in at the forefront of the manufacture of innovative and complex orthodontic the dental-medical field, Ortho products. Prof Randall German, San Diego State University, recently Organizers has a keen focus on regulatory affairs and Foster Boop toured its MIM facility with a group of PIM Design students and reports serves as Director of Regulatory on the development and use of MIM at the company. Affairs and Quality Assurance with more than 20 years’ experience. Sue Fix is Director of Operations and has nine years prior experience in dental device manufacturing and supply chain management, with another ten years managing procurement and purchasing. Chief Financial Officer for As part of the PIM Design course of some students outside the facility cases for orthodontists. They acquired the Dental Specialties Group is Alison taught as a senior mechanical (Fig. 2). Micro Metal Products in 1981 and Weber. engineering elective at San Diego Ortho Organizers was founded San Marcos Medical Plastics in 2001. Chhattar Kucheria is Senior State University, a group of 16 in 1976 by Lindsay Brehm, a The company subsequently grew and Research Scientist and Edward students visited Ortho Organizers former employee of “A Company” changed hands, and in 2006 moved to Fig. 3 The Maestro Low-Profile Bracket System from Ortho Organizers features Soblewski is Production Manager, in Carlsbad, California in December (Johnson and Johnson). Lindsay its current 65,000 square foot facility rounded contours for patient comfort and highly complex structures that and these two individuals kindly 2013. The location is on a hilltop near is the son of Waldemar Brehm, a in Carlsbad (north San Diego County). machined brackets cannot duplicate (Courtesy Ortho Organizers) guided the visit by the San Diego the Pacific Ocean (Fig. 1), with palm famous orthodontist and teacher In 2008 it was purchased by Henry State University PIM Design class. trees making up a lovely industrial of orthodontics. The first products Schein, Inc., a Fortune 500 Company. Not included in the visit is a separate setting, as evident in the photograph were organisation racks and storage Ortho Organizers (commonly known facility that forms elastomeric as O2) became part of the Dental products, archwires, and waxes. The Specialties Group where it operates company also has other products under ISO 13485 and FDA CFR 820 such as gold caps, ceramic brackets, standards. and sapphire brackets. One impressive aspect of the Ortho Organizers today company is the commitment to In the past few years Ortho Organizers education. They host up to 250 has grown rapidly, both by the short courses per year, taught by absorption of other companies and by industry leaders as a service to the the leverage from the Henry Schein profession. In addition, in-house sales force. The current management training is important in developing the team has deep experience in the workforce. Recent courses have given dental-medical arena, starting emphasis on sleep apnea treatment with the President Russ Bonafede using orthodontics. (since 2009) who has 24 years in Ortho Organizers is well regarded Fig. 4 Further details of the design and function of the Maestro Low-Profile Fig. 1 The Ortho Organizers headquarters in Carlsbad, California (Courtesy orthodontics, implant dentistry, and in the industry and has been noted Bracket System from Ortho Organizers including features that enable the Ortho Organizers) related surgical fields. Ted Dreifuss is frequently for leadership via awards. positioning of brackets in their ideal location (Courtesy Ortho Organizers)

what Ortho Organizers calls digital and tool surface finish. Tooling is dentistry. Additive Manufacturing for single cavity for the larger distalizer orthodontics exists now in plastics, parts, but reaches two, four or even so projecting adoption of the process eight cavities for the orthodontic for metals is realistic. For now, Ortho brackets. One consequence is that Organizers sees no disadvantages to moulding is automated with robots, a captive MIM operation, especially in requiring only a couple employees for light off the fast response possible. the nearly dozen moulding machines. The only mentioned negative Fig. 5 shows a picture of the moulding aspect of MIM is the cost of moulds. area consisting of Boy moulders with Considering that each tool requires a robots. Tools are repaired in house. few weeks tool room effort, and there Mould filling simulations are are a thousand designs, a comment provided in some cases by outside was made that replacing the tooling vendors, but this is not a typical would now require considerable effort. activity for Ortho Organizers. On From a technological view, the occasion there is some difficulty Fig. 5. Moulding area in the Ortho Organizers MIM facility in Carlsbad, company has 17 issued patents with balancing mould filling, but Fig. 8 The Carriere Distalizer™ appliance manufactured by Ortho Organizers. California (Courtesy Ortho Organizers) and licenses another six patents otherwise most of the tool design This larger MIM orthodontic product, consisting of ball, rod, pad, and hook, has while operating with well over 50 builds on years of experience. entered production and is a high value addition to the MIM portfolio. Lengths Most recently in October 2013 they constitute the primary production, trademarks, including Nickel-Lite® Tools maintenance varies with the range from 16 to 27 mm (Courtesy Ortho Organizers) were featured with the cover article 17-4 PH (AISI 630) stainless steel and for the cobalt-chromium MIM geometry, but tool life reportedly 200 to 300 people. About 5% of The company reports about 20 in Orthotown, and in the past two a trademarked Nickel-Lite® cobalt- brackets. New designs arise from reaches to about 300,000 shots prior the employees are technical, competitors. Ortho Organizers is years their brochures and packaging chromium alloy. internal efforts or via inventors, to return to the tool room. mostly young engineers involved in positioned in the top third of the designs have been given notice by A typical MIM bracket geometry is usually well regarded orthodontists. automation, process development, industry based on sales and is industry trade groups. shown in Figs. 3-4. Surprisingly, there A few years ago they purchased Debinding and sintering and tooling developments. growing rapidly. Their growth is a are more than 1500 distinct SKU another MIM company, ClassOne The moulded components are staged The sale of orthodontic brackets combination of the leverage from (Stock Keeping Unit) numbers in the Orthodontics, and now produce The application of MIM at on trays and spaced to avoid contact. produced by MIM is a competitive Henry Schein, acquisitions, and MIM inventory. Consequently, Ortho and sell the Carriere self-ligating Ortho Organizers Debinding is rather rapid since the business. In the USA there are 9,500 organic growth; reportedly giving Organizers love the flexibility that brackets and distalizers as part of components are small. The first step is orthodontists and the specialisation a 200% increase in the past three Ortho Organizers initiated MIM comes with a captive MIM facility. In their premier product line. a solvent debind followed by backbone is distinguished by further years years. In the USA they promote via a production with a license from a captive facility the production runs removal during heating to the sintering of training after dental school. combination of 20 traveling field sales Injectamax (formerly located in are shorter, and products shifts are temperature. Three furnaces are In addition, about 7,000 general agents that directly call on dentists, nearby Escondido, California, now frequent, so inventory is replenished MIM tooling expertise available in the furnace room, but practitioner dentists do some ten inside sales agents, ten customer part of the ARC Wireless Group). with short lead times. In terms of production, the company most production is performed in an orthodontia cases. Thus, Ortho service representatives, and ten Essentially they still practice that With this trend, of course, a natural forms its own tooling, with EDM Elnik batch furnace in hydrogen. The Organizers is looking at over 16,000 selling teams acting for the Dental technology, but with many adaptions, forward projection is an eventual electrodes used to form inserts heating cycle has a sequence of holds potential customers in the USA. Specialties Group of parent Henry such as relying on premixed shift to Additive Manufacturing to in-house. Considerable engineering to ensure proper breakdown of the Curiously, orthodontic treatments are Schein. They also export to more than feedstock and adjusting the solvent fabricate one bracket at a time, just expertise exists in terms of gate size, backbone polymer prior to soaking at generally outside dental insurance 90 countries and as mentioned export debinding technology. Two alloys in time, but that is off in the future in wall size, draft angles, runner design, the peak temperature. One furnace coverage, so the company has low accounts for over 50% of sales. run per day is typical. sensitivity to changes occurring in the An additional bell jar hydrogen insurance industry - orthodontia is an Author furnace can be employed for sintering, elective treatment. but most of its use is for brazing. A Statistics shared during the visit Professor Randall M. German third vacuum furnace is employed also are that a typical orthodontist in Fellow APMI, ASM, and ACerS for brazing. Some of the components the USA has 200 to 300 new cases College of Engineering are laser welded instead of brazed. per year, of which about 15% are San Diego State University After sintering the components move adults. The roughly 7,000 general San Diego, California, USA to finishing and inspection, involving practitioners that practice limited Email: [email protected] bench labour and working through orthodontia average about 20 new magnification glasses. starts per year. Each new case is a Contact sales opportunity for MIM. Although Ortho Organizers plastic appliances are an alternative Production volumes and Corporate Headquarters to the MIM brackets, generally the 1822 Aston Avenue markets plastics with lower elastic modulus Carlsbad, CA 92008-7306 Fig. 6 An Andrews2™ bracket manufactured by Fig. 7 An illustration showing the siting of a MIM orthodontic Production ranges from 1.4 to fail to produce the desired permanent United States Ortho Organizers. The inner surface features an bracket, in this instance a lateral perspective of an Andrews2™ 2 million brackets per month. repositioning of the teeth in the www.orthoorganizers.com 80-Gauge micro-etched bondable mesh pad for bracket manufactured by Ortho Organizers (Courtesy Ortho Likewise in recent years the typical 24 month treatment time used improved adhesion (Courtesy Ortho Organizers) Organizers) employment has ranged from in orthodontics.

An introduction to the Hot Isostatic Pressing (HIP) of MIM components

Whilst Metal Injection Moulding can achieve sintered part densities that are significantly higher than conventional Powder Metallurgy products, there are a number of advantages to achieving full density in a MIM part. As Dr Stephen J Mashl explains, using HIP to achieve full density MIM products can improve mechanical properties, assure a higher quality of surface finish for polished and electroplated applications and offer greater peace of mind for medical device manufacturers. There are, however, a number of considerations to bear in mind when planning the HIPing of MIM parts.

During the 1970s and 1980s, when Reasons to HIP MIM illustrating the effect of residual the Metal Injection Moulding (MIM) products porosity upon tensile strength, process was seeing tremendous ductility measured as percent growth, some parts makers would Hot Isostatic Pressing, or HIP, is elongation, and impact resistance. state that MIM components could a common post-sintering process In these plots residual porosity is sinter to full density, thus implying by which residual porosity in MIM quantified as relative density where: that the finished MIM product parts can be eliminated. This article Relative Density = 1-Pore Fraction was pore-free. Given the very high examines the HIP of MIM materials, as-sintered density levels of typical presents the reasons for considering Thus with 2 volume percent residual MIM materials and the significantly the addition of HIP to a process porosity or a pore fraction of 0.02, lower density values of conventional scheme and reviews the potential the relative density would be 0.98. pressed and sintered ferrous PM problems and benefits that might be A pore-free material has a relative parts, this optimistic view can be encountered in the combined process. density of 1.0. understood. In the three graphs that In truth however, most MIM To improve mechanical properties comprise Fig. 1, the slope of the line components have between 1 and 3% To an engineer, the improvement representing the property data as residual porosity after sintering. In of mechanical properties is always it approaches the pore-free state, most applications, this small amount desirable. The effect of residual where the relative density equals 1.0, of residual porosity is acceptable porosity on the mechanical properties indicates the relative sensitivity of that and a MIM part performs very well of PM materials is well understood property to small amounts of residual in the as-sintered condition. In other with studies dating back more than porosity. The steeper the slope of instances, this small amount of 60 years. One landmark study by the line as it approaches a relative residual porosity is a problem and its Alexander Squire in 1947 examined density of 1.0, the greater the effect presence limits specific properties the effect of varying amounts of of porosity on the property examined. or performance to a level less than residual porosity in iron PM materials In Fig. 1, Squire’s graphs have been optimal. [1]. Fig. 1 shows Squire’s data modified to illustrate the impact of

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t Table 2 Charpy V-notch impact test results for MIM 17-4PH e e c l c i a r s 3 p stainless steel produced from blended powder*. After e n Density (g/cm ) 7.81 8.20 P m e I T LaGoy, Bulger [3] Density 95 100 (% Pore-Free) *The powder employed in making the samples represented here was a blend of carbonyl iron + master alloy (75% Hardness (HRC) 16 15 by volume) combined with water atomised, pre-alloyed Relative density Relative density Relative density powder (25% by volume). HIP was performed with a 4 hour Table I Tensile properties of MIM Co-28 w/o Cr-6 w/o Mo. hold at 103 MPa , at the temperature indicated. After Sago, et al. [2] Fig. 1 Three graphs showing the effect of residual porosity, reported as relative density, on mechanical properties. A relative density of 1.0 represents the pore-free state and is indicated by the vertical broken line. The gray, shaded region immediately to the left represents the range from 98% dense to the fully dense state. The difference in properties at in ultimate tensile or yield strength but a 33% increase in manufacture of jewellery and highly decorative items such these two density levels varies from small (4% change in ultimate tensile strength), to moderate (a 10% change in tensile ductility. as the eyeglass frame shown in Fig. 4. When a surface ductility), to large (a 40% variation in fracture toughness). The data is from Alexander Squire’s 1947 paper “Density Impact toughness data presented by LaGoy and Bulger is polished to a mirror-like finish for appearance, fine Relationships in Iron-Powder Compacts” [1]. [3] is shown in Table 2. Again matching the behaviour porosity exposed during the polishing becomes readily predicted by Squire, the gains in impact toughness are visible to the naked eye. The presence of even a small noise of repeated measurements and large. In this segment of their work, where two HIP amount of porosity can send a near-finished part to the (a) (b) thus the effect is seen as negligible temperatures and two sintering temperatures were used, scrap bin. or non-existent. The improvement it is interesting to note that the highest impact toughness in ductility can be more significant value is reported for the lowest sinter temperature and and, when a parts maker faces a lowest HIP temperature. While no error data was provided challenging ductility specification, to allow evaluation of the significance of the reported the use of HIP may bump tensile differences, it is possible that grain growth, occurring ductility to a level sufficient to during sinter, HIP or both processes resulted in the lower ensure customer satisfaction. The sinter and HIP temperatures being most effective. truly significant improvements in It should be noted that residual pores are only one Fig. 2 Optical micrographs showing, (a), the microstructure of a cobalt-chrome mechanical properties with HIP of several types of microstructural defects that are medical implant alloy (F2886) sintered and solution annealed to a density of are seen in the areas of impact encountered in MIM products. Inclusions, in the form of 7.80 g/cm3 (95% of pore-free density) and (b), The same material after sinter, resistance/fracture toughness and oxides, sulfides, silicates, etc., have a detrimental effect HIP, and solution anneal to a density of 8.25 g/cm3. The complete elimination high cycle fatigue. Elimination of the on mechanical properties similar to porosity. A high of residual porosity in the sintered and solution annealed alloy following HIP last few percent of porosity in a MIM population of these non-pore defects can limit or eliminate is apparent. Comparison of the scale markers indicates a nominal five-fold component can lead to dramatic any improvement that might be achieved with HIP. It increase in grain size with HIP. After Sago, et al. [2] improvements in these areas. is also important to realise that changes taking place The images shown in Fig. 2 and during sinter, HIP, or heat treat can offset each other. For 2% porosity on strength, ductility and where the line contacts the broken the data in Tables I and II illustrate example, it is possible to HIP a component and remove all impact resistance and also show the line representing a relative density porosity, potentially enhancing ductility, only to have grain ipmd.net the behaviour predicted by the Squire relative improvement that one might of 1.0, the relative effect of HIP can data. Fig. 2a shows the unetched growth and its detrimental effect on ductility counter the expect were that porosity removed be evaluated on these three specific microstructure of a MIM cobalt- positive effect of pore removal. Your on-line source for PM industry with HIP. A gray band covers the mechanical properties. For ultimate chrome medical implant product. ipmd.net density regime from 0.98 to 1.0, i.e. a tensile strength, the improvement The as-sintered material contains a For appearance sake: highly polished surfaces news, technology and more.... 2% porosity range. It is very common with HIP can be estimated at 4%. A fairly high 5 volume percent porosity. Improvement in mechanical properties is not the only Your on-line source for PM industry for MIM ferrous alloys to contain 10% increase in ductility is predicted HIPing this material yields the result reason to consider the use of HIP to remove residual 2% porosity and this comparison and a large, 40% improvement in shown in Fig. 5b, a pore-free material, porosity from MIM parts. Highly polished surfaces may be news, technology and more....Sign up for our FREE weekly PM e-newsletter illustrates the typical change in impact resistance is indicated. High albeit one in which the HIP process required for functional reasons such as in the polishing of Sign up for our FREE weekly PM e-newslettertoday at www.ipmd.net/enews density that can be achieved when cycle fatigue life is another property appears to have induced a 5 fold the mould dies employed in plastic forming. As illustrated today at www.ipmd.net/enews as-sintered MIM parts are HIPed to that, like impact toughness, is very increase in grain size. in Fig. 3, in these applications sub-surface porosity full density (relative density = 1.0). By sensitive to small amounts of residual The tensile properties that that becomes exposed during the polishing operation is examining the point at which the line porosity. accompany the images in Fig. 2 are considered a defect [4-6]. representing Squire’s data contacts In practice, when a MIM part is presented in Table I. Comparing Polishing need not be done for functional reasons, a Scan the QR code to Scan the QR code to visit www.ipmd.net the left-most edge of the gray band HIPed, the improvement in tensile and as-sintered to HIPed tensile high gloss finish may be desired for aesthetic reasons visit www.ipmd.net and comparing that to the point yield strength often falls within the properties one observes no change alone. Metal Injection Moulding is increasingly used in the

IPMD website for EuroPM2012.indd 1 8/8/2012 10:23:26 AM

Fig. 3 Pores, such as those shown on the right, that Fig. 4 When MIM surfaces are highly polished for aesthetic Fig. 7 An image of partially consolidated Fig. 8 A schematic of pore isolation resulting from grain growth. Image become exposed during a polishing operation meant to reasons, such as the decorative eyeglass frame shown spherical powder. During the consolidation (a) shows the initial state with grains to the left and right of the pore and deliver a mirror-like high gloss surface are considered here, exposure of subsurface porosity during polishing can process the mated particle-particle surfaces the grain boundary extending vertically away from the pore. Conditions defects. The use of HIP to eliminate near-surface send a near-finished part to the scrap bin. After Williams become grain boundaries, regions of atomic are such that the grain to the left is moving to the right. Images (b) and porosity prior to polishing operations has been shown to [7] (Photo courtesy OBE GmbH & Co. KG) misalignment that serve as a high-speed (c) show the grain boundary moving rightward but being pinned in place dramatically improve yields (courtesy Fraunhofer IPT ) [4] route for atoms and vacancies to move, thus by the now deformed pore. In (d), the grain boundary has separated facilitating further densification from the pore and it will continue to move to the right, now unhindered parts such as the a high-compression (a) (b) by the pore. Densification of the pore will now slow considerably [10] jaw used in laparoscopic surgery shown in Fig. 6. In medical applications, fine during HIP rely on diffusion, drives sintering and allows MIM it is possible to reach the point where sub-surface porosity exposed during specifically the transport of atoms to components to achieve the very high pores within the sintered material machining and finishing operations is the pore surface and the movement of as-sintered densities characteristic have just become isolated but have regarded as a harbour for bacteria [9]. atomic vacancies to the part surface. of the process, in this case it works not separated from grain boundaries. In today’s litigious society, elimination During the initial stages of HIP when against the parts maker. Likewise in HIP, keeping temperature of the risk of infection in the operating powder particles are deformed room can be a driving force large plastically, the mated surfaces of collapsed particle surfaces fuse and ‘the move to incorporate HIP Fig. 5 Two micrographs showing near-surface porosity in a die casting (a) that, enough to justify the additional cost become grain boundaries, connecting following polishing and plating (b) results in a highly visible imperfection in the of HIP, even when the elimination must be taken with consideration the pores to each other and to the plated surface. While these images are from sectioned die castings, identical of porosity is not required to meet part surface. This concept can be behaviour can occur in MIM components. After Annetts [8] mechanical property specifications. for all of the factors that affect visualised in Fig. 7. densification during HIP and the Grain growth in MIM alloys – Along these newly formed grain Electroplating and electropolishing boundaries, where the atomic lattice an obstacle to densification resultant mechanical properties’ might be undertaken for either of one grain is mismatched with functional or aesthetic reasons, If HIP is to be incorporated into the lattice of an adjacent grain, the depending upon the application. a processing scheme, it may be relative openness of the atomic Fig. 8 shows, schematically, at the low end of the feasible range, Regardless, this is another situation necessary to review upstream structure serves as a superhighway the process of a grain becoming maximising pressure, and minimising where near-surface porosity, such procedures if optimum mechanical for atom-vacancy movement, isolated by a pore while the dwell time at temperature will as that shown in Fig. 5a becomes property improvement is to be enhancing the rate at which a microstructure of the MIM 420 decrease the driving force for grain exposed during surface preparation achieved. The relationship between material will densify under HIP stainless steel component shown in growth and thus facilitate maximum and results in a defect such as that pore fraction and mechanical conditions. Fig. 9 is “over-sintered” if HIP is to densification. shown on the cross section of a plated properties is well known and it is MIM products are made using be considered. The material shown in die casting in Fig. 5b. Again, highly this relationship that drives the metal powders that are much finer Fig. 9 has experienced grain growth polished highly reflective surfaces manufacturers of MIM components to than those used in other HIP PM to the point where many pores are Summary tend to make small surface defects pursue increasingly higher sintering operations. Grain growth is driven by now isolated within grains. With There are many reasons why a more visible. temperatures in order to decrease nature’s desire to decrease a systems such a structure, it is unlikely that a company might consider using HIP Fig. 6 MIM produced medical pore fractions in the as-sintered total energy by decreasing the amount conventional stainless steel HIP cycle to eliminate porosity from a MIM components are often HIPed to To prevent infection: medical part. While this approach may help in of high energy surface, in this case, will fully eliminate the pores from this product. Improvement in mechanical eliminate sub-surface porosity that applications achieving higher density levels, it can grain boundary surface. Because MIM material. properties, especially impact would become exposed in final The medical industry is a sizable be counterproductive if HIP will be materials are made from powders The parts maker can take steps to toughness and fatigue are one; visual machining operations. This now market for the MIM industry and the used to attain pore-free density. Grain that are much finer than other PM avoid grain growth and promote full appeal and medical safety are others. surface connected porosity is seen as HIP of MIM components to be used growth and its effect on diffusional products, MIM materials have a densification during HIP. By using the Regardless of the reasons for adding a harbour for bacteria and a potential in surgical applications appears to be densification are the issue. higher driving force for grain growth. sinter temperature that is on the low HIP to a MIM production operation, source of infection (image MPIF) growing with increasing production of The latter stages of densification While this same driving force is what end of the spectrum for a given alloy the move to incorporate HIP must be

The HIP process Prior to HIP, the sintered MIM components are assumed to have been sintered to a point where The Hot Isostatic Pressing (HIP) process can be all porosity is isolated from the surface. It is also described as a high temperature pressure treatment. assumed that nothing resides within the isolated

When processing MIM materials the goal is to remove

pores that might hinder densification, e.g., large porosity from the metal product. To accomplish this, © molecular weight, low diffusivity gasses such as the parts are heated to a point where the flow stress argon. These assumptions are not always true. of the alloy is significantly decreased and diffusion Not all porosity can be removed via hot isostatic becomes active. The applied, hydrostatic pressure pressing. As shown in Fig. 2, pores or pore-networks then drives densification, initially via the plastic flow that connect to the surface of the part will not be of the metal and in the later stage of the process by eliminated with HIP. In this situation the high pressure diffusional creep mechanisms. Industrial HIP units can typically achieve temperatures up to 1300°C and Fig. 9 The microstructure of a MIM 420 stainless steel pressures of 210 MPa, while specialised units have component in the as-sintered condition. While pores reached 2200°C and 700 MPa. Typically an inert gas are still seen to decorate the current grain boundaries, is used as a pressure transfer medium with argon many pores have become isolated within the grains after being most common. A basic HIP system is shown Fig. 4 HIP Dimples on the surface of investment cast high temperature sintering. The pore indicated by the schematically in Fig. 1. platinum alloy jewelry in the rough, as-cast state. The red arrow still pins a grain boundary but it is about to As applied to the processing of sintered MIM dimples indicate that metal has flowed into a near- become isolated as that boundary breaks free and moves components, the HIP process is simple in concept. surface pore. After Fryé, et al. [16] to the lower left of the image. It is likely that this part would not consolidate to a pore-free density level during a gas simply penetrates the pore and the forces acting conventional HIP cycle. Image courtesy of Sandvik Osprey on the exterior of the part are matched by equal (Tingskog) [11] and opposing forces acting within the pore. If gas is trapped within a pore at the point at which the taken with consideration of all of the factors that affect Fig. 2 A schematic showing the HIP of material pore becomes isolated during sintering and that gas densification during HIP and the resultant mechanical containing a surface-connected pore. In this situation cannot diffuse away from the pore during HIP then properties. A casual approach, simply using established high pressure gas enters the pore and the gas pressure a phenomenon known as TIP (Thermally Induced de-bind and sinter practice and adding the most within the pore matches the external applied pressure. Porosity) is often observed. In this situation, the inexpensive HIP option that appears suitable for the alloy No densification occurs. Image after Mashl [14], a trapped gas becomes pressurised as the external being processed may not deliver the full potential of the modification (with permission) of images from Atkinson, hydrostatic force acts on the exterior of the part. The combined sinter plus HIP process. A high concentration of Davies [15] parts cool under pressure and thus following HIP the non-metallic inclusions or the inability of the HIP cycle to original pores are now much smaller but they contain eliminate porosity that has become isolated within grains, a pressurised gas. Any subsequent exposure to a result of grain growth during sintering and/or HIP can elevated temperature at ambient pressure, such as in conspire to thwart the intentions of the parts maker. On a post-HIP heat treatment will see the metal softened the other hand, when HIP is combined with conventional during heat treat and the pores expand back to their MIM processing and the entire process route is examined near original volume. and designed to work toward the achievement of a pore- With the exception of surface connected and gas free product, exceptional properties and performance is filled porosity, HIP is very effective in completely possible. eliminating porosity. A common question is “Will my parts become distorted during HIP?” The quick Fig. 1 A schematic of a hot isostatic pressing (HIP) answer is “Yes”. When pore volume is eliminated, Author system. The HIP unit, shown in the centre of the image there will be an overall volumetric shrinkage that can be described as a pressure vessel that contains a Dr Stephen J Mashl occurs, equal to the pre-HIP pore volume. In MIM resistance heated furnace. The parts to be processed Michigan Technological University products, where the post-sinter porosity is general are placed within the furnace, the pressure vessel is Fig. 3 When a pore is sub-surface and does cannot Materials Science and Engineering small and uniformly distributed within the part there closed and the furnace/pressure vessel is evacuated and contain any low diffusivity gasses HIP can completely 1400 Townsend Drive will not be any localised distortion, rather a uniform then back-filled with an inert gas. The gas supply and eliminate that pore. Change in shape and dimensions Houghton, MI 49931-1295, USA shrinkage of the piece. As shown in Figs. 3 and 4, compressors provide the high pressure gas which serves do occur. There will be an overall volumetric shrinkage Email: [email protected] in cases where near-surface porosity is present, as the pressure transfer medium. Electrical power heats equal to the volume fraction of porosity present prior indentations may be observed on the surface of the the furnace, and water is used to cool the pressure to HIP. Localized deformation during HIP can result in part after HIP. This is the result of the local flow of References vessel. In a typical HIP cycle, temperature and pressure the formation of dimples in the surface of the part, an metal into the subsurface pore volume. [1] Squire, A. , Density Relationships in Iron-Powder are ramped up to the target values simultaneously, held indication that metal has flowed into a near-surface Compacts, AIME Transactions V.171, 1947, pp. 485-505. at their desired values, then the furnace is cooled and pore. Image after Mashl [14], a modification (with [2] J. A. Sago, M.W. Broadley, J. K. Eckert, Metal Injection pressure is released. After Mashl, et al. [13] permission) of images from Atkinson, Davies [15] Molding of Alloys for Implantable Medical Devices,

International Journal of Powder docstoc.com/docs/79746433/Paper- Near Net Shapes Using Hot Isostatic Metallurgy, Volume 48, Issue 2, 2012, Defect-Investigation-Improvement- Pressing, JOM, July 1999, pp. 29-31 Centorr Vacuum Industries: pp. 41-49. Gas-Porosity [14] S. J. Mashl, Hot Isostatic Pressing [3] J. L. LaGoy, M. K. Bulger, Effect of [9] B. Hota, Contamination, of Castings, in “ASM Handbook, HIP on the Microstructure and Impact Disinfection, and Cross-Colonization: Vol. 15 Casting”, ASM International, Celebrating 60 years of Strength of MIM 17-4 PH Stainless Are Hospital Surfaces Reservoirs Materials Park, OH, 2008, pp. Steel, Advances in Powder Metallurgy for Nosocomial Infection?, Clinical 408-416. and Particulate Materials - 2009, T. J. Infectious Diseases; Vol. 39., 2004, [15] H. V. Atkinson and S. Davies, innovation in vacuum furnace Jesberger, S.J. Mashl, Editors, MPIF, pp. 1182–1189. Fundamental Aspects of Hot Isostatic Princeton, N.J. 2009. [10] ] R. M. German, Powder Pressing: An Overview, Metallurgical [4] Fraunhofer IPT, Process Metallurgy Science, 2nd Edition, and Materials Transactions A, Vol. production Strategies for Defect-Free, Metal Powder Industries Federation, 31A, December, 2000, pp. 2981-3000. Polished Steel Surfaces, www. Princeton, N.J. USA 1994, p.262. [16] T. Fryé, J. T. Strauss, J. Fischer- ipt.fraunhofer.de/content/dam/ [11] T. Tingskog, Effects of Powder Bühner, U. E. Klotz, The Effects of ipt/en/documents/110_02_ Size and Chemistry on Densification Hot Isostatic Pressing and Thermal Centorr Vacuum Industries is one of North America’s largest manufacturers Polishingdefectstcm362-71094.pdf and Properties of 316L MIM Parts Processing of Platinum-based [5] Uddeholm, Polishing of Mould Made Under Different Sintering Castings on Mechanical Properties of standardised and custom high temperature vacuum furnaces and the Steel, www.uddeholm.com/files/ Atmospheres, MIM 2013 – and Microstructures, Unpublished company has supplied furnaces to the MIM industry for nearly 30 years. During polishing-english.pdf.pdf International Conference on Injection Manuscript this period the company’s product range has continued to evolve as MIM [6] Uddeholm, Defect Chart and Hints Molding of Ceramics, Metals, has transformed into a dynamic global industry. Nick Williams interviewed for High Gloss Polishing of Steel Carbides, March 4-6 Orlando, FL, Surface, http://www.uddeholm.com/ 2013. Centorr’s Bill Nareski and Scott Robinson and reports on the company’s files/Defectchart-eng.pdf [12] S. T. Lin and R. M. German, history, its long association with the MIM industry and the unique perspective [7] N. Williams, Automation and a Mechanical Properties of Fully that the company can offer on technical and commercial developments. Focus on Value-Added Services Helps Densified Injection-Molded Carbonyl Metal Injection Moulding Thrive at Iron Powder, Met.Trans. A, Vol. 21a, OBE, PIM International, March 2011 Sept. 1990, pp. 2531-2538. [8] J. Annetts, Defect Investigation & [13] S. J. Mashl, J. C. Hebeisen, C. G. Improvement – Gas Porosity, www. Hjorth, The Production of Large P/M

This year Centorr Vacuum Industries line from the smallest laboratory floor of new breaking technology and, (CVI), based in Nashua, New Hamp- furnace to large production-sized when customers are looking to take shire, USA, celebrates sixty years of industrial equipment. Our experience a new advanced material from the vacuum furnace production. Over this in laboratory furnaces and working laboratory to full scale commercial period the company has installed over with corporate laboratories, as well production, we can be there with 6500 furnaces worldwide. The MIM as many major universities with the large scale equipment which we industry is an important market for a materials science programme, tailor as needed to run the customer’s the company and over the last year allowed us to get in on the ground process.” more MIM furnaces were commis- sioned than any other product line in the company’s diverse offering, accounting for 25% of its total equipment sales. Centorr Vacuum Industries was actually formed in 1989 following the merger of two separate furnace companies, Centorr Furnaces, founded in 1962 in Suncook, New Hampshire, a maker of small laboratory and R&D furnaces, and Vacuum Industries, a manufacturer of large production vacuum furnaces founded in 1954 in Somerville, Massachusetts. Bill Nareski, CEO of Centorr Vacuum Industries, told PIM Interna- tional, “It was the perfect fit between the two companies. It gave the Fig. 1 Centorr Vacuum Industries manufactures some of the world’s largest business an extremely broad product vacuum furnaces, including several 30 m long furnaces for the nuclear industry

MIM sales at 25% match or exceed MIM furnace development the annual MIM output of most of at Centorr our competitors. Our MIM numbers are just dwarfed by our higher sales Centorr was an early entrant into the figures for the over 65 different styles market for Metal Injection Moulding of furnaces that we offer for hundreds furnaces. “We broke into the field by of applications in the metals and being the first company to offer MIM ceramics industry.” The company process and cycle support in our exports approximately 40 - 50% of Applied Technology Center. Our early sales, with most of these furnaces work for some of the MIM industry’s being to Asia, Europe and Canada. pioneers turned into our first orders In January 2002 CVI completed from companies such as Remington a new building at its Nashua Arms, Megamet, Porite and headquarters which includes a tower Moldmasters,” stated Scott Robinson, facility with 5 ton hook and crane with Market Manager for the PIM and PM 1200 amp service and 350 KVA chilled sectors. glycol system. This enables CVI to CVI’s first dedicated design for Fig. 2 A Centorr MIM-Vac furnace under construction design and build large Vacuum Hot the growing MIM industry was the Fig. 3 A MIM-Vac furnace installed at Dynacast’s US MIM operation Presses, Chemical Vapour Deposition Injectvac™ furnace, introduced in the and Chemical Vapour Infiltration 1980s, which included a graphite hot furnaces as well as other vertical zone and a revolutionary gas plenum furnace designs for custom applica- retort design with hole pattern tions in the nuclear industry. designed to ensure proper flow “This investment in facilities dynamics of the inert and process and testing is necessary in order to gases over the surface of all the parts. support ongoing interest in advanced The Injectavac™ furnace processed ceramics for the semi-conductor, MIM parts from wax-polymer binder automotive and armour markets,” removal through to sintering in one stated Nareski. “To-date the new continuous cycle and included a dual building has been used for the pumping system (high-vacuum and construction of two large scale low-vacuum) which allowed it to be vacuum/controlled atmosphere hot used to remove both the first stage presses for advanced ceramics for wax binders as well as the second use in China and the United States, a stage polymers, before going up to tall vertical furnace for a proprietary sintering temperatures. process, a SiC CVD furnace and a host The first stage wax binders were Fig. 3 A Centorr MIM Gas Plenum Retort constructed of advanced Lanthanated Fig. 4 A MIM-Vac furnaces at Dynacast’s Singapore operation of other furnaces.” removed using a diffusion pump (sub- Molybdenum (ML) and TZM compositions for improved strength and durability For large furnace projects that atmospheric evaporation) at dewax do not fit in the company’s existing pressures less than 10-3 torr. The over 20 units installed in the USA and better utilised. CVI employs approximately sixty between 15 and 25% of the company’s building, CVI has access to another second stage polymers, on the other Europe and an additional 22 units in As newer, higher quality MIM people at its Nashua facility, with total annual sales. “While this may site in Nashua with up to 3,715 m2 of hand, would clog the diffusion pump China, Korea, and Japan sold through feedstock materials entered the around twenty additional sales and seem low compared to other vacuum manufacturing space. Since 2008 this but thermally break down at tempera- CVI’s licensee.” market more stringent demands on service agents representing the furnace companies, who specialise in facility has been used to construct a tures over 350°C into compounds As processes and technologies physical properties such as carbon company in Europe, Asia, Australia with relatively high vapour pressures. evolved the MIM industry moved away control became important and new and South America. The Nashua The high vapour pressures allow the from first stage thermal debinding in designs utilising a refractory metal facility has a 2,790 m2 manufacturing ‘Over the past ten years, CVI’s use of CVI’s proprietary Sweepgas™ batch furnaces and relied more on hot hot zone were needed to process and laboratory area plus an additional BRS™ (Binder Removal System) to water or solvent debind in the case these materials in a cleaner environ- 1,860 m2 of office space. A large 3 x MIM furnace business has grown carry the vapours away from the parts of traditional wax/polymer binder ment. 3 x 3 m pit in the main facility allows to between 15 and 25% of the in the direction of the pumps. Inert systems, or catalytic debinding for Leaning on its experience in for development of tall equipment, gas is bled into the furnace chamber polyacetal feedstocks. This processing high temperature refractory metal essential to support the company’s company’s total annual sales’ and the retort plenum, where it of first stage binder offline meant furnace designs for high temperature optical fibre drawing furnace product entrains polymers vapourised from that MIM vacuum furnaces no longer sintering at temperatures from line which supports the photonics the work pieces and carries them needed to handle the lengthy wax 1600°C to 2600°C, and its experience and telecommunications industry, as only one or two product lines or serve number of large 30 m long furnaces, out towards the BRS pump. “The unit debind portion of the cycle. This in debinding of over 200 different well as the construction of metal wire a single main industry and live or die some of the largest vacuum furnaces was very successful at the time,” allowed furnace manufacturers to types of organic binders, CVI annealing furnaces. on the strength of that business, in in the world, for processing nuclear commented Robinson, “and CVI focus on second stage debinding introduced its new line of Metal Hot Over the past ten years, CVI’s CVI’s case - with sales of between tubing for zirconium fuel rods and enjoyed the largest installed base of followed by sintering, where such Zone MIM units, named the MIM-Vac, MIM furnace business has grown to $25 and $30 million annually - our Inconel power water reactor tubing. graphite MIM furnaces worldwide with expensive capital equipment could be in 1999. “Today’s MIM-Vac™ furnaces

small, complex components using a Opportunities in micro-MIM far wider variety of metals,” stated Centorr is following the technical Nareski. work done in the micro-MIM field “Their new twist on the MIM very closely as it believes that this process involved the use of their own will continue to grow into one of the revolutionary die-casting machines, largest and most profitable segments modified to run conventional of MIM. The company has recently MIM feedstock. We believe it was enhanced its MIM furnace portfolio their desire to have equally high with the further development of performing furnace equipment to go a small continuous belt furnace along with their new process. After designed specifically for the micro- a few in-depth meetings where we MIM market. Based on CVI’s standard discussed the features and benefits continuous belt furnace design the of our design we agreed that, while furnace is constructed in a similar cost was an important factor in any way to a vacuum furnace, with water- purchase decision, Dynacast should cooled chamber and refractory metal take all factors into consideration hot zone. It can achieve a hydrogen Fig. 5 Refractory metal hot zones in Centorr’s small Fig. 6 Trays of small hinges on varied ceramic setter including overall cost of ownership gas dew point of -60°C in the main Fig. 7 The MIM-Vac ‘T/P’ Trap (Trap continuous belt furnace designed specifically for the materials including sapphire, ceramic paper and alumina and life expectancy of the expensive chamber after as little as 45 minutes Over Pot) for easy wax/polymer micro-MIM market powder hot zone components.” of purging with inert gas. Unlike removal features a double O-ring CVI also commented that it is conventional belt or pusher furnaces, groove seal for H2 safety are the result of almost 30 years of of time. This results in consistent providing two to three times the life reassured by ongoing growth and the hot zone can be brought up to experience in PIM technology and microstructures and repeatable expectancy of competitive designs. follow up orders from well estab- maximum temperature in as little as over 40 years debinding and sintering carbon control. The judicious use of lished firms in the MIM industry such 60 minutes and the unit can be turned experience in metals and ceramic advanced molybdenum alloys in the A unique perspective on as Parmatech Corporation, which is off at night and is cold within an hour. parts. The core design is based on our hot zone and retort, such as Lanthan- continuing the growth and expansion “Our belt furnace has been used ® MIM industry growth Workhorse Metal Hot Zone furnaces ated Molybdenum and TZM, offers plan that it started in 2010. There is successfully to process small MIM which have been sold worldwide for excellent creep resistance, higher Equipment suppliers are well placed also optimism about the growth of parts, such as orthodontics, in our the sintering of PM parts, with over recrystallisation temperatures and to understand industry growth trends MIM in Asia. Applied Technology Center using a 350 units in the field, and a variation longer service life. Our revolutionary and Centorr Vacuum Industries 100% hydrogen environment and has of the binder removal technology from new gas-plenum retort has rows of is no exception. Nareski told PIM Trends in materials achieved product densities of up to Sintervac® units that were developed perforations allowing even gas flow International, “We are encouraged Commenting on trends in MIM 98% theoretical density in 17-4PH by the recent period of high growth feedstock usage Robinson stated, and 316L parts with cycle times under in MIM over the past three years, “The range of MIM feedstock on the 120 minutes door-to-door. Future ‘The judicious use of advanced spurred in part in the US by the rapid market truly offers MIM producers a work in this field will centre around increase in the firearms business. It wide choice of materials. We continue further optimising cycle times,” molybdenum alloys in the hot zone is also refreshing to see firms new to to be surprised at the differences stated Robinson. “We believe that MIM, such as Dynacast International, and retort, such as Lanthanated that various feedstock systems this new small inline continuous MIM embrace this technology as a way to have on the day-to-day operation of belt furnace design could be a real Fig. 8 A basket of dual mechanical Molybdenum and TZM, offers excellent increase their product offering and MIM furnaces and their impact on game changer in terms of reducing filtration media is claimed to be more provide their customer base with maintenance schedules. We have manufacturing costs and provide efficient that condensation-based creep resistance, higher recrystallisation new materials and improved physical some customers who are cleaning a greener footprint for MIM parts trapping approaches properties.” temperatures and longer service life’ traps every one or two cycles, whilst makers.” As reported in the December 2013 others just check the traps once a hot zone and retort lifetimes,” stated issue of PIM International (Vol. 7 No. quarter!” Robinson. “Other work in this area for the tungsten carbide industry with across all the work trays and now 4, p 16), CVI received orders for four Efficiency gains and process In terms of the evolution of MIM has primarily centred on improving over 600 units in use worldwide,” includes removable plenum panels MIM-Vac M furnaces for Dynacast’s improvement material grades, CVI sees progress trapping efficiencies and looking Robinson stated. inset in a strong structural molyb- new MIM operation in 2013. “In in MIM titanium. “As the technology Centorr has worked with a number for ways to reduce the downtime “The MIM-Vac™ furnace is denum framework that allows fast our opinion, Dynacast was a savvy for stainless steels and low-alloy of key customers to improve the caused by maintenance tasks, all in designed primarily for second stage and easy removal and replacement of purchaser who had tremendous steels and their applications becomes debinding efficiency of their process an effort to shorten MIM cycles and binder removal and sintering, and has individual panels, minimising repair production experience as an saturated, it is only natural that the and explore ways to tighten up the the turnaround time between runs. To a number of design improvements costs and downtime.” international investment casting firm industry will look to new materials for hot zone and retort to ensure a higher do this we have been working closely specific for use with MIM feedstock. The company states that the use operating 22 manufacturing facilities this innovative processing technique. degree of carbon removal. “In one with vacuum dry pump manufacturers Tight partial pressure control and of a heavy duty molybdenum skeleton in 16 countries. In February 2013 Titanium MIM presents its own case the collaboration resulted in a to find ways to improve the robust even gas flow, in conjunction with framework with large cross-section they announced they would be adding barriers to commercialisation but reduction in the carbon content in operation and service life of their effective event-based programming structural members results in less MIM to their service offering and the it is impressive to see the progress stainless steel parts by over 50% and equipment.” and sound retort design, allows warping and creep over the life of the addition of MIM as a manufacturing that has been made in powder and reduced the effect of carburisation of CVI’s Applied Technology Center the entire load to view the same retort, as evidenced by current units process meant that the company feedstock formulations.” the hot zone components, increasing undertakes all in-house research series of conditions as a function in the field which, CVI claims, are could expand its ability to produce

customers know that we will be process end product with acceptably Outlook around for the long term providing low oxygen levels. spare parts, hot zones and “When the end-user considers “CVI has been at the forefront of field service, as well as furnace the overall capacity required, they high-temperature vacuum/controlled maintenance programmes, upgrades need to factor in their product mix. atmosphere furnace manufacturing and retrofits, rebuilds and controls. Large volumes of only one or two for decades and we have no intention In a recent informal survey, we found different parts can point towards of slowing down. My long-term goal that nearly 70% of the equipment using continuous furnaces, while for the company is to build on the we have built since 1980 was still up a mix of several different product position of strength we already have and bring Centorr Vacuum Industries to a point where we are considered ‘The need for this type of universally the primary resource for ultra-high-temperature equipment in equipment is only going to grow all the significant applications,” stated Nareski. “The need for this type of in the future and we’re going to equipment is only going to grow in the be prepared to meet that need’ future and we’re going to be prepared to meet that need.” “Our depth of experience in Fig. 9 MIM-Vac furnaces are conveniently mounted on a skid which allows for Fig. 10 A MIM-Vac control panel and running and we routinely provide grades or part sizes usually requires engineering and manufacturing has full unobstructed access to the chamber and surrounding equipment spare parts for some equipment built the flexibility that only vacuum batch resulted in several new advancements during the 1970s. It is this attention MIM units can offer with their ability and technologies for the processing of and is regarded as a major asset to designs. The variable and program- periodically, either manually or with to quality that allows our capital to vary cycle times and temperatures MIM parts. We have excellent financial the business. The Applied Technology mable belt speed allows for fast ramp routine solvent flushes.” equipment to perform under all for each individual need. While stability and a history of offering Center can simulate processes from rates and the small cross-section “Centorr has learned these facts types of conditions with repeatable small lower-cost box furnaces of 1 customers a long-term partnership high-vacuum to positive pressure uniform temperature hot zone at since our development work in the and reliable service.” to 2 ft3 are prevalent in the industry so they can be assured of a ready inert gas and operation in 100% < +/- 3°C means that parts can be 1980s and we have found several ways and used by firms as they gear up supply of spare parts and frequent upgrades and improvements to the hydrogen gas, with capabilities processed in a quarter of the time to reduce the time required for these Selecting the right MIM their production line, once volumes from 1000°C to 2800°C. This allows when compared to batch furnace maintenance tasks and make them increase it can make sense to design in order to keep their equip- furnace customers to test run their materials cycles.” easier to accomplish. We all know consider larger vacuum/hydrogen ment operating on the cutting edge.” in different gas atmospheres, vacuum that you could write the best SOPs CVI states that, when planning a MIM MIM furnace designs that routinely levels and hot zone materials when Furnace maintenance for your team to follow, but the more operation, of utmost importance is process 6 or 9 ft3 of material at a time Contact making the final adjustments to a new CVI strongly emphasises the difficult something is to maintain, the being sure of the actual material and offer active fan-cooling features Scott Robinson process. importance of good training and less likely it will get done right, or types that a part producer will be that can drastically shorten overall Centorr Vacuum Industries “Process evaluation is an maintenance procedures in order done at all! Our MIM furnaces have processing. Low-alloy steels are cycle times producing higher output,” 55 Northeastern Blvd important aspect of customer for MIM part producers to achieve easily accessible large water-cooled commonly processed in simple large stated Robinson. Nashua, NH 03062 service, enabling prospective users the highest levels of efficiency, traps with a removable basket filled sintering furnaces outfitted with “When it comes to understanding United States of high-temperature equipment to productivity and reliability from a with two different types of filtration small traps and no retorts, using total cost of ownership, a MIM firm Tel: +1 603-595-7233 test ideas and perfect operating MIM vacuum batch furnace. “For any media, including a simple binder pot vacuum or low partial pressures of needs to understand their costs for Email: [email protected] procedures so that equipment can be company installing vacuum batch on the bottom that can be removed inert gas, because the debinding power and gas usage and weigh this www.centorr.com properly specified to perform planned units for the first time there will and cleaned after each run. While step is less critical due to the high against their production schedule. operations. Testing in our Applied definitely be a learning curve as they one trap is good, two are even better, carbon content in the remaining While vacuum batch MIM furnaces Technology Center’s continuous get to know the furnace and develop and we include a second trap on the parts. typically have larger power supplies furnace has allowed several MIM a plan for its maintenance. These exit-end of the dry pumping system Higher grades of stainless steel than continuous furnaces, they are manufacturers to produce high- units are not heat treatment furnaces to catch any residual binder that such as 17-4PH and 316L require only operational during heating and quality materials in a quarter of the where you fill up the vacuum pumps makes it through the manifolding and more precise operating conditions not on 24/7 as with continuous pusher time required in a conventional batch with oil once a quarter and “let ‘em dry pump. With this design smelly with higher partial pressures (from designs. Hydrogen gas usage for an furnace design due to the reduced run”. These furnaces process several binder off-gas and small pieces of 100-300 torr) of typically Hydrogen average MIM cycle in a 9 ft3 furnace furnace cross-section and lower kilograms of nasty plastic binder uncombusted residual binder that gas and require more consistent gas could be as low as 25,000 litres for thermal mass. Because of the tight- residue each and every cycle and make it past the flame tower exhaust, flow across the surface of the parts; some alloys where reduced hydrogen ness of the vacuum-tested chamber they do it in such a way as to keep don’t rain down all over your nice hence expensive refractory metal gas flow is used to prevent decarburisa- and refractory metal hot zone inside the internals of the furnace clean clean furnace room,” commented plenum retort designs, to ensure low tion of the parts, and up to 80,000 and use of a proprietary patented enough to process low-carbon grades Robinson. carbon content in the finished parts. litres per cycle for other grades like molybdenum mesh belt design, these of expensive materials. Traps need to CVI’s Engineering and Aftermarket This can be below 0.03% in the case 17-4PH. Vacuum batch units addition- belt furnaces can operate in 100% be emptied and cleaned, manifolding Field Service Group plays an of some 316L applications. Likewise, ally do not require 24 hour operation hydrogen atmospheres at dewpoints needs to be checked at major important role in maintaining a titanium MIM grades also require the as the units can be scheduled so that as low as -60°C, offering cleanliness preventative maintenance campaigns reputation for high quality capital cleanliness that only a vacuum batch loading and unloading can occur at unlike traditional continuous furnace and dry pumps need to be cleaned equipment. Nareski stated, “Our MIM furnace can provide in order to defined times.”

Element C Si Mn P S Ni Cr Mo Nb

APMA 2013 conference: Content 0.25-0.35 0.75-1.75 ≤1.5 ≤0.04 ≤0.04 19-22 23-27 ≤0.5 1.2-1.5

Table 1 Chemical composition of HK30 powder, wt.% [1]

Advances in MIM applications because of unsatisfactory dimen- N2-sintered Ar-sintered sional tolerances and poor surface and materials presented in finish. The use of MIM as a net-shape Sintering Temp. (°C) 1300 1300 approach to producing these small Density (g/cm3) 7.65 7.50 and intricate parts in large quantities Xiamen has been able to solve the problem in Micro hardness (HV5/25) 247 162 an effective way. Rockwell harness (HRB) 90 78 A research group consisting of Ultimate strength R (MPa) 730 560 W Wang, M Ouyang, D Ye, J Song, F m Yield strength Rp (MPa) 332 194 APMA 2013, the 2nd International Conference on Powder Metallurgy in Pen and Y Yu from Xiamen Honglu 0.2 Tungsten Molybdenum Industry Co. Elongation A (%) 12.5 33.4 Asia, took place in Xiamen, China, November 3-6, 2013. This, the second Ltd. along with Z Zhuang from China conference to be endorsed by the Asian Powder Metallurgy Association National R&D Center for Tungsten Table 2 Properties of sintered parts at different sintering atmosphere [1] (APMA), has helped to firmly establish this conference series as important Technology, reported the research international events to match Europe’s EuroPM and North America’s results of MIM processing of HK30, one of the heat resistant austenitic (a) (b) PowderMet conferences. Lin Dongguo and Seong Jin Park, from Pohang stainless steel powders. They also University of Science and Technology (POSTECH), Korea, report on a showed images of actual production number of presentations relating to MIM applications and materials. components such as the nozzle ring for variable geometry turbochargers (VGT) fabricated by the MIM process. Based on a wax-polymer binder system, HK30 MIM feedstock was prepared. The powder morphology and particles size distribution are (c) (d) shown in Fig. 1, and Table 1 shows the APMA 2013 was the second interna- Japan Powder Metallurgy Association formats. Main topics included PM iron chemical composition of this powder. tional conference on Powder Metal- (JPMA), Japan Society of Powder & base materials, refractory metals and The MIM feedstock was prepared lurgy in Asia to be endorsed by the Powder Metallurgy (JSPM), Korean hardmetals, PM functional materials, with a powder loading value of Asian Powder Metallurgy Association Powder Metallurgy Institute (KPMI), powder forming, post-sintering treat- 60 vol. %, and the feedstock was (APMA) following the first conference, Korean Powder Metallurgy Asso- ment and PM non-ferrous materials. injection moulded into tensile test APMA 2011, held in Jeju, Korea, from ciation (KPMA), Powder Metallurgy In addition to a large number of specimens with the appropriate October 30 to November 2, 2011. Association in India (PMAI), Malaysian papers from China, reflecting the conditions. Two-stage debinding The 2013 event was successfully Powder Metallurgy and Particulate rapid progress and development of was carried out for the debinding Fig. 2 Microstructures of HK30 parts sintered in different atmospheres: (a) LOM organised by the China Strategic Alli- Materials Association (MPM2A) and China’s PM industry, papers were process; solvent debinding was image, N2 sintered; (b) SEM image, N2 sintered; (c) LOM image, Ar sintered; ance for Technological Innovation in Powder Metallurgy Australia (PMA). submitted by participants from all done in heptane for 8 h, and thermal (d) SEM image, Ar sintered [1] Powder Metallurgy Industry (SATI-PM) The conference’s technical world regions including the USA, debinding was done in N2 flow gas in in conjunction with the Taiwan Powder programme featured around 180 Europe, Japan, Korea, India, Australia, a batch furnace. Finally, sintering was Fig. 2 shows the microstructures The authors concluded that the Metallurgy Association (TPMA). papers that were presented in six Malaysia and Taiwan. carried out at 1300°C for 120 min in of HK30 parts sintered in different MIM process for HK30 heat resistant

Co-sponsors of the event were the sessions in both oral and poster partial atmosphere (N2 or Ar). atmospheres. For N2-sintered parts, stainless steel was now well advanced Advances in MIM technology Table 2 shows the effect of the grain size was in the range of and the MIM process highlighted had sintering atmosphere on final 60-70 μm and it was detected that Cr been successfully applied for the The process and properties for MIM properties of the sintered parts. In and Fe rich phases existed along the fabrication of the guide vanes of the

heat resistant stainless steel conclusion, the N2-sintered parts grain boundary. At the same time NbC nozzle ring for VGT applications as Heat resistant austenitic stainless have higher density, hardness, tensile particles dispersed uniformly in the shown in Fig. 3. steel is widely used for components strength and yield strength, but austenite matrix. These precipitates working at high temperature, such the elongation is much lower than were thought to be the reason for the Performance improvement of MIM as engine and turbocharger parts. the Ar-sintered ones. The authors increases in mechanical properties. Fe-50%Ni soft magnetic material Investment casting (IC) has been a claimed that the differences were However, in Ar-sintered parts smaller Fe-50%Ni is one of the most well- conventional process for manufac- mainly caused by the differences grain sizes of around 30-40 μm were known soft magnetic materials and turing these components in complex in microstructure formation during found and it was considered that MIM has been proved as a predomi- shapes. However the parts always the sintering process because of the this increased the elongation of the nant method for the production of Fig. 1 SEM image and particle size distribution of HK30 powder [1] needed some secondary operations different atmospheres. sintered parts. soft magnetic parts as an alternative

(a) (b) to traditional casting and machining. (a) (b) (c) A paper by Jidong Ma, Mingli Qin, Li Zhang, Lusha Tian and Xiaofeng Zhang, University of Science and Technology Beijing, China, aimed at studying the MIM process for fabricating high magnetic property Fe-50%Ni alloy, where the values of maximum permeability and saturation induction were 88745 and 1.58 T (d) (d) (f) Fig. 3 HK30 products fabricated by MIM, (a) HK30 guide vanes; (b) an respectively, far higher values than assembled VGT nozzle ring [2] typically reported for MIM Fe-50%Ni parts. (a) (b) Carbonyl iron and carbonyl nickel powders with particle sizes of 4.33 μm and 4.45 μm respectively were used as starting materials. The powder morphologies are shown in Fig. 4, where iron powder was regular spher- Fig. 5 Microstructures of different samples: (a) sintered at 1320°C, 2 h; (b) sintered at 1360°C, 2 h; (c) sintered at ical but nickel had branched chain. 1360°C, 10 h; (d) sintered at 1360°C, 12 h; (e) sintered at 1360°C, 10 h, HIP; (a) sintered at 1360°C, 10 h, HIP and 6 h The feedstock was made by mixing heat treatment [2] the two kinds of powders with weight Fig. 4 SEM images for powders: (a) carbonyl iron; (b) carbonyl nickel ratio of 1:1 and mixed with a wax- a further increase in sintering time. Rapid grain growth occurred with HIP Near spherical tungsten powder based binder system. After injection The authors claimed that for soft and heat treatment because of the prepared from tungsten oxide Sintering Sintering Saturation Coercive Maximum Relative moulding and debinding, sintering magnetic materials the saturation elimination of porosity and the high An impressive tungsten powder temperature time induction force permeability density + Hot Isostatic pressing (HIP) + induction depends on the material temperature involved. fabricating method was reported in a (°C) (h) Bs (T) Hc (A/m) μm (%) heat treatment was carried out. and its density, but is not affected by Finally, the authors concluded paper by Wang Congcong et al. from 1300 2 1.315 15.60 12386 93.8 Ring-shaped samples were used to grain size. Compared to saturation that a high performance Fe-50%Ni University of Science and Technology, 1320 2 1.368 14.36 13222 94.3 measure the magnetic properties. induction, the maximum permeability soft magnetic alloy was successfully China on behalf of their co-authors, Table 3 illustrates the effects of and coercive force are microstructure fabricated by MIM and the maximum Gai Guosheng and Yang Yufen from 1340 2 1.386 13.09 15673 94.6 sintering temperature and sintering sensitive parameters influenced by permeability value reached 112 Tsinghua University, China. Tungsten 1360 2 1.397 11.06 21897 94.6 time on the density and magnetic density, porosity and grain size. When mH/m, a significantly advanced result oxide powder was treated by the properties of sintered Fe-50%Ni alloy. the grains grow to a certain size, the compared to previously reported Particle Composite System (PCS) to 1360 6 1.468 8.25 36058 97.0 The density, saturation induction and driving force and resistance reach values for MIM Fe-50%Ni of 22.36- obtain the nearly spherical tungsten 1360 10 1.484 6.84 43541 97.2 maximum permeability increased a balance. Further sintering cannot 42.50 mH/m) after sinter + HIP + heat powder through reduction technology. PCS is a device that treats the 1360 12 1.484 6.82 43542 97.2 with increase of temperature from induce the grain growth and the treatment. 1300-1360°C, but the coercive force density does not increase any further. powder in a dry mechanised way 1360 14 1.484 6.79 43581 97.2 decreased. It was the same situa- Fig. 5e shows the microstructure Developments in MIM by high speed gas impact, which after a HIP process. There are no can modify the materials processed Table 3 Effects of sintering conditions on density and magnetic properties [2] tion for an increase in sintering time. related R&D After sintering for 10 h, there were pores and the sample is fully densi- into spherical tungsten powder by Relative Treatment B (T) H (A/m) μm modest value changes for density and fied. Table 4 shows the different prop- A significant amount of research compression and frictional force density (%) s c magnetic properties. erties of samples before and after work relating to conventional Powder between the particles. This manu- Sinter 97.2 1.484 6.84 43541 Fig. 5 shows the microstructures HIP. The authors indicated that the Metallurgy was reported during the facturing process provides some existence of internal stresses after four day conference and research significant advantages, such as a HIP 100 1.564 10.90 32039 of specimens fabricated in different process conditions. Some results can HIP caused a decrease of maximum relating to refractory metals and hard simple process, efficient production, Table 4 Density and magnetic properties before and after HIP [2] be obtained from the microstruc- permeability. materials accounted for a significant short production term, easy param- tures in Fig. 5 a-d as follows: i) the Additionally, high temperature heat proportion of this. China has the eter control, low cost etc. Relative amount of porosity decreased with treatment was carried out with a view largest refractory and hard materials The raw material used in this study Time (h) B (T) H (A/m) μm s c density (%) the increase in sintering temperature to eliminating or reducing stresses industry in the world, and Xiamen, was tungsten oxide powder with an 2 1.568 2.98 78159 100 from 1320-1360°C; ii) grain growth and improving magnetic proper- where APMA 2013 took place, is a average particle size of 12.61 μm. developed from about 30 μm to 100 ties. The effects of heat treatment major centre for the production of The raw powders were treated in a 4 1.570 2.82 81869 100 μm with temperature increase from on magnetic properties are shown in tungsten and its alloys in China. In modified PCS device with a rotational 6 1.572 2.66 86446 100 1320°C to 1360°C and a similar Table 5. The maximum permeability this second part of our APMA 2013 speed at 4000 r/min for five different effect was seen with an elongation of increased largely with longer heat conference report, two papers relating processing times (5, 10, 30, 45 and 8 1.578 2.56 88714 100 sintering time; iii) grain boundaries treatment times and changed little to powder production technologies 60 min). The modified powders were 10 1.579 2.52 88754 100 became straight when sintering time when a certain value was reached. for tungsten and its alloy powders, reduced in a hydrogen atmosphere was 10 h at 1360°C and there were Fig. 5f shows the microstructure of a and two papers relating to application at 780°C for 120 min to obtain nearly Table 5 Effects of heat treatment on magnetic properties [2] minor changes in microstructure with sinter + HIP + heat treatment sample. developments, are reviewed. spherical tungsten powders.

The SEM morphologies of the tung- Synthesis of superfine W-Ni-Fe (a) (b) (a) (b) sten oxide powders under different powders by a chemical method processing times with PCS are shown The W-Ni-Fe alloy is an important in Fig. 6. At first, the raw tungsten material for both scientific and oxide powder showed blocky granular military applications due to its excel- shape and sharp corners, but with lent wear resistance, good ductility the increase of PCS processing time, and high strength. Many methods the powders became subglobose as a have been investigated to improve the result of worn-off powder edges and mechanical properties of tungsten corners. As mentioned in this study, heavy alloys through the refinement (c) (d) after 15 min treatment, the edges and of microstructures. A paper about Fig. 8 SEM images of two powder: (a) calcined powders; (b) reduced powder [4] corners of large particles had almost the preparation of superfine W-Ni-Fe been removed and reached the best composite powders using a soft Sintering temperature (°C) treatment effect. When the processing chemical method, the Glycine-Nitrate Density time went up to 60 min, the particle Process (GNP), was given by Yan Liu 1350 1400 1450 1500 size decreased obviously because of a and Jigui Cheng et al. from Hefei Sintered density g/cm3) 17.32 17.62 17.93 18.33 crush phenomenon, which indicated University of Technology, China. too much energy and ground off edges. The raw materials used for Relative density (%) 92.3 93.9 97.5 98.6 The relationship between particle synthesis were APT, Fe(NO ) ∙9H O 3 3 2 Table 8 Densities after sintering at different temperatures [4] size and processing time is shown in and Ni(NO ) ∙6H O. They were (e) (f) 3 2 2 Table 6. dissolved in distilled water to form The 15 min treated tungsten oxide a homogeneous solution with the (a) (b) powder with best treatment effects Ni and Fe content of 3.5% and 1.5%, was reduced in hydrogen atmosphere respectively. Black precursor powders at 780°C for 120 min. The results were obtained by heating up the

are shown in Fig. 6c and Table 6. glycine (C2H5NO2) added solution. It The reduction of tungsten oxide can was then calcined at 500°C to remove typically be divided into four steps as residual organics and reduced in follows: hydrogen atmosphere at 800°C to Fig. 6 SEM images of tungsten oxide powders under different PCS processing 1) WO3 + 0.1H2 = WO2.9 + 0.1H2 convert into W-Ni-Fe alloy powder. times: (a) raw material; (b) 5 min; (c) 15 min; (d) 30 min; (e) 45 min; (f) 60 min [3] 2) WO2.9 + 0.1H2 = WO2.7 + 0.18H2 The SEM morphologies for precursor 3) WO + 0.72H = WO + 0.72H powders and the reduced powder are 2.72 2 2 2 (c) (d) Time (min) 0 5 15 30 45 60 4) WO2 + H2 = W + 2H2O shown in Fig. 8. The precursor powder had an average particle size of around D50 (μm) 12.61 4.92 4.76 4.24 4.15 2.65 In Fig. 7, the surface of the powder was polyporous and flawed after 2.4 μm with nearly spherical shape. Table 6 Mean particle size under different processing time reduction because the cracks made However, after reducing the powders became smaller, with an average by generated H2O evaporated from (b) (a) the particles as can be seen in the particle size of about 150 nm, and chemical equations mentioned above. the powders become agglomerated This also led to a loose structure and because of their high surface energy. some large particles broke down The synthesised W-Ni-Fe powders into small ones. Finally polyporous were sintered at temperatures Fig. 9 Microstructures of W-Ni-Fe samples sintered at different temperatures: nearly spherical tungsten powder was ranging from 1350-1500°C to study (a) 1350°C; (b) 1400°C; (c) 1450°C; (d) 1500°C [4] obtained with high porosity due to the their sintering behaviour. Table 8 water vapour release effect during shows sintered densities at different occurred and a maximum density of powder, spherical particles with an reduction. The EDS analysis results sintering temperatures. The nano- 98.6% was achieved. average size around 150 nm, was sized particles and fine tungsten, Microstructures of the W-Ni-Fe successfully produced by the gluyine- Fig. 7 SEM images of powders before and after reduction: (a) before reduction; (Table 7) showed that tungsten oxide nickel and iron ingredients in W-Ni-Fe sintered compacts are shown in nitrate process. After sintering at (b) after reduction [3] powder was almost totally reduced into pure tungsten powder. played an important role in improving Fig. 9. From Fig. 9 a-c the grains 1480°C, a high relative density (above Finally, the author concluded that sintering densification. A relative shown are irregular in shape and the 96%) and 2 μm grain sized W-Ni-Fe Sample Element Energy (keV) Mass (%) Atom (%) the method using PCS followed by density of about 92.3% was achieved average grain sizes increased from was obtained and with liquid-phase O K 0.525 20.07 74.26 the reduction process can be used to when sintered at 1400°C, a tempera- 2.51 μm (1350°C) to 3.99 μm (1450°C). sintering at 1500°C the sintered Before reduction produce nearly spherical or spherical ture below the melting point of γ-(Fe, However, when sintering at 1500°C, density increased to 98.6% and the W M 1.774 79.93 25.74 tungsten powder particles in mass Ni) phase, which was compatible to the tungsten phase was nearly microscopic hardness values was O K 0.525 0.47 5.21 production, which simplifies the that obtained from thermomechanical spherical in shape and grain growth about 480 MPa. After reduction method. At 1500°C, a higher tempera- was clear. W M 1.774 99.35 94.79 production process and also has many advantages, such as low cost, easily ture than the melting point of γ-(Fe, The authors concluded that a Table 7 EDS analysis of powder before and after reduction [3] controlled parameters and so on. Ni) phase, liquid-phase sintering superfine 95W-3.5Ni-1.5Fe composite

High-density tungsten/polymer density reached 11.6 g/cm3 at powder (a) (b) (a) (b) composites used in lead-free X-ray loading of 60 vol. %, a higher value radiation shielding than that of pure lead (11.3 g/cm3), Tungsten and its alloys have become which was helpful in improving its some of the most essential industrial radiation shielding ability. Also, the materials in numerous applica- tear strength and tensile strength tions because of their outstanding reached 18 kN/m and 5.9 MPa, performance, such as high density, respectively. hardness, conductivity and so on. A Lead equivalent value is the thick- report on new application of tungsten ness of lead that gives the same (c) (d) (c) (d) was given by Guozhang Zhao et reduction in radiation. In this work, al. from Xiamen Honglu Tungsten lead equivalent values of different Molybdenum Industry Co., Ltd, China, tungsten/TPE composites were with co-authors Zhigang Zhuang measured under conditions of 120 (Xiamen Tungsten Co., Ltd, China) and kV for incident voltage, 2.5 mm Al for Qingdong Zhong (Shanghai University, filtration and 6.0% for uncertainty. The China). Their paper aimed at the study results are shown as Fig. 12. A lead of high-density tungsten/polymer equivalent value of 2.43 mm Pb was composites used in lead-free X-ray obtained with 2 mm in thickness at 60 Fig. 13 Microstructures of W rod and W wire: (a) axial section of W rod; (b) cross radiation shielding. vol. % powder loading. section of W rod; (c) axial section of W wire; (d) cross section of W wire [6] (e) (f) Because of the outstanding The author said that three effects, shielding performance against both Compton Effect, Photoelectric Effect Content Content Content Element Element Element X-rays and γ-rays, tungsten and its and Electro Pair Effect, are the main (ppm wt) (ppm wt) (ppm wt) alloys have been utilised in many interaction patterns between X-rays Si 0.04 K <0.01 U <0.0001 radiation protection systems as a and substance. In this work, since the lead-free material. In this work, incident voltage is 120 kV, the former P 0.07 Na <0.01 Th <0.0001 a tungsten/polymer composite two effects played the leading role with high density, perfect radiation in absorption of X-ray energy. Thus, Ca 0.04 Ti 0.02 C 32 shielding performance, good flexi- the X-ray tube voltages of devices in Cr 0.07 Mo 0.05 N 42.9 bility, excellent workability and perfect nuclear medicine and security inspec- Fig. 10 SEM images of fracture surfaces of tungsten/TPE composites: (a) 10 vol. Fe 0.08 Ba 0.31 O 450 environmental suitability, based on tion are generally below 120 kV, this %; (b) 20 vol. %; (c) 30 vol. %; (d) 40 vol. %; (e) 50 vol. %; (f) 60 vol. % [5] thermoplastic elastomer (TPE) and tungsten/TPE composites sheets can Co 0.008 As 0.01 S 10 micro-sized tungsten powders, was satisfy radiation shielding require- Ni <0.005 Cu 0.01 H 63.9 successfully produced with powder ments at different X-ray exposure (a) (b) loading of 60 vol. %. The composite conditions and working environments. Total purity of W: 99.999931 wt.% was calendered into 2 mm thick Finally, they have concluded that Table 9 Impurities analysis of 6N W powder [6] sheets for properties measurement. a lead-free high-density tungsten/ Fig. 10 shows the microstructures polymer composite was produced for industries. The 5N W (>99.999 wt.%) • 6N W rods (wire): of fracture surfaces of tungsten/TPE the field of X-ray andγ -ray radiation and 6N W (>99.9999 wt.%) electrodes 6N W powder -> CIP -> Sintering composites with different tungsten shielding. The composite was demon- are usually used in ultra-high-perfor- -> Swaging & Drawing -> powder loadings. A widely particle strated to have the necessary performance (UHP) gas discharge lamps, Straightening (Electrolytic size distributed tungsten powder was mance such as high density, perfect and high purity W-Ti and W-Si are cleaning) used after physical and chemical radiation shielding performance, good Fig. 11 Densities and mechanical properties at different powder loading: (a) used for sputtering targets in semi- modification in order to obtain high flexibility, excellent workability and • High purity W alloys: density and shore A hardness; (b) tear strength and tensile strength [5] conductor chips. flowability and high bulk density. At environmental suitability. 6N W powder & Ti (Si) powder -> In-house developed 6N W powder powder loading of 60 vol. %, the tung- CIP -> Hot pressing -> Machining has been introduced in this study. sten particles were tightly stacked, Ultra high purity tungsten and its & Polishing (a) (b) Based on the powder, W rods and smaller ones were packed in spaces applications. The contents of impurity elements wires were made for special lighting between larger ones and spaces in Another paper was reported by Yang in 6N W powder are shown in Table 9, applications, and 5N W-Ti and close-packed particles were filled Yu et al., also from Xiamen Honglu and the mean particle size was 4N W-Si sputtering targets were with TPE. The author claimed that the Tungsten Molybdenum Industry Co., about 2.4 μm with a nearly spherical also developed successfully. Three blurred boundaries between tungsten Ltd, focused on production and appli- shape. Using this powder, W elec- different processes were used to particles and TPE matrix showed an cation of ultra-high purity tungsten trodes (diameter: 12-40 mm) and W produce each product as following: efficient polymer-filler interfacial powder. wires (diameter: 0.02-12 mm) were network had been constructed. Ultra high purity (>99.9999 wt.%) • 5N W electrodes: produced with a W purity value of The densities and mechanical tungsten and its high purity (>99.999 6N W powder -> CIP -> Sintering 99.99989 wt.% and 99.999922 wt.%, Fig. 12 Lead equivalent values of different tungsten/TPE composites: (a) properties of tungsten/TPE compos- wt.%) alloys are the vital materials for -> Forging -> Machining & respectively, and their microstruc- different powder loading (b) different thickness [5] ites are summarised in Fig. 11. The special lighting and semiconductor Polishing tures are shown in Fig. 13. Higher

APMA 2013 Gallery Advances in PIM process simulation speed up the development of micro parts

Simulation technology for the Powder Injection Moulding (PIM) process has advanced rapidly in recent years, with software now tailored specifically to APMA 2013 Opening Ceremony APMA 2013 Award Presentations modelling the injection moulding of PIM feedstock. In this report Jochen Heneka and Tobias Müller, Karlsruhe Institute of Technology (KIT), Germany, and Dr Marco Thornagel and Dr Laura Florez, SIGMA Engineering GmbH, Germany, present an overview of the most important developments for the simulation of PIM applications along with a case study illustrating how effectively simulation can support mould design and quality control in micro-PIM applications.

APMA 2013 Exhibition Opening APMA 2013 Welcome Banquet

purity was couple with lower diameter purity powders can be used in the References The simulation tools available into feedstock behaviour while being That deviations were found are product, because the fine wires were MIM industry for the production of a [1] W Wang, et al., The process and to the PIM industry have evolved moulded. Large deviations were understandable: thermoplastics are fabricated by self-resistance sintering number of new high purity tungsten properties of metal injection molded substantially over the last five found, however, and simulation was quite different in nature from PIM at higher temperature around 2700- and tungsten alloy parts. heatresistant stainless steel, as years. During Arburg’s 50th regarded sceptically as a tool able to feedstock and its rheological and 2800°C, which was favourable to presented at APMA 2013, China Anniversary PIM Conference, held deliver, at best, only a general idea of thermal behaviour requires different improving the purity of W. Also, 5N Authors [2] Jidong Ma, et al., Improvement of in Lossburg, Germany, June 2013, flow behaviour. modelling. In the last few years W-10Ti alloy and 4N W-30Si alloy magnetic performance of Fe-50%Ni Ingo Cremer (EPMA President targets were produced successfully Lin Dongguo alloy by Powder Injection Moulding, as 2007–2013) gave an overview of the with W purity value of 99.999 wt.% and Pohang University of Science and presented at APMA 2013, China leading new technologies in PIM. 99.99 wt.% respectively. Technology (POSTECH) [3] Wang Congcong et al., Nearly In his presentation he highlighted The authors have concluded that 77 Cheongam-Ro, Nam-Gu, Spherical Tungsten Powder Prepared simulation as one of the key using the in-house developed tech- Pohang, Gyeongbuk, by Reduction of Modified Tungsten technological trends for PIM and nology a type of 6N W powder had Korea Oxide and Its Mechanism Analysis, as stated that simulation software “is been mass produced, and using Tel: +82 54 279 8763 presented at APMA 2013, China now mature” and “a must for part this powder full dense 5N and 6N W Email: [email protected] [4] Yan Liu, et al., Synthesis of development.” rods and wires had been produced ultrafine W-Ni-Fe powders by soft Simulation is not new to the PIM successfully. In parallel, related W Dr Seong Jin Park chemical method, as presented at industry. It is widely recognised that alloy products, 5N W-10Ti and 4N Pohang University of Science and APMA 2013, China the injection moulding stage is critical W-30Si sputtering targets, had been Technology (POSTECH) [5] Guozhang Zhao et al. Microstruc- for green part quality and that errors developed for micro electronic indus- 77 Cheongam-Ro, Nam-Gu, ture and Properties of High-Density induced here cannot be corrected tries successfully. Pohang, Gyeongbuk, Tungsten/Polymer Composites, as later on. Therefore, from the very There is no doubt that this type of Korea presented at APMA 2013, China beginning moulders have relied on material will be used in many other Tel: +82 54 279 2182 [6] Yang Yu et al., Ultra high purity conventional injection moulding industrial areas where there is a need Email: [email protected] tungsten and its applications, as simulation tools – designed to model Fig. 1 PIM feedstock shows an increase in viscosity at low shear rates, respon- for very high purity levels in the final the behaviour of thermoplastic sible for several flow effects. A suitable rheological model must be used in the product. It is believed that such high presented at APMA 2013, China materials – to gain some insight simulation to capture this particular behaviour [1]

requirements, weld line appearance, been possible to determine in which air entrapments, required cycle cases air, water or even a copper time and the balance of multi-cavity insert should be used to remove moulds. Also regions of extreme heat from a particular hot-spot in a shearing, where particle segregation moulding application, or to identify is likely to appear, can be identified at which material alloys to select for the an early stage. mould to improve cycle time.

Modelling viscosity changes at low Advanced modelling of powder- shear rates binder separation A model recently integrated in SIGMASOFT® is investing significant SIGMASOFT® which captures the development resources to predict the increase in viscosity at low shear effect of powder-binder separation rates has brought enormous benefits [2]. When flowing through narrow to the flow front predictability [1]. This Fig. 4 Left: overall demonstration micro turbine used in the SFB 499. Right: Fig. 2 An increase in the shear rate can produce particle separation from the cross sections in the mould, particular viscosity increase is not turbine guide wheel [3] binder system. Simulation can identify the high shear rate regions susceptible feedstock may undergo high only highly relevant for the packing to particle segregation [2] shear rates, which force particle phase, but also for the behaviour segregation from the binder, as can Case study: Simulation of quality and precision. A vario- of the feedstock close to the mould be seen in Fig. 2. This undesired delivers first-shot success thermal process control is required, walls where the shear rate is low, as effect can lead to pores or differences in micro PIM and the cavities must be evacuated to seen in Fig. 1. in local density of the sintered part, provide the best preconditions to get In comparison to thermoplastic which in extreme cases may lead to Despite being a highly profitable a complete mould filling. Otherwise materials, which show a plateau at stress concentration and part failure. market with limited competition, defects such as diesel-effect marks, low shear rates, the filling pattern is By using tracer particles the defects micro moulding still remains or sink marks, can appear. The runner changed, as well as the position of created by segregation can already be somehow a “taboo” area for PIM system and the inserts are crucial; weld lines and effects such as jetting identified. are more likely to appear. The internal In 2013 a major breakthrough stress distribution is also different. was brought to the market with a ‘When flowing through narrow All these effects call for the use of new technology, called SIGMASOFT® software able to capture PIM flow Virtual Molding. Besides predicting cross sections in the mould, behaviour, instead of conventional the flow and solidification behaviour software for thermoplastic moulding of feedstock materials, it is now feedstock may undergo high simulation. possible to reproduce the complete shear rates, which force particle Fig. 3 SIGMASOFT® includes material models able to capture the moulding injection moulding process, with Understanding the thermal behaviour of microparts. The pressure curves for the two-cavity mould (left on all its details over several cycles. segregation’ interaction between mould and the top) proved to correlate good with real measurements [4] The effect of several moulding feedstock parameters, such as the waiting Another important commercial use time between cycles, the insert companies. There are several reasons insert manufacturing is expensive ® important developments have been As a result, the time-to-market is of SIGMASOFT software has been in pre-heating temperature or the for this. On the one hand the handling, and time consuming, because the made to integrate suitable material shortened, the mould design – even the selection of a tempering system. effect of after-moulding thermal positioning and assembly of micro requested tolerances are often on models able to capture the particular the design of the tempering media or Because the thermal conductivity and treatments can be considered. This parts, as well as quality inspection, the limits of conventional machining behaviour of PIM feedstock. layout – is optimised and, foremost, the heat capacity of PIM feedstock new technology, released at the K are challenging. On the other hand, methods, such as HSC milling or ® The SIGMASOFT software the risk of mould rework or iteration can be one order of magnitude higher Show 2013, brings the accuracy of micro-dimensions bring a completely micro-EDM, and sometimes special provided by SIGMA Engineering on the steel mould is reduced and in than those of thermoplastics, it is simulation to a complete new level new behaviour into the process. The manufacturing methods such as X-ray GmbH based in Aachen, Germany, some cases even avoided altogether. also necessary to use thermal models and delivers a vast insight into the tiny dimensions change the basic or UV LIGA processes are required. has proved that simulation is now that are able to simulate the complex root causes of several effects found in physical behaviour of the feedstock, These cost factors require careful far closer to solving the challenges A review of current thermal interaction between mould the injection moulding process. and phenomena which do not have mould design and make later iteration faced by the PIM industry than ever and feedstock. A highly developed applications of simulation in As a result of these developments any relevance in conventional PIM costly and risky. before. Models integrated to predict thermal solver originally developed for it is possible to move ever closer suddenly have a major importance. Powder Injection Moulding the rheological behaviour at low shear the simulation of foundry processes to the needs of PIM industry. The Effects such as surface tension, Simulating injection moulding in rates, and the ability to predict the SIGMASOFT® software has been used is able to calculate, at every time-step integrated models are now able increased surface-to-volume ratio micro dimensions effect of the high thermal conductivity widely in PIM companies, for material in the moulding cycle and at every to reproduce with unprecedented or heat transfer in micro dimensions In recent years significant of PIM feedstock in the thermal selection and part design through to location of the mould, the precise accuracy the flow and thermal require a steep learning curve. development efforts have been made, behaviour of the mould, now deliver mould evaluation and process setup. temperature, product of the complex behaviour of feedstock so that in parallel to our PIM activities, to a very accurate correlation between When developing a new application, heat balance between the hot mistakes can be avoided early in The challenges of mould design for improve the prediction of injection simulation and reality, capturing even simulations are run to compare the feedstock releasing large amounts the design stage and an optimum micro PIM moulding simulation in micro complex flow kinetic effects such behaviour of different materials, to of energy into the mould, and the solution minimising cost and time Moulds used for micro PIM need to dimensions. Micro dimensions create as jetting or particle segregation. evaluate factors such as the pressure moulding system. It has for example effort can be found. fulfil special requirements in terms specific challenges for simulation

picture. The required moulding The development of a ZrO2 micro turbine guide wheel pressure was considerably lower, At the Karlsruhe Institute of and weld lines were placed in Technology (KIT), Germany, a non-functional areas of the part research project (SFB 499) was (between the turbine blades). In conducted dealing with the process summary, the design of the optimised chain for the development of highly runner system promised good stressed micro parts made out of pre-conditions for the later replication ceramic and metallic alloys [3]. Within of the green parts, and was used for the project, a micro turbine guide the fabrication of the mould in steel. The moulded ZrO2 micro turbine wheel was moulded out of ZrO2, as seen in Fig. 4. As a requirement, the guide wheel green parts showed a free-form surfaces of the blades had well shaped outer contour without to be free of defects to fulfil their any visible defects (Fig. 7). The mould function. with the optimised mould inserts Fig. 5 Left: first design of the turbine guide wheel with three runner channels. In this case simulation was used and runner system provided a stable Right: pressure result after 1.5 s filling time. Incomplete filling is seen [3] to validate the concept proposed for replication process suitable for mass production without additional part moulding. In a first step, the Fig. 7 Three-plate mould built following simulation recommendations and iteration needed on the steel mould. feedstock, containing 50.5% ZrO2 green parts produced [3] and a combination of polyethylene, The sintered parts had a theoretical paraffin wax and dispersant as binder, density of over 99%, without the of PIM industry, involves several was characterised. The viscosity was presence of shrink holes, burrs or References chip-offs and the linear shrinkage features and material models which measured using a high pressure [1] M. Thornagel: “Injection moulding was around 21%. This first-shot dramatically improve reliability and capillary rheometer and with the simulation: New developments offer success was based on, amongst other accuracy of the flow and thermal same equipment the thermodynamic rewards for the PIM industry”. PIM factors, the use of injection moulding behaviour predicted. Even in micro- properties were studied, producing International, Vol.6 No.1 March 2012, simulation at the mould design stage moulding applications, simulation has a PvT curve (pressure vs. specific pages 65-68. and on the rigorous characterisation proved to be a useful tool up to the volume and temperature). Beyond [2] M. Thornagel: “MIM-simulation: of the feedstock data. point of delivering first-shot success. this, the thermal conductivity and A virtual study on phase separation”. Motivated by the success achieved, Simulation has to be understood specific heat capacity were measured. EuroPM2009, Copenhagen, October a new micro PIM project was as a valuable tool and has to be well- The first tested concept considered 2009 proposed at the KIT. A design concept integrated into the part and mould three distribution channels, [3] J. Heneka, T. Müller, M. Thornagel: was created and optimised, based on design process. Only then will the systematically arranged as seen in “Micro-Molded CIM-Components: the described simulation approach. expected success potential for micro Fig. 6 Left: Improved runner design with eight channels. Right: pressure result Fig. 5. The moulding parameters Simulation based Mold- and Process After the feasibility of the production PIM actually be achieved. after 1.5 s filling time. Complete filling is observed [3] foreseen in the simulation were an Development”. EuroPM2013, process was demonstrated through injection time of 1.5 s, a holding Gothenburg, Sweden, September 2013 simulation, the virtual results were as the tiny geometrical dimensions and simulated pressure curves are pressure time of 1.6 s and cooling Acknowledgements [4] M. Thornagel: can influence the numerical presented for the two cavity mould. used to apply for the necessary time of 15 s. The simulation showed The micro-moulding project was “Spritzgusssimulation an algorithms. A specific R&D project The shape of the pressure curves, funding. The budget was awarded, the an incomplete filling, high injection carried out with the support of the Werkzeugkonzepten für Nano- was undertaken to integrate and the maximum level and the signal- mould built and the next first-shot pressure and the presence of weld Karlsruhe Nano Micro Facility (KNMF, Kompositen. BMBF Projekt PROMI“, validate material models suitable lost point are well predicted by the success achieved. lines in functional areas over the www.kit.edu/knmf), a Helmholtz final project presentation. Fakuma turbine blades. Research Infrastructure at Karlsruhe 2011, Friedrichshafen, October 2011. ‘Micro dimensions create specific After these defects were observed, Summary Institute of Technology (KIT, www. a new design was proposed: the PIM has become a key production kit.edu). The funding of this work Contact number of runner channels was challenges for simulation as the technology for the manufacturing within Collaborative Research raised to eight and all edges Dr. Marco Thornagel, Dr. Laura Florez of metal and ceramic micro parts. Center SFB 499 by Deutsche tiny geometrical dimensions can were rounded to improve the flow SIGMA Engineering GmbH The moulding stage determines Forschungsgemeinschaft (DFG) is conditions of the melted material, as Kackertstr. 11 part quality, as defects induced gratefully acknowledged. Thanks influence the numerical algorithms’ can be seen in Fig. 6. Each runner 52072 Aachen here cannot be healed later on. also to the colleagues in the SFB 499, channel was connected to the turbine Germany Furthermore, in micro PIM the costly especially Markus Welz and Klaus for the modelling of micro-parts [4]. simulation. Thus, it was proved that a guide wheel in the middle of each Tel: +49 241 89495 0 mould manufacturing methods do not Plewa for their work. In Fig. 3, the two micro applications predictive simulation tool is available turbine blade to avoid weld lines in Fax: +49 241 89495 20 make iteration on steel mould viable. used to validate the research results for micro moulding applications. In functional areas of the final part. The Email: [email protected] These arguments make simulation are presented. The upper left image combination with the PIM specific production parameters used in the www.sigmasoft.de an important and profitable tool to be is an instrumented two cavity mould functionality, MIM and CIM micro- simulation were the same as in the applied early in the design stage. and the lower left image is a micro applications can therefore also now first simulation. SIGMASOFT®’s software, developed tensile test specimen mould. On the be simulated with using SIGMASOFT® The results of this second iteration specifically to serve the interests right side of Fig. 3 both measured software. showed a significantly improved

Global PIM Patents The structure and performance of WC-10%Co Cemented Carbide inserts made by Powder Injection Moulding The following abstracts of PIM-related patents have been derived from the European Patent Organisation databases of patents from 1,2 1,2 1,3 throughout the world. She Q. Wang , Sunhe Liu , Wen Guanghua 1 Zhuzhou Cemented Carbide Cutting Tools Co., Ltd, Zhuzhou, Hunan, 412007, China 2 State Key Laboratory of Cemented Carbides, Zhuzhou, Hunan, 412000, China 3 3 Central South University, Changsha, Hunan ,410083, China

Corresponding author: Shequan Wang; Email: [email protected]

green compact into a brown body by JP2011099406 (A) debinding, holding the brown body Powder Injection Moulding (PIM) is a very important Powder Metallurgy (PM) forming method that METHOD OF MANUFACTURING on a solid implant base body made can meet the precision requirements for the manufacture of complex shaped cutting tool inserts. FUEL INJECTOR AND NOZZLE of pure titanium or titanium alloys, PIM processing imparts less deformation and is suitable for the manufacture of complex shaped SINTERED BODY and producing the finished implant parts. This paper investigates the structure and performance of WC-10%Co cemented carbide cutting Publication date: 2011-05-19 from the solid implant base body by tool inserts made by PIM. The performance of PIM products is affected by both the binder and the Inventor(s): Yamagishi Hiroaki, sintering. The surface of the implant debinding process during manufacturing. By adding a special polymer binder, which comprised Honda Motor Co Ltd, Japan is sprayed with titanium plasma, PW, oil, DOP, HDPE, EVA etc., mixed together with powder, inserts were manufactured by injection The problem to be solved with where the layer thickness of the moulding. The solvent and thermal debinding processes were analysed. By adapting and optimising this patent is to provide a method titanium coating is 1-10 mu m. the debinding and sintering processes, high quality inserts were produced. Cutting test results of manufacturing a fuel injector indicate that the lifetime of the inserts after Physical Vapour Deposition (PVD) coating is better for into a cavity corresponding to the capable of promptly and reliably those made by PIM than those made by conventional die compaction. forming fine fuel injection ports at shape of the nozzle to be formed. After mould closure an injection the front end of a metallic nozzle DE102009046003 (A1) moulding step of pressing and without the need for expensive METHOD FOR PRODUCING A filling binder-added powder metal facilities. COMPONENT WITH A CERAMIC into the cavity is performed. The method of manufacturing the FIRST AREA AND A METALLIC The sliding pins are moved back fuel injector includes a pin inserting SECOND AREA to the injection moulding die. The step. Protruding sliding pins, having Publication date: 2011-04-28 nozzle moulding is removed from diameters, numbers, positions and Inventor(s): Dirscherl Florian, angles corresponding to the fine fuel the injection moulding die and then Robert Bosch GmbH, Germany With the development of high performance cutting technology, injection ports to be formed at the sintered to manufacture a nozzle This patent describes the method cemented carbide cutting tool inserts are becoming ever front end of the nozzle are inserted sintered body with slender tubular Cemented Carbide for producing a component with a more complex as tolerance requirements increase [1, 2]. Die Binder from an injection moulding die voids formed by the sliding pins. Powder ceramic first area and a metallic compaction technology cannot meet the requirements of second area, where a ceramic complex inserts because of the non-uniformity of the density. KR20110125549 (A) DE102010028432 (A1) material is present in the first area Powder Injection Moulding (PIM), which is derived from and a metallic material is present HEAT RESISTANT STEEL ARTICLES MANUFACTURING A SPATIAL plastic injection moulding, is a net-shape forming process that Mixing AND METHOD FOR PREPARING THE IMPLANT STRUCTURE FROM PURE in the second area. The process combines high part complexity with high production quantities. SAME TITANIUM comprises of applying the ceramic The products prepared by PIM are expected to have a more Publication date: 2011-11-21 Publication date: 2011-11-03 material in a first tool area of a tool homogeneous microstructure since hydraulic pressure is applied Pelletising Inventor(s): Song Jun Ho et al., PIM Inventor(s): Grundei Hans Dr Ing, S by means of a first injection moulding during injection moulding and the mould is filled uniformly, Korea Co Ltd, Korea & G Implants GmbH, Germany step. The metallic material is applied which avoids the density gradients experienced in conventional Injection A Metal Injecting Moulding (MIM) The patent describes a method of in a second tool area of the tool by press/sinter processing [3]. It is important to control the solid method of manufacturing a heat- manufacturing a spatial implant means of a second injection moulding load ratio of the binder because of the high WC powder density. Debinding resistant steel part in order to enhance structure made of pure titanium or step. During the production of inserts by PIM, it is important to reduce erosion resistance, hardness, wear titanium alloy with an open-mesh, Laser radiation and microwave product defects, improve accuracy and control carbon content resistance, and durability under a high three-dimensional network structure radiation is used to heat the tool to [4, 5]. Additionally, cemented carbide is sensitive to the binder Sintering temperature is discussed in this patent. having mesh sizes of 1.5-6 mm 1200-1500°C. The tool is heated in and the debinding process. By investigating the ultra-fine (sub- The heat-resistant steel part is formed partially covering the surface. The such a way that the ceramic material micron) WC–10%Co insert manufacturing process, this paper Inspection from Cr-Ni-Nb heat-resistant steel process comprises of producing a is connected with the metallic summarises some critical results by investigating the application and has a surface hardness of over green compact via metal Powder materials. of PIM for the production of ultra-fine submicron cemented 180VHN. Injection Moulding, transforming the carbides. Fig. 1 The PIM process

3 tolerance on dimension. The injection moulding machine and Component Chemical structure Melting temperature Tm(°C) density r(g/cm ) Content % a) b) mould is of course a factor in achieving stable insert weight;

2 paraffin CnH2n+2 54~80 50 however, the flowability and shape retention of the mixing powder is critical. Fig. 2 shows images of the insert ZTBD02002- — [CH-CH2]-[CH-CH2] y]n — — MG. From this picture, it can be seen that there are no cracks or EVA 90 0.96 10 other defects. COCH3

HDPE — [CH-CH]n — 140 0.98 12 Analysis of the debinding process c) d) Solvent debinding process SA CH3[CH2]16COOH 66 0.96 2~3 After the green inserts were produced, solvent debinding, which DOP C H [COOH (CH ) CH ] 18 0.97 2~3 6 4 2 2 6 3 2 is critical for the quality of the inserts, took place. During solvent OA — 0~5 0.917 1~2 debinding, the soluble component of the binder is dissolved in the solvent solution. The binder component paraffin dissolved when Table 1 Binder components the solvent was heated to around 80°C. Running this process too Experiment debinding and the sintered insert. The mechanical properties quickly or with higher temperatures will cause defects. Porosity of the specimens were determined using an Instron material will form from the surface to the middle during solvent debinding Fig. 3 SEM morphology of different debinding times (a: before Materials tester and a HV hardness tester. The magnetic performance was and the pores that are created become connected. Fig. 3 shows debinding, b: 50 min debinding, c: 100 min debinding, d: 240 The WC–10%Co powder mixture used in the experiment measured by ZS-1 Co-magnetic and coercimeter 93-IE. The the structure of the inserts during different solvent debinding min debinding) was supplied by Zhuzhou Cemented Carbide Works. The thermal performance of EVA and HDPE was analysed by DSC. stages. Normally, the dissolved component should be desorbed characteristics of the WC powder are 0.79 μm Fisher particle Cutting tests were made by machining and the machined material almost entirely during solvent debinding. Correct selection of size and that of the Co powder is 1.23 μm. 0.5% TaC (1.2 μm) was 0.45% carbon steel. solvent debinding temperature and time will contribute to quality was also added. uniformity. The binder components comprised PW (Paraffin Wax), oil, Results and discussion As can be seen from Fig. 3, by adopting the experimental DOP (Dioctyl-Phthalate), HDPE (High-Density Polyethylene), process, there are no defects in the solvent debound insert and EVA (Ethylene Vinyl Acetate) etc., and this binder is then mixed Manufacture of the PIM inserts the porosity distribution is uniform and this will contribute to together with the powder. The contents and properties of each Because of the high density of the cemented carbide powder good thermal debinding. binder component are listed in Table 1. and the selection of a finer WC particle size for the WC-10%Co material used in the experiment, the solid powder loading rate Thermal decomposition of undissolved binder material Experimental procedure cannot be set at a high value [6][7]. In order to achieve ideal After the low molecular weight component of the binder system The binder ingredients were melted in a special device at 150°C rheological performance and shape retention, the EVA and has been removed, the remaining binder in the cemented carbide for 1 h. Then, the WC–10%Co powder mixture was blended with DOP components in the binder were increased and HDPE was will decompose prior to sintering. Heating up rate and time are the binder in a SHR-10A mixer at 140°C for 2 h. The inserts decreased. The solid load ratio selected was 55%. By adopting related to the heat characteristic of the polymer binder. By DSC were then injection moulded in a HTF58x2 injection moulding a suitable mixing process, the inserts ZTBD02002-MG were analysis, we can obtain the data of the polymer heat up. Figs. machine at 140°C at an injection pressure of 55 MPa. After this, manufactured using the WC-10%Co feedstock. The quality 4 and 5 show two polymer TG-DSC curves. The curves show Fig. 4 HDPE TG-DSC curve a solvent debinding step was performed, followed by a thermal uniformity of the finished PIM insert is related to the uniformity that HDPE and EVA will melt at 136°C and 92°C separately. debinding step. Sintering took place at 1410°C for 1 h in a at the time of injection. During the injection moulding process, HDPE will start to decompose at 408.9°C, strongly decompose COD633 furnace. Fig. 1 shows the PIM manufacturing process. the quality uniformity can be checked by the deviation of the in the temperature range of 440-468°C and decomposition weight of the inserts [8]. Table 2 shows the insert weight data. will end at 467.9°C. EVA will start to decompose at 300°C, Property measurements The weight deviation is between 1.754 g and 1.783 g, with the strongly decompose in the temperature range of 416-460°C and An SEM JSM-5600LV was used to observe the cross-sectional percentage of the weight deviation being 0.3%. The tolerance decomposition will end at 480°C. microstructures of the green PIM insert, the insert after solvent is 0.004 g, which can meet the accuracy requirement of 0.1% Based on the thermal characteristics of EVA and HDPE, three debinding and sintering cycles were designed as follows:

1.782 1.780 1.781 1.782 1.779 1.779 1.780 1.780 1.782 1.783 Cycle 1: From room temperature the furnace is heated to 1.782 1.783 1.783 1.779 1.782 1.779 1.781 1.783 1.780 1.780 350°C at a speed of 2°C/min followed by a holding time 1.783 1.779 1.780 1.780 1.780 1.781 1.780 1.780 1.782 1.783 of 60 min, then heated to 450°C at a speed of 3°C/min followed by a further holding time of 60 min. Finally the 1.783 1.783 1.782 1.782 1.782 1.779 1.780 1.781 1.780 1.781 furnace is heated to 1410°C at a speed of 10°C/min for a 1.783 1.780 1.780 1.782 1.780 1.782 1.781 1.780 1.781 1.782 sintering period of 60 min in an argon atmosphere of 40 bar 1.781 1.782 1.782 1.779 1.782 1.780 1.781 1.781 1.779 1.779 pressure. Up to the 450°C hold, a H2 flow rate of 50 slm and Fig. 5 EVA TG-DSC curve a pressure of 1020-1030 mbar are used. 1.783 1.780 1.780 1.782 1.780 1.782 1.781 1.780 1.781 1.782 1.781 1.782 1.782 1.779 1.782 1.780 1.781 1.781 1.779 1.779 Cycle 2: From room temperature the furnace is heated to Cycle 3: From room temperature the furnace is heated to 320°C followed by a holding time of 120 min, then to 380°C 380°C at a speed of 2°C/min followed by a holding time of 1.782 1.783 1.783 1.779 1.782 1.779 1.781 1.783 1.780 1.780 followed by a holding time of 60 min, and then to 450°C at 180 min, then heated to 450°C at a speed of 2°C/min followed 1.783 1.779 1.780 1.780 1.780 1.781 1.780 1.780 1.782 1.783 a speed of 2°C/min followed by a holding time of 60 min. by a holding time of 120 min. It is then heated to 1410°C at 1.783 1.783 1.782 1.782 1.782 1.779 1.780 1.781 1.780 1.781 Finally the furnace is heated to 1410°C at a speed of 10°C/ a speed of 10°C/min for a sintering period of 60 min in an 1.782 1.780 1.781 1.782 1.779 1.779 1.780 1.780 1.782 1.783 min, for a sintering period of 60 min in an argon atmosphere argon atmosphere of 40 bar pressure. Up to the 450°C hold, of 40 bar pressure. Up to the 450°C hold, a H2 flow rate of 50 a H2 flow rate of 50 slm and a pressure of 1020-1030 mbar Fig. 2 Insert ZTBD02002-MG Table 2 Insert weight data (g) slm and a pressure of 1020-1030 mbar are used. are used.

a) a) b) c)

d) e) f) Cycle 1

Fig. 9 Wear morphology of inserts after 30 grooves (a, b and c: PIM inserts; d,e and f die compacted inserts)

Considering the forming method, a surface quality comparison is 0.15 μm, while the flank wear of the die compacted inserts is Cycle 2 was made. The surface structure of the PIM inserts is more 0.26 μm. Fig. 10 shows that the flank wear value of PIM inserts uniform and flat. The roughness values of the PIM insert and die after machining 100 grooves is equal to that of the die moulded Fig. 6 Metallographic images of the WC-10% inserts produced Fig. 8 SEM morphology photo of AlTiN coated inserts compacted inserts are Ra0.346 and Ra0.345 respectively. Fig. 7 inserts after machining 60 grooves. using cycles 1 and 2 (a: PIM, b: Die compacted) shows the surface structure. The cutting lifetime of PIM inserts is therefore longer than that From the images in Fig. 7, we can see that the surface of the of die compacted inserts. One of the reasons for this is that the D Hc TRS a) b) Com Metallog- Method (g/ (KA/ Hv (N/ PIM insert is more uniform than that of the die compacted insert. uniform density of the PIM inserts results in higher accuracy of (%) raphy cm3) m) mm) After confirming the necessary PIM production process, the inserts the complex inserts and less deformation. Secondly, compared Die ZTBD02002-MG were made by both PIM and die compaction. with die compaction, there is less friction in the case of the PIM 14.44 8.9 22.8 1670 2240 A02B00C00E00 compacted The dimensions of the insert ZTBD02002-MG were measured. process, so this improves the cutting edge quality compared to PIM cycle 1 14.42 10 21.3 1630 1980 A02B00C06E00 The 3-dimensional shrinkage rates of the die compacted inserts the die compacted inserts. Fig. 10 shows that there are micro- are 18.37% (length), 18.03% (width) and 17.36% (height). The breaks in the cutting edge of the die compacted inserts compared PIM cycle 2 14.45 9.0 22.6 1660 2320 A02B00C00E00 3-dimensional shrinkage rates of the PIM inserts are 18.55% with the PIM inserts. Thirdly, by adapting the binder and PIM cycle 3 14.45 8.9 23.1 1670 2280 A02B00C00E00 (length), 18.53% (width) and 18.85% (height). The shrinkage debinding process, the mechanical performance of the ultrafine rate deviation of the PIM products is 0.3% while that of the die 10%Co-WC cemented carbide inserts is the same as that of the Table 3 Physical and mechanical performances of WC-10%Co moulding inserts is 1%. The PIM inserts ZTBD02002-MG are die compacted inserts. debinding and sintering process 1, 2 and 3 plus a conventional therefore more accurate than the die compacted inserts. die compaction process c) d) Inserts cutting test Conclusion Through these three different debinding and sintering cycles, it Groove cutting tests were undertaken with both the PIM and By adopting a binder comprising PW, oil, DOP, HDPE, EVA was shown that there is a carbon phase in the inserts produced die compacted inserts. The inserts were coated with AlTiN. etc. and mixing together with the ultrafine powder WC-10%Co, using the first cycle. The structure is normal in the second cycle SEM images of the coated inserts are shown in Fig 8. These ZTBD02002-MG inserts were made via Powder Injection as shown in Fig. 6. The physical and mechanical performance is images show that the inner structures of the PIM inserts and the Moulding. Because of the high specific surface of the fine WC showed in Table 3. die compacted inserts are very similar to each other. Because powder, the solid load of the binder is approximately 55%. From Fig. 6 it is shown that the low debinding temperature the blank surface of the PIM inserts is more uniform, the joint Although this is a relatively low solid loading, the weight of the and short debinding time will cause debinding deficiencies and between the substrate and AlTiN coating is better for the PIM green inserts is very stable and there is good shape retention. there is carburisation in the cemented carbide. On the other inserts. After sintering, there is more uniform shrinkage rate in the hand, in cycle 2, with appropriate debinding temperature and The machined material is a 0.45% carbon steel. The cutting three orthogonal directions compared with the die compacted sufficient time, the binder can decompose adequately. Although parameters are: cutting speed 120 m/min, the depth of cut 3 mm inserts. Fig. 7 The surface morphology of die compacted and PIM the holding time of cycle 3 is longer than that of cycle 2, the final and the feed 0.1 mm/r. After 30 grooving tests, Fig. 9 shows that Using the TG-DSC method, the thermal characteristics of inserts (a and c are die compacted sintering inserts; b, d are performance varies little as shown in Table 3. This indicates that the flank wear of PIM YBG202/ZTBD02002-MG is lower than HDPE and EVA were investigated and appropriate debinding PIM inserts) the debinding time in cycle 2 is long enough. that of the die compacted inserts, the flank wear of PIM inserts and sintering processes were designed. Compared with the die

a) b)

Technical Programme Available May 2014

Fig. 10 a) wear morphology of PIM inserts after 100 grooves b) wear morphology of PM die compacted inserts after 60 grooves

compacted inserts, there is similar mechanical performance, [7] J.Bruhn, B.Terselius. (Hogskolan Kristianstad, Sweden.), morphology structure and surface roughness. The surface Injection Moulding Of Tungsten Carbide-Cobalt. EURO PIM’97 INTERNATIONAL structure of the PIM inserts is more uniform than that of the papers which were presented at the First European Symposium die compacted equivalents. For complex shape inserts, there is on Powder Injection Moulding, which was held in Munich, higher accuracy when using the PIM process, because there is a Germany, in October 1997. CONGRESS & EXHIBITION more uniform density distribution. [8] Shye YunnHeng, Norhamidi Muhamad, Abu Bakar Sulongn, An AlTiN coating was applied to the WC-10%Co/ Abdolali Fayyaz Sri Yulis, M.Amin, Effect of sintering ZTBD02002-MG inserts and cutting tests were undertaken. The temperature on the mechanical and physical properties of results show that the lifetime of the PIM inserts is longer than WC–10%Co through micro-powder injection molding(μPIM), 21 - 24 September 2014 that of die compacted inserts. Ceramics International 39 (2013) 4457–4464 The Messezentrum Salzburg, Austria Acknowledgements The authors thank the National Science and Technology Program Top Grade NC Machine and Base Equipment 2012ZX04003041 project.

References [1] Wang Shequan, Li Chen, Ping Li and Yong Du, Mechanical properties and Microstructure evolution of TiN Coatings Alloyed with Al and Si. 17th Plansee Seminar 2009, Vol.2 Mechanical Properties [2] Wang Shequan, Chen Li, Yin Fei, Li Jia, Research on microstructure and properties of TiN, (Ti, Al)N and TiN/(Ti, Al)N multilayer coatings, The 2006 Powder Metallurgy World Congress, Busan, Koera, 2006. 9 [3] Zhu Baojun, Qu Xuanhui, Tao Ying, Powder injection molding of WC–8%Co tungsten cemented carbide, International Journal of Refractory Metals & Hard Materials 20 (2002) 389– 394 [4] Tao Li , Qingfa Li , J.Y.H. Fuh , Poh Ching Yu , L. Lu, Two-material powder injection molding of functionally graded WC–Co components Int. Journal of Refractory Metals & Hard Materials 27 (2009) 95–100 [5] M.Youseffi, I.A.Menzies. (Loughborough University of Technology, (UK.) Injection Moulding Of Tungsten Carbide- For more information and to Cobalt Using. Powder Metall., Vol40, No 1, 1997,62-26. [6] Yan Li , Zhimeng Guo, Gelcasting of WC–8wt%Co tungsten view the Technical Programme cemented carbide, International Journal of Refractory Metals & Hard Materials 26 (2008) 472–477 visit www.epma.com/pm2014 Developing the Powder Metallurgy Future the Powder Developing 78 Powder Injection Moulding International March 2014 © 2014 Inovar Communications Ltd Vol. 8 No. 1 Vol. 8 No. 1 © 2014 Inovar Communications Ltd March 2014 Powder Injection Moulding International 79 Events / Advertisers | contents page | news | events | advertisers’ index | email |

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