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INTERNATIONAL

July/August 2007

43/4

powdermetallurgy

international journal of

REACH: New European Regulation2007 PM Design Excellence AwardsState of the North American PM Industry—2007High-Performance Nickel-Steel Powder MixesPrecipitation Hardening PM Stainless Steels

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rom developing new materials that lead toproperty advancements or PM process efficiency,to working with our customers to achieve the mostcost efficient solutions using PM technology, we’recommitted to providing powder metallurgy solutions…for every part of the world! And, alongthe way, be assured we will continue to invest in

manufacturing capacity to support industry growth globally while providing design, process, andmaterial system education wherever it is needed. Powder metallurgy solutions…for every part of theworld. It’s much more than a tagline. It’s our commitment to you.

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Powder metallurgy solutions…for every part of the world.

© 2006 Hoeganaes Corporation

international journal of

powdermetallurgy

The International Journal of Powder Metallurgy (ISSN No. 0888-7462) is a professional publication serving the scientific and tech-nological needs and interests of the powder metallurgist and the metal powder producing and consuming industries. Advertisingcarried in the Journal is selected so as to meet these needs and interests. Unrelated advertising cannot be accepted.

Published bimonthly by APMI International, 105 College Road East, Princeton, N.J. 08540-6692 USA. Telephone (609) 452-7700. Periodical postage paid at Princeton, New Jersey, and at additional mailing offices. Copyright © 2007 by APMI International.Subscription rates to non-members; USA, Canada and Mexico: $90.00 individuals, $210.00 institutions; overseas: additional$35.00 postage; single issues $45.00. Printed in USA by Cadmus Communications Corporation, P.O. Box 27367, Richmond,Virginia 23261-7367. Postmaster send address changes to the International Journal of Powder Metallurgy, 105 College Road East,Princeton, New Jersey 08540 USA USPS#267-120

ADVERTISING INFORMATIONJessica Tamasi, APMI International105 College Road East, Princeton, New Jersey 08540-6692 USATel: (609) 452-7700 • Fax: (609) 987-8523 • E-Mail: [email protected]

INTERNATIONAL

EDITORIAL REVIEW COMMITTEE P.W. Taubenblat, ChairmanI.E. Anderson, FAPMIT. AndoS.G. CaldwellS.C. DeeviJ.J. DunkleyW.B. EisenZ. FangB.L. FergusonW. FrazierK. Kulkarni, FAPMIK.S. KumarT.F. MurphyP.D. NurthenJ.H. PerepezkoP.K. SamalH.I. SanderowD.W. Smith, FAPMIJ.E. SmugereskyR. TandonT.A. TomlinD.T. Whychell Sr., FAPMIM. Wright, PMTA. Zavaliangos

INTERNATIONAL LIAISON COMMITTEED. Whittaker (UK) ChairmanV. Arnhold (Germany)E.C. Barba (Mexico)P. Beiss (Germany) C. Blais (Canada)P. Blanchard (France)G.F. Bocchini (Italy)F. Chagnon (Canada) C-L Chu (Taiwan)H. Danninger (Austria)U. Engström (Sweden)N.O. Grinder (Sweden)S. Guo (China)F-L Han (China)K.S. Hwang (Taiwan)Y.D. Kim (Korea)G. Kneringer (Austria)G. L’Espérance, FAPMI (Canada)H. Miura (Japan)C.B. Molins (Spain)R.L. Orban (Romania)T.L. Pecanha (Brazil)F. Petzoldt (Germany)S. Saritas (Turkey) G.B. Schaffer (Australia)Y. Takeda (Japan)G.S. Upadhyaya (India)

Publisher C. James Trombino, CAE [email protected]

Editor-in-Chief Alan Lawley, [email protected]

Managing EditorPeter K. [email protected]

Advertising ManagerJessica S. [email protected]

Copy EditorDonni [email protected]

Production AssistantDora [email protected]

President of APMI International Nicholas T. [email protected]

Executive Director/CEO, APMI International C. James Trombino, CAE [email protected]

3 Editor's Note5 PM Industry News in Review9 PMT Spotlight On … Patricia A. Ditson

11 Consultants’ Corner Myron I. Jaffe15 APMI Fellow Awards Thomas F. Murphy and Howard I. Sanderow17 2007 PM Design Excellence Awards Winners

P.K. Johnson

HEALTH & ENVIRONMENT27 The New European REACH Regulation: A Major Challenge

to Manufacturers and ImportersP. Brewin

ENGINEERING & TECHNOLOGY 33 State of the PM Industry in North America—2007

E. Daver and C.J. Trombino

RESEARCH & DEVELOPMENT 39 High-Performance PM Steels Utilizing Extra-Fine Nickel

L. Azzi, T. Stephenson, S. Pelletier and S. St-Laurent51 Precipitation Hardening PM Stainless Steels

C. Schade, P. Stears, A. Lawley and R.D. Doherty

DEPARTMENTS60 Meetings and Conferences61 APMI Membership Application 63 PM Bookshelf64 Advertisers’ Index

Cover: Grand Prize–winning parts from MPIF’s 2007 Design Excellence Awards Competition

Contents 43/4 July/August 2007

You buy more than metal powder – you buy knowledge!

w w w . n a h . c o m

EDITOR’S NOTE

Volume 43, Issue 4, 2007International Journal of Powder Metallurgy 3

In 1927 Irving Berlin composed a popular ballad titled “The Song is Ended.”To quote from the lyrics of one stanza in the song:

“The song is endedBut the melody lingers onYou and the song are goneBut the melody lingers on”

In a musical sense this song captures the essence of PowderMet2007—while the technical program and exhibition are now history, the positive vibesremain, the memory of a Rocky Mountain high.

This post-show issue of the Journal includes the text of the “State of the PMIndustry in North America—2007” address given by Edul Daver and JimTrombino. Also included is Peter Johnson’s coverage of the “2007 PM DesignExcellence Awards Competition.” Grand Prize–winning parts are displayed onthe front cover.

A regular contributor to the “Consultants’ Corner,” Mike Jaffe providespractical insight into diverse readers’ questions. Issues he addresses are thecompaction of flake-like particulates, a performance comparison between newsophisticated presses and older basic units, and environmental aspects ofnitrogen-based sintering atmospheres compared with those based on the combustion of natural gas.

The new European legislation titled Registration, Evaluation, andAuthorization of Chemicals (REACH) is designed to make manufacturers andimporters register the details of chemicals (including metals and alloys) in acentral European database. Impetus for this law stems from ever-increasingconcerns for the protection of human health and the environment. FormerEPMA Technical Director Peter Brewin traces its genesis and explains the newregulation, its projected impact on metal powder suppliers and PM parts producers, and the implementation timetable. In a global economy, MPPA andPMPA members need to be fully cognizant of REACH—now.

Two “Research & Development” articles complete the technical content ofthis issue. Azzi et al. demonstrate that the physical and sintered properties ofbinder-treated nickel-copper steel mixes can be enhanced by using extra-finenickel powder (D50 = 1.5 µm) instead of standard-size nickel powder (D50 = 8 µm). In the second article, Shade et al. document the physical and mechanical properties and attendant microstructures of two precipitation-hardening PM stainless steels: 17-4PH, a high-chromium, martensitic stainlesssteel; and a new cost-effective, low-chromium dual-phase (ferrite/martensite)alloy that utilizes copper in the precipitation reaction. The latter alloy exhibitshigh strength, toughness, and fatigue resistance coupled with moderate corrosion resistance.

In the “everything-you-always-wanted-to-know-but-were-afraid-to-ask” category, nanotechnology terminology probably ranks high on the list. Beafraid no more since all is revealed in a new ASTM standard designated E-2456-06 titled “Standard Technology Relating to Nanotechnology.”Terminology is given for agglomerate, aggregate, fine particle, nano, nanoparticle, nanoscale, nanoscience, nanostructured, nanotechnology, non-transitive nanoparticle, transitive nanoparticle, and ultrafine particle.Central to the terminology is the word “nano,” meaning 10-9 meters (m), orpertaining to things on a scale of approximately 1 to 100 nanometers (nm).

Alan LawleyEditor-in-Chief

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PM INDUSTRY NEWS IN REVIEW

Remington Arms SaleRemington Arms Co. has agreed tobe sold to Cerberus CapitalManagement LP, N.Y., a private-equity firm, reports BloombergNews. The transaction terms include$118 million in cash and assump-tion of $252 million of debt.

New PM Plant Opens in China Miba AG, Laakirchen, Austria,opened a new plant, Miba PrecisionComponents China, in the SuzhouIndustrial Park, near Shanghai, onMarch 26. The company has invest-ed 10 million euros in the plant andwill produce bearings and PM partsfor the Asian market.

New PIM PublicationPowder Injection MouldingInternational is a new magazinescheduled to be published quarterlyby Inovar Communications Ltd.,Shrewsbury, U.K. The publicationwill cover the global markets formetal, ceramic, and cemented carbide injection molding.

Microwave Sintering Introducedto U.S. MarketSpheric Technologies, Inc., Phoenix,Ariz., will showcase the Spheric/Syno-Therm line of high-temperature microwave furnaces atPowderMet2007, the MPIF/APMIInternational Conference on PowderMetallurgy & Particulate Materials,May 13–16, in Denver, Colorado. Thefurnaces are manufactured by Syno-Therm Co. Ltd. in China.

Updated Literature on PowderAttritorsUnion Process, Inc., Akron, Ohio,offers a new mini CD containingupdated literature describing itssize-reduction and dispersing equipment. The company supplieswet and dry grinding attritors, smallmedia mills, grinding media, labservices, reconditioning services,and custom toll processing.

HIP Conference Call for Papers The International Conference on Hot Isostatic Pressing (HIP’ 08)requests abstracts for technical presentations. The conference willbe held May 6–9, 2008, inHuntington Beach, Calif.

Powder Sales Up Höganäs AB, Sweden, reported an 8 percent sales increase to approximately $211 million for thefirst quarter of 2007. Operatingincome increased 15 percent toabout $28 million.

Tungsten Production Increase North American TungstenCorporation Ltd., Vancouver, BC,Canada, reported production at itsCantung mine in March increased to25,998 metric ton units (MTUs) oftungsten concentrate (WO3) from24,472 MTUs in February. The average grade for March was 1.5percent of WO3 with an averagerecovery of 74.6 percent.

New Edition of Standard TestMethods Released The Metal Powder Industries

Federation (MPIF) has announcedthe publication of the 2007 Editionof Standard Test Methods for MetalPowders and Powder MetallurgyProducts. The most current versionsof these standards, which are usedin the manufacture of both metalpowder and powder metallurgy products, are required by QualityAssurance programs in order tomaintain full compliance.

Titanium Development FundingAwarded The U.S. Department of Defense isproviding $1 million to support additional research on compactingtitanium powder to full densityusing patented adiabatic technologydeveloped by LMC, Inc., DeKalb, Ill.The grant supports the formation ofthe National center for TitaniumMachining in Rockford, Ill.

GKN Releases 2006 PM Sales GKN plc, London, England, reported2006 powder metallurgy (PM) salesof approximately $1.164 billion, aslight decline from 2005. NorthAmerican sales were significantlyweaker, while sales in Europe andthe rest of the world increased.

Acquired PM Parts CompanyRenamedNetShape Technologies, Inc. (NTI), isthe new name of the former HawkPrecision Components Group,acquired by Saw Mill Capital LLC.The company plans on locating corporate headquarters in theLouisville, Ky., vicinity.

The following items have appeared in PM Newsbytes since the previousissue of the Journal. To read a fuller treatment of any of these items, goto www.apmiinternational.org, login to the “Members Only” section, andclick on “Expanded Stories from PM Newsbytes.”



Swedish Metal Powder MakerDoubles Capacity in BrazilHöganäs AB, Sweden, will investabout $7.5 million to build a newiron powder atomizing plant inBrazil. The company decided todouble its iron powder manufacturing capacity therebecause of strong and growingdemand in South America for PMgrade and consumable powders.

Distinguished Service to PowderMetallurgy AwardsTwelve North American individuals,each of whom has worked a minimum of 25 years in the PMindustry and has made long-termcontributions and achievementsdeserving of special recognition,

Award-Winning PM Parts Outstanding powder metallurgy(PM) parts were recognized in the2007 Powder Metallurgy DesignExcellence Awards Competition during the recent PowderMet2007conference in Denver. The competition, the 43rd such eventsponsored annually by the MetalPowder Industries Federation(MPIF), singled out parts used indiverse market segments—automotive, lawn & garden/off-highway, hardware/appliances,hand tools/recreation, medical/dental, and industrial motors/controls & hydraulics.

have been awarded theDistinguished Service to PowderMetallurgy Award given by theMetal Powder Industries Federation(MPIF). The presentation of theawards took place at the IndustryRecognition Luncheon during thejust concluded PowderMet2007International Conference onPowder Metallurgy & ParticulateMaterials conference in Denver.

ARC Metals Celebrates 20thAnniversaryARC Metals, Ridgway, Pa., a custom pre-mixer and recycler offerrous metal powders, will celebrate its 20th year in business.Hoeganaes Corporation purchasedthe company in 1997.



Mathson Industries To OpenNew Plant Mathson Industries, Inc., Troy,Mich., has announced it will opena new 103,000 sq. ft. plant inHodges, Greenwood County, S.C.The company will invest $5 million in the new facility that willcreate an estimated 50 new jobs.

Parts Maker Installs NewInspection System Chicago Powdered Metal ProductsCo., Schiller Park, Ill., hasinstalled the 3100 process compensated resonant test (PCRT)system made by MagnafluxQuasar Systems, Glenview, Ill. The new system with two testheads will inspect all PM partsproduction for a new automotiveprogram.

Miba Sales Grow Fiscal year 2006/2007 sales at

Components Association. Thebreakdown covers iron and copper-base PM parts, bearings,and friction materials.

Italian PM Industry GainsIn 2006 the PM parts productionin Italy increased 10 percent toalmost 32,000 short tons of ironand copper-base parts, reportsASSINTER, the Italian PM association. The industry’s 22companies posted total sales of223.6 million euros.

EPMA Conference The European Powder MetallurgyAssociation’s (EPMA) EuroPM2007 Conference & Exhibitionwill take place in Toulouse,France, October 15–17. The technical program features 250oral and poster technical papers,special interest seminars and aworkshop.

Miba AG, Laakirchen, Austria,increased about 5.7 percent fromthe previous fiscal year to 367 million euros. The companyearned 22.2 million euros beforeinterest and taxes, compared with22.4 million euros in the2005/2006 fiscal year.

New Powder for Higher-DensityPartsHoeganaes Corp., Cinnaminson,N.J., has introduced AncorMax200, a new lubricant/binder system for high-density PM gears and parts. The company is targeting AISI 8620 steel properties.

PM Grows in ChinaProduction of PM parts and prod-ucts in China increased 15 percentin 2006 to about 86,000 shorttons, reports the PM Association ofChina General Machine

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ijpm


Education:Rochester Institute of Technology, BS Mechanical

Engineering, 1995Kettering University, MS Manufacturing Management,

1999

Why did you study powder metallurgy/particulatematerials?Since I grew up in St. Marys, I had an early introduc-tion to the powder metallurgy (PM)industry. While I did not study PM orparticulate materials specifically, I wasalways looking for PM applications inmy engineering studies and in myearly work.

When did your interest in engineering/science begin?I have always had an interest in sci-ence and mathematics, particularlyphysics and the physical sciences. Iwas a “closet” geek, even back in highschool.

What was your first job in PM? What did you do? My first employment in the PM industry was a tempo-rary job sorting parts in a PM plant in St. Marys.Knowing that I did not like that very much, I decidedthat more education was in my future.

Describe your career path, companies worked for,and responsibilities.Out of high school I served an apprenticeship as adesigner for OSRAM Sylvania for four years. I contin-ued working for Sylvania, both full and part-time,while my children were small. I returned to college in1991, dragging my kids with me. During college Iworked for Cummins Engine in three separate studentcoop engineering assignments. After college, I went towork for Dresser Industries as a quality engineer. Fromthere I went to The Carbide Graphite Group, Inc., as aquality manager. I joined North American Höganäs in2002 as their quality control manager.

What gives you the most satisfaction in yourcareer?I enjoy finding resolution to an issue, whether it istraining, conflict management, or helping a customerreach a successful problem outcome. Finding the solu-tion that works for all parties involved is my goal andis most satisfying.

List your MPIF/APMI activities.I am a member of the West PennChapter of APMI International. I alsoserve on the MPPA standards commit-tee and on the material standards com-mittee for brass and bronze. I haveattended the Basic and Advanced PMShort Courses and have also attendedPM technical conferences.

What major changes/trend(s) in thePM industry have you seen?I think the major trend is toward moretechnology. Parts are becoming more

complex so that every push in new directions is goodfor the PM industry.

Why did you choose to pursue PMT certification?I was trying to increase my knowledge of the industryand I felt that this was a good benchmark of thatachievement.

What are your current interests, hobbies, and activities outside of work?I enjoy reading almost anything. Also, I like working onour yard; some might call this landscaping or garden-ing, but I am not that artistic. I also enjoy time spentwith my family.

SPOTLIGHT ON ...

PATRICIA A. DITSON

Director Quality, Safety and EnvironmentalNorth American Höganäs, Inc.111 Hoganas Way Hollsopple, Pennsylvania 15935Phone: 814-479-3668Fax: 814-479-2003E-mail: [email protected]

ijpm

Call OSRAM SYLVANIA at 570/268-5000, visit www.sylvania.com

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"What is the most practical way to compactlow–bulk density, flake-like particulate? Having designed and built a press to compactmaterials like this that exhibit the flow charac-

teristics of damp "corn flakes," I am painfully awareof the problem. It simply does not flow like any nor-mal metal powder or other common granular sub-stance. Trying to make a compact about the size ofa marshmallow with consistency could not beaccomplished with any type of feed shoe or hopper.

To get a compact of the required accurateweight, it was necessary to weigh out each chargeby hand and then load the charge into a feed ori-fice above the die. The charge was then "coaxed" inthe die so that it could be compacted.

I chose to deal with this question in the hopethat a reader might have found a solution andwould be willing to respond.

What does a detailed comparison of new,expensive, sophisticated presses with older,simpler, inexpensive, basic presses teach?Back in the 1950s and 1960s most powdermetallurgy (PM) presses were relatively simple

machines. Many were not originally designed forPM but for compacting medicine tablets, candy andeven Lydia Pinkham's Pills or briquettes of varioussubstances. These presses made "parts" from PMmaterials by compression in a shaped die. Many ofthese presses were single action, pressing fromonly one direction. Both fixed-die and floating-dieconfigurations existed, and many had manuallyoperated clutches and brakes. We had several KUXpresses that had no clutch and almost worthlessbrakes. Later, presses had the capability to pressmore than one level by multiple punches andplatens, floating dies, slide blocks, and variousother ingenious systems. Almost all the adjust-ments were made "by hand" and the parts were

affected by factors suchas press heat-up, pow-der flow, hopper level,feeder-shake consisten-cy (if any), and ambientconditions. “Feedback"of the output character-istics was accomplishedthrough the operator making measurements andthen corrections. Frequently, corrections weremade only after defective PM parts were identified.This scenario is still generally true today for thebasic presses. However, these basic presses filledthe need for relatively fast and inexpensive opera-tion and were satisfactory for producing simple PMparts—but probably not for parts demanding a lowdefect level, or where product liability concernswere high.

In general, these basic presses were easy to setup and could be run rapidly, with a top speedoften determined by the ability to get a reasonablyconsistent fill. The set up person would need sometraining but a high degree of technical skill wasnot essential. A factory could be set up with newor used presses at relatively low capital expense tomake a wide variety of PM parts. More complexparts could be made using innovative tooling sys-tems and adaptations. However, complete controlover the compacting process was difficult, particu-larly with multiple-level parts. Uniformity of densi-ty, elimination of powder-transfer shears, andcracking were frequent problems.

Over the years these problems have been (or arebeing) solved by utilizing presses that provide:

(a) More precise guidance systems.(b) More precise speed control.(c) More precise and controllable powder-feed

systems.(d) Feedback of pressures, weights, and meas-

Volume 43, Issue 4, 2007International Journal of Powder Metallurgy

CONSULTANTS’CORNER

11

*M.I. (Mike) Jaffe, Box 240, 144 Brewer Hill, Mill River, Massachusetts 01244-0240, USA; Phone: 413-229-3134, Fax: 413-229-3622; E-mail: [email protected]

QA

MYRON I. (MIKE) JAFFE*

QA

CONSULTANTS’ CORNER


urements.(e) Calculation of trends and setting of function

limits. (f) Automatic compensation for some variables.(g) Ability to control motion of punch levels to

achieve the most uniform compression pat-terns.

(h) Ability to monitor each part to eliminatedefective parts and/or to stop the process.

(i) Automated set-up procedures that can bearchived and recalled.

(j) Automated quality checking of compact byresonance, magnetic, electrical, optical, orother systems.

(k) Ability to monitor position of various levelswith extreme accuracy and feed this infor-mation back into the control loop.

(l) Controllable hydraulic or air cylinders inplace of springs.

I am sure that this list is not complete but all ofthese functions add significantly to the originalcost and maintenance of the press. They will per-mit the production of PM parts of the highest pos-sible quality with a minimum chance of error. Intoday's production atmosphere, many PM usersmay be hesitant to purchase any critical partsmade on older, simpler presses.

What is the environmental benefit to usinga nitrogen-based sintering atmosphere, asopposed to atmospheres based on the com-bustion of natural gas (i.e, endothermic)?First, let us look at the two methods. Endo isproduced by the reaction of a hydrocarbon gas

and air in a heated retort that contains a catalyst.As the mixture is too rich to burn, it consumesheat so an external source must be supplied(endothermic by definition). With natural gas in a2.5 to 1 air-to–natural gas volume ratio, the resultis about 40 v/o N2, 40 v/o H2 and 20 v/o CO, plustraces of CO2, H2O and CH4. This mixture needs tobe cooled rapidly to prevent reversal of the reac-tions. If the retort is heated by gas, the combus-tion gases enter the atmosphere somewhere. Thehydrogen going into the sintering furnace providesfor de-oxidization and the nitrogen is basically anonreactive carrier. The CO could be a problem ifthe non-combusted gas is allowed to vent or leakinto the surroundings or the atmosphere. However,with correct furnace operation the CO is burnedwith the hydrogen and air.

For the local environment (around the plant)

proper operation with tight equipment, correct air-gas ratios and gas flows, a clean catalyst, correcttemperatures, consistent gas chemistries, propercalibration of the instruments, and proper furnaceconditions should suffice. However, any variationin these factors could lead to improper results andpossibly some environmental problems, both localand in the atmosphere.

Nitrogen-based atmospheres have severaladvantages at the user level although it may bemore expensive than exo or endo. If the source iscryogenic nitrogen, it is simply a case of opening avalve to get the gas (assuming that it is properlyvaporized). If it is used with hydrogen this couldalso be simple if it is supplied as pressurized gas.If the hydrogen is from dissociated ammonia, it isstill a relatively simple process in which theammonia is passed through a catalyst heated to atleast 982°C (1,800°F). The nitrogen–hydrogenatmosphere is basically clean in the furnace. Itdeoxidizes the parts yielding some water vapor,and burns off in the vent stacks along with thelubricant vapors. Generally, for sintering, therewill be a provision in the furnace to allow thelubricants to burn.

Burning of the lubricants needs to be donewhether the atmosphere is nitrogen–hydrogen orendo. If lubricants are not burned completely theunburned lubricant vapors escape to the environ-ment as volatile organic compound (VOC) emis-sions. Some lubricant burning technologies ormethods are commercially practical to minimizethe VOC emissions. Note that some metal-basedstearates such as zinc stearate are severelyrestricted in some states as they produce zincoxide which is considered a hazardous waste.

From a domestic (North American) point of view,either can be reasonably friendly if properly con-trolled. The nitrogen–hydrogen atmosphere ismuch easier, as there is less to go wrong. Globally,I cannot comment on the relative environmentalimpact of the production of the hydrocarbon gases,nitrogen, hydrogen, or on the electricity due to thevarious methods and sources of electricity.

The response to this question incorporatedinput from Harb Nayar, TAT Technologies.

Q

A

Readers are invited to send in questions for futureissues. Submit your questions to: Consultants’Corner, APMI International, 105 College Road East,Princeton, NJ 08540-6692; Fax (609) 987-8523; E-mail: [email protected]

ijpm

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Team Profile

Brian OrgesManufacturing SpecialistT: 440.243.5151 Ext 226 | F: 440.243.4868Email:[email protected]

Location: Cleveland

7550 Lucerne Drive Suite 110

Cleveland, OH 44130

Barbara McElweeProject CoordinatorT: 440.243.5151 Ext 250 | F: 440.243.4868

Email:[email protected]


A prestigious lifetime award recognizing APMI International members for their significant contributions to the society and their high level of expertise in the science, technology, practice,or business of the PM industry

2007 FELLOW AWARDRECIPIENTS

The 2007 APMI Fellow Awards were presented at PowderMet2007 in Denver, Colorado.

Tom has distinguished himself as one of the fewrecognized experts in thefield of ferrous PM metallography throughoutthe world. With over 40years of dedicated service

to the PM industry, he has been instrumental in developing methods for sample preparation, characterization, and testing for both powders and PMcomponents. He has a unique talent for expressing metallographic interpretation to both experienced andinexperienced individuals, and has devoted his efforts to advance metallography to both the industrial and academic worlds. As Scientist, Research &Development, for Hoeganaes Corporation, Tom utilizedhis passion for metallography to organize and initiate theannual APMI PM Metallography Competition in 1992. Histalents have earned him a seat on the Board of Directorsof the International Metallographic Society, where he isactive as a judge for the IMS Metallography Contest. A member of APMI for over 16 years, he is an active member of the International Journal of PowderMetallurgy Editorial Review Committee, and has servedon the APMI Student Liaison Committee. Tom has beena mainstay of the MPIF Conference Program Committeesince 1990 and was a co-chair of PowderMet2007. He has authored or co-authored over 30 technical publications, and has participated as a co-chairmanand/or speaker at various MPIF seminars and shortcourses. Tom received the MPIF Distinguished Serviceto Powder Metallurgy Award in 2005.

INTERNATIONAL

Howard has made importantcontributions to PM and iswidely recognized for hisconsulting work in research,process & product development, design, manufacturing, and production. With over 35 years of APMI membership, hehas parlayed his strong metallurgical background (BSMetallurgical Engineering from Rensselaer PolytechnicInstitute and MS Metallurgical Engineering from theUniversity of Pennsylvania) with business savvy (MBAfrom Wright State University) to assist in technologytransfer through technical marketing, education/teaching,and many other technical industrial advancement programs. As president of Management & EngineeringTechnologies, he has authored or co-authored over 50publications, and contributed to over 225 technical articles and presentations. He is a past president of thePowder Metallurgy Parts Association, a current memberof the MPIF Technical Board, Chairman of the MPIFStandards Committee, Executive Director of the Centerfor Powder Metallurgy Technology, and currently theNorth American Program Leader of the Global PMProperty Database. A longtime member of the MPIFConference Program Committee, he was a co-chair ofthe 1985 MPIF Annual Powder Metallurgy Conferenceand the 2002 PM World Congress. Howard received theMPIF Distinguished Service to Powder Metallurgy Awardin 1995.

THOMAS F. MURPHY HOWARD I. SANDEROW

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The annual 2007 MPIFPowder Metallurgy DesignExcellence Awards competition featuredawards for outstandingpowder metallurgy (PM)parts used in diverse end-market segments—automotive, lawn & garden/off-highway, hardware/appliances, handtools/recreation, medical/dental, and industrialmotors/controls &hydraulics. PM replacedcompetitive parts-makingprocesses such as die casting, plastic injectionmolding, machining, stamping, laser welding,gear hobbing, and conventional forging. PM’sprecision, reliability andcost savings, as well as itsnet-shape and complexdesign benefits, are maximized in demandingapplications. The winningparts are outstanding examples of advances inconventional press & sinterPM processing, metal injection molding (MIM) andhot isostatic pressing (HIP).Sponsored by the MetalPowder IndustriesFederation (MPIF), the competition showcases PM’s cost savings, designbenefits, precision, and special properties that outperform competitivematerials and processes bya wide margin.

2007 PM DESIGN EXCELLENCE AWARDSCOMPETITION WINNERSPeter K. Johnson*

DESIGN EXCELLENCE AWARDS WINNERS

*Managing Editor, International Journal of Powder Metallurgy, APMI International, 105 College Road East, Princeton, New Jersey 08501-6692,USA; E-mail: [email protected]

GRAND PRIZE WINNERS The seven parts selected as the Grand Prize winners are shown in

Figure 1.

Presented atPowderMet2007 inDenver, Colorado.Figure 1. Grand Prize winners


STEEL CLUTCH HUB WINS AUTOMOTIVETRANSMISSION GRAND PRIZE

Stackpole Automotive Gear Division,Mississauga, Ontario, Canada, and its customerMagna Powertrain, New Process Gear Division,East Syracuse, New York, received the GrandPrize for a high-precision PM steel clutch hub,Figure 2. Stackpole selected a special low-costlean-alloy FeMnCrC PM material to meet strictdimensional control, compressibility, and durabil-ity requirements in a demanding environment.The complex six-level part operates in the clutch-ing system of an active four-wheel transfer case inlight trucks and SUVs. The clutching systemreplaces a manual synchronizer system, providingfull-time active control of torque transfer. It allowsvariable torque distribution to the vehicle’s frontwheels on the fly. High-temperature sintering at1,280°C (2,336°F) provides impressive properties:a minimum density of 7.0 g/cm3, 1,138 MPa(165,000 psi) tensile strength, yield strength of1,034 MPa (150,000 psi), and an apparent hard-ness of 35 HRC. The complex castellated geometryrequired innovative tooling in closed-loophydraulic compacting presses to precisely controllengths, diameters, densities, weight, and run-out, as well as an even density distributionthroughout the part. The tool set has three toolsacting as dies. The part is compacted close to anet shape with only 56 g (1.96 oz.) of material

removed from a 1.28 kg (2.82 lb.) sintered part.Annual production exceeds 600,000 parts.

FORWARD–REVERSE ACTUATOR ASSEMBLYWINS LAWN & GARDEN/OFF-HIGHWAY GRANDPRIZE

FMS Corporation, Minneapolis, Minnesota, andits customer Team Industries, Bagley, Minnesota,share the Grand Prize for an assembly of six net-shape precision PM parts that make up the for-ward–reverse actuator assembly, Figure 3, in golfcart transmissions. By changing the electricalswitch, the assembly actuates the transmissionlinkage to engage either forward or reverse gear-ing. The parts are made to a typical density of 6.9g/cm3. Most of the parts require heat-treatedproperties of 830 MPa (120,000 psi) tensilestrength, 760 MPa (110,000 psi) minimum yieldstrength, 300 MPa (43,000 psi) fatigue strength,and a typical hardness of 35 HRC. The movementover wires (MOW) tolerance on the gears is 0.058mm (0.0023 in.). While no machining is per-formed on the parts, secondary operationsinclude zinc plating and vacuum oil impregnation.Team Industries estimates that PM delivered a50% cost savings over the next most competitivefabrication process.

2007 PM DESIGN EXCELLENCE AWARDS COMPETITION WINNERS

Figure 2. PM steel clutch hub

Figure 3. Forward–reverse actuator assembly


FIRE PROTECTION LOCKING SYSTEM WINSHARDWARE/APPLIANCE GRAND PRIZE

Metal Powder Products—Anaheim, Anaheim,California, won the Grand Prize for a 316L stain-less steel secure cap cover, Figure 4, that is usedwith two other PM parts in a fire hydrant protec-tion locking system. The complex part, featuringlarge external tabs that are precisely oriented toan internal depressed wave form that allows it tomesh with two other PM parts, required five tool-ing levels. It weighs 1,920 g (4.2 lb.). Made to adensity of 6.5 g/cm3, the cap cover has a 138 MPa(20,000 psi) yield strength, a 55 HRB apparenthardness, and an as-sintered elongation exceeding20%. The customer subjects the part to a rigorousimpact-and-abuse test to prove its integrityagainst vandals. The three external lugs mustwithstand the impact of a 4.54 kg (10 lb.) sledgehammer and a torque loading of more than 227 kg(500 lb.) The main body must be resistant todrilling. The customer realized a greater than 80%reduction in comparable machining time by choos-ing PM over conventional machining.

TRIGGER GUARD WINS HANDTOOLS/RECREATION GRAND PRIZE

The Grand Prize goes to Megamet Solid MetalsInc., Earth City, Missouri, for a trigger guardmade by metal injection molding, Figure 5, forModern Muzzleloading, Inc., Knight Rifles,Decatur, Alabama. The metal injection molded(MIM) guard supports the trigger group and ham-mer in the “quick detachable trigger” mechanismin a 50 caliber muzzle-loading hunting rifle. Madeto a density of 7.4 g/cm3, the 88.6 g (3.1 oz.) low-alloy MIM steel part has an as-sintered tensilestrength of 650 MPa (94,250 psi) and 400 MPa(58,000 psi) yield strength. The part is held tocritical dimensions of ±0.12 mm (±0.005 in.).Megamet performs four secondary operations:reaming three holes, tapping two screw holes, anddeburring. The customer applies a black oxidesurface finish and drills one hole because of adesign change. Choosing the MIM process provid-ed substantial cost savings.


Figure 4. Fire hydrant secure cap cover

Figure 5. Trigger guard


ORTHODONTIC PARTS WIN MEDICAL/DENTALGRAND PRIZE

Flomet LLC, DeLand, Florida, and its customerOrmco Sybron Dental Specialties, Orange,California, won the Grand Prize for three parts—bracket, slide, and removable drop-in hook,Figure 6—used in the Damon 3MX self-ligationorthodontic tooth-positioning system. One bracketand one slide go on each tooth with the hook anoption for about five percent of the teeth. The tiny,intricate parts are made by metal injection mold-ing from 17-4 PH stainless steel powder to a den-sity of 7.5 g/cm3. They have impressive physicalproperties: a tensile strength of 1,186 MPa(172,000 psi) and yield strength of 1,090 MPa(158,000 psi). The slides and brackets are heattreated. There are 30 bracket part numbers, threeslide numbers and one hook design. All of theparts are made to a net shape. The customertumble polishes the parts and performs a brazingoperation before assembly. Flomet produces up to600,000 parts weekly.

PUMP ROTOR WINS INDUSTRIAL MOTORS/CONTROLS & HYDRAULICS GRAND PRIZE

Lovejoy Sintered Solutions LLC, DownersGrove, Ill inois, and its customerPetrotec–India/Portugal, Gujarat, India, won theGrand Prize for a complicated five-level pumprotor, Figure 7. The rotor functions in a hydraulicpump assembly that draws up petroleum fuelsfrom an in-ground tank to the above-ground noz-zle. It is used in conjunction with a PM idler gearand PM side pump cover. The rotor has nine legs,each 50 mm (1.97 in.) long and 10 mm (0.39 in.)wide, creating a five-to-one aspect ratio. The finalsintered density is approximately 7.1 g/cm3.Made from MPIF F-0005-25 PM material, the rotorhas a tensile strength of 228 MPa (33,000 psi), ayield strength of 190 MPa (27,550 psi), and a 56HRB apparent hardness. Lovejoy performs somemachining on the hub and cup. The customerestimates a 30% cost savings versus themachined casting used previously. In pre-qualifi-cation testing, six pumps were assembled withsample parts and run for six million cycles at1,000 RPM. After disassembly the PM rotorsshowed no wear.


Figure 6. Orthodontic bracket system parts

Figure 7. Pump rotor


DIPOLE CRYOMAGNET END COVER WINSGRAND PRIZE IN OTHER MARKET SEGMENTCATEGORY

A dipole cryomagnet end cover, Figure 8, fabri-cated by Bodycote HIP–Surahammar, in Sweden,for Metso Materials Technology Oy, Finland, fordelivery to the particle physics center of CERN(European Organization for Nuclear Research),Switzerland, won a Grand Prize. The end cover isused in the Large Hadron Collider, the world’slargest and highest-energy sub-atomic particleaccelerator, which consists of over 34 km (21 mi.)of tunnels and caverns, built more than 100 m(328 ft.) underground, that will enable scientiststo study and understand the structure of matterand the forces that hold it together.

Made from 316LN stainless steel powder, thepart is hot isostatically pressed to full density.Bodycote reports that the powder resulted fromconsiderable development work by the metal pow-der supplier. The powder maker modified themelting and atomization processes to minimizethe formation of oxide inclusions to meet strin-gent impact and toughness requirements. Thesuperconducting dipole cryomagnets operate in acryogenic environment at -268°C (-450°F). AsHIPed to a near -net shape weighing 115 kg (253 lb.), the finished end cover weighs 69.5 kg(153 lb.). The nominal bulk dimensions are 580 mm (23 in.) dia. × 230 mm (9 in.) height.

Bodycote incorporated finite element analysis,computer-aided design, numerically controlledsheet metal–cutting technology and cutting-edgerobotic welding and part manipulation to producethe end covers. This resulted in a more than 50times increase over the typical production rate offully dense HIPed PM near -net shapes, anunprecedented breakthrough in HIPing productiv-

ity. About 2,700 end covers have been delivered toCERN. The design of the part features severalcomplex configurations. For example, both theinner and outer surfaces of the broad face areradiused with the inner surface approximatelyparallel to the outer surface. The exterior of thecurved surface has either 8 or 10 projections,depending upon which version of the part is pro-duced. The design differs slightly depending onwhich side of the dipole magnet it is located. ThePM HIPed part meets the equivalent mechanicalproperties of 316LN wrought stainless steel,including internal toughness and high ductility. Ithas a yield strength of 334 MPa (48,430 psi) atroom temperature and 1,118 MPa (162,100 psi) at-267°C (-450°F), and a tensile strength of 664MPa (96,280 psi) at room temperature and 1,768MPa (254,910 psi) at -268°C (-450°F). The cus-tomer performed a post-HIP heat treatment:1,050°C annealing (1,922°F), water quenching,and machining.


Figure 8. Cryomagnet end cover


AWARD OF DISTINCTION WINNERS Seven parts were selected for an Award of

Distinction, Figure 9.Capstan Atlantic, Wrentham, Massachusetts,

won the Award of Distinction in the AutomotiveTransmission category for an assembly of twoparts, called the sprocket assembly–drive andsprocket–driven, Figure 10, used in an SUV trans-fer case. The three-level sprocket has a precision-machined tooth radius, hub diameter, andtapered inside diameter, as well as a precise invo-lute profile to facilitate a smooth chain roll-off inoperation. Made from a modified MPIF FL-4405PM material, the parts feature a final single-pressed density of 7.4 g/cm3, a tensile strengthexceeding 1,379 MPa (200,000 psi), an apparenthardness of 45 HRC, and a microindentationhardness of 60 HRC. The sprockets are carbo-nitrided for tooth-wear resistance.

Burgess-Norton Manufacturing Co., Geneva,Illinois, won an Award of Distinction in the Lawn& Garden/Off-Highway category for two actuatorarms, Figure 11—right-hand and left-hand—usedin a zero–turning radius control system for high-end commercial and residential riding lawnmow-ers. The innovative PM arms provided close to a40% cost savings, replacing two six-piece assem-blies, eliminating 12 parts and related labor andassembly costs. The former assembly consisted ofa weldment, a wire-form part, two stampings, ashoulder bolt, and attaching hardware. The PMlever arms incorporate a bevel gear and stop luginto a lever that controls a hydraulic system.

Made from MPIF FC 0208-50 material, the actua-tor arms have a density of 6.7 g/cm3, a tensilestrength of 345 MPa (50,000 psi), and a hardnessrange of 75–100 HRB, providing good wear prop-erties. Each part weighs 658 g (1.44 lb.). Morethan 200,000 of the parts are produced annually.

NetShape Technologies, Inc., Campbellsburg,


Figure 9. Award of Distinction winners

Figure 11. Actuator armsFigure 10. Sprocket assembly


Indiana, captured the other Award of Distinctionin the category for a new differential carrier gear,Figure 12, made for Ariens Company, Brillion,Wisconsin. Made from MPIF material FX-1008-50,the part is used in a transmission for the Ariensprofessional Snothro line of 8.5 horsepower-and-higher snow blowers. The new design improved thedrive torque output of the unit by speeding up thepinion and increasing the ratio after the frictiondisc in the transmission. The gear enables remotelocking and unlocking of the differential. Formedas a net shape to a density of 6.8 g/cm3, the com-plex five-level part has a minimum tensile strengthof 520 MPa (75,000 psi), a transverse rupturestrength of 900 MPa (130,000 psi), a yield strengthof 620 MPa (90,000 psi), and a fatigue limit of 234MPa (34,000 psi). Quenching and tempering is theonly secondary operation performed on the part.

SSI Technologies, Inc., Janesville, Wisconsin,won the Award of Distinction in the Hardware/Appliances category for PM and MIM parts used intactical hinge-style handcuffs, Figure 13, made byASP, Inc., Appleton, Wisconsin, a law enforcementproducts supplier. The handcuffs use 14 PM parts,of which five are different designs—a lock pawl,bow, side and center links, and main links. Twelveparts are made from three stainless steel materialsand two parts are made from MPIF FD-0405-60steel. The four main links are made by metal injec-tion molding to a minimum density of 7.5 g/cm3

and have a tensile strength of 540 MPa (78,000

psi). The other parts are processed by convention-al or high-temperature sintering. The bow has atensile strength of 710 MPa (103,000 psi), and hasa large 2.29 mm (0.090 in.) radius in the areasthat touch the wearer’s wrist. These radii had beenmachined in the previous design. Three modified316 stainless steel parts and two duplex stainlesssteel MIM parts make up the linkage assembly. Aproprietary and patent-pending design allows theassembly to be swaged together without using riv-ets. The stainless steel parts meet stringent gov-ernment corrosion resistance requirements.

PMG Holding, S.A., Mamer, Luxembourg, wonthe Award of Distinction in the Hand Tools/Recreation category for a stainless steel camshaftpulley, Figure 14, made for Yamaha Marine Co.,Ltd., in Japan. The pulley operates in the timingcontrol for a 4-stroke 115 hp outboard motor. Withan outer diameter of 110 mm (4.33 in.), it is con-sidered large for PM stainless steel. It is made to adensity of 6.7 g/cm3 and has a tensile strength of296 MPa (42,920 psi) and yield strength of 151MPa (21,895 psi). Successfully producing the largepulley required a special powder-mixing techniqueof first coating the particles with a liquid binder,followed by the addition of a substantial amount ofa special lubricant. These additives were complete-ly removed by precisely controlled vacuum dewax-ing. Machining the inner diameter counterbore isthe only secondary operation.

Kinetics, a Climax Engineered MaterialsCompany, Wilsonville, Oregon, has earned the


Figure 13. Tactical hinge-style handcuff componentsFigure 12. Differential carrier gear


Medical/Dental Award of Distinction for a 316Lstainless steel MIM pin shroud, Figure 15, madefor ArthroCare Corporation, San Juan Capistrano,California. The critical part is used in the compa-ny’s Opus Magnum Knotless Implant device forarthroscopic surgical repair of torn rotator cuffs.The implant device secures a sutured tendon tothe shoulder bone. The pin shroud is implantedinto a patient and is critical to the functioning ofthe rotator cuff surgical procedure. Made close tonet shape, the MIM pin has a typical density of7.85 g/cm3, a tensile strength of 538 MPa (78,000psi), and yield strength of 200 MPa (29,000 psi),and typical apparent hardness of 69.4 HRB. MIMreplaced an assembly made by wire-EDMing threeparts and assembling them to each other by laserwelding. Choosing the single MIM parts reducedthe customer’s final assembly time by two-thirds,from 15 min to just 5 min per unit.

The final Award of Distinction, in the IndustrialMotors/Controls & Hydraulics category, was cap-tured by Webster -Hoff Corporation, GlendaleHeights, Illinois, and its customer, NorgrenAutomotive Inc., Mt. Clemens, Michigan, for a PMaluminum lever block, Figure 16. The part is usedin a quick-change vacuum cup system that han-dles parts and/or materials. Made to a density of2.45 g/cm3, the multi-level shape has a tensilestrength of 110 MPa (16,000 psi) and yield strengthof 48 MPa (7,000 psi). The 3.05 mm (0.120 in.) thin

center section of the part produces a weak spot inthe green state, requiring robotic removal andtransfer to the sintering furnace. The 2.41 mm(0.095 in.) center inside dia. makes the center corerod vulnerable to breaking during sizing of thepart. Additional secondary operations includevibratory deburring and staking the center hole.

The awards were presented during thePowderMet2007 International Conference on PowderMetallurgy & Particulate Materials held in Denver,May 13–16, sponsored by MPIF and APMI Inter-national. Past winners of the MPIF International PMDesign Excellence Awards Competition can beviewed by visiting www.mpif.org.


Figure 15. MIM pin shroud

Figure 16. Lever block

Figure 14. Stainless steel camshaft pulley

ijpm

This global PM event is sponsored by:

METAL POWDER INDUSTRIES FEDERATIONAPMI INTERNATIONAL105 College Road EastPrinceton, New Jersey 08540 USATel: 609-452-7700Fax: 609-987-8523www.mpif.org

INTERNATIONAL

In cooperation with:

2008 World Congress on Powder Metallurgy & Particulate MaterialsJune 8–12, Washington, D.C.

NEXT JUNE THE PM WORLD CONVENES IN WASHINGTON, D.C.

GAYLORD NATIONAL RESORT & CONVENTION CENTERNational Harbor on the Potomac

• International Technical Program

• Worldwide Trade Exhibition• Special Events


The new European lawtitled Registration,Evaluation, andAuthorization of Chemicals(REACH) is designed tomake manufacturers andimporters register thedetails of chemicals (including metals andalloys) in a newly formedcentral European database.Impetus for the regulationstems from ever-increasingconcerns for the protectionof human health and theenvironment. This articletraces the genesis ofREACH, attendant legal and technical issues, implications for PM inEurope, and for importers ofpowders and PM parts. In aglobal economy, the NorthAmerican PM industryshould be fully cognizant ofREACH.

THE NEW EUROPEANREACH REGULATION: A MAJOR CHALLENGE TOMANUFACTURERS ANDIMPORTERSPeter Brewin*

HEALTH & ENVIRONMENT

*Former Technical Director, European Powder Metallurgy Association, www.epma.com; E-mail: [email protected]

INTRODUCTIONThe REACH Regulation1 (Box 1) completed the legislative process in

Brussels in December 2006 and entered into force (EIF) in all memberstates on June 1, 2007. The immediate effect will be to place a largebureaucratic burden on manufacturers and importers (M/I) of chemi-cal substances based in Europe in assembling the RegistrationDossiers which are the heart of the regulation. Irrespective of whethera chemical substance has proved a problem in the past, these dossiersmust demonstrate that its intrinsic hazards have been quantified andmeasures proposed to control risks of human and environmental expo-sure appropriate to each identified use right down the supply chain,including disposal.

Different deadlines are set depending on tonnage; the registrationdossier for most bulk metals will have to be completed by December2010. After the different deadlines it will be illegal for unregistered sup-pliers to place chemical substances on the market. This will have impor-tant implications for company purchasing policies. Additionally usersof chemical substances share legal responsibilities for correct riskmanagement under the Duty of Care provisions of the regulation.

A key element of REACH is the legislative treatment of chemicalsknown to be highly dangerous. In its full effect REACH is intended toeliminate these from Europe. In the interim, continued use of these

REACH stands for the Registration, Evaluation and Authorization of CHemicals. It is anew European law designed to make companies register the details of chemicals in anewly formed central European database. It affects any Europe-based organization whichproduces, trades, processes, or consumes any chemical "substance" including metalsand alloys. Under REACH it is up to manufacturers and importers (M/I) to prove that theirproducts are safe at all stages of processing and use by downstream users down thecomplete lifecycle. Further details of the legislation can be downloaded from the followingWeb site: http://ec.europa.eu/environment/chemicals/reach/reach_intro.htm.

BOX 1: WHAT IS REACH?


chemicals will be subject to an authorizationprocess to minimize risks to humans or the envi-ronment. Metals which are proven or suspecthuman carcinogens are liable to authorization.

The regulation consists of 141 articles. Criticalto the scope and effect are the definitions, some ofwhich are given in Box 2.

BACKGROUNDMany European laws are “directives” translated

into local laws and enforced at the level of the indi-vidual member states. In contrast, REACH will bea European “regulation” for which there will be nolatitude for local interpretation. Implementationwill be by competent authorities at the memberstate level. Some of these are already threateningto refuse operating permits if manufacturers fail tosatisfy REACH requirements.

REACH arose as a result of several factors:• previous legislation on the control of haz-

ardous chemicals had not worked (littleincentive to test for effects on human healthor the environment)

• pressure from retail consortia to counter thethreats of consumer litigation

• public perception that industry puts profitsahead of social conscience

• a desire for greater transparency and publicopenness on data on the hazards of man-made organic chemicals

• European manufacturing industries underes-timated the power of the "green" lobbies

The Precautionary Principle underlies REACH(Article 1):

• if there is uncertainty, maximum danger isassumed

• authorization of substances of high concernirrespective of risk-management measuresproposed

• restriction of substances of high concern if ittakes too long to supply data

• no data, no market (Article 5)Intensive lobbying was carried out by the met-

als and other industries in the months leading upto the final Brussels vote in December 2006, withthe aim of rectifying some of the anomalies of thedraft produced in June 2006 by the commissiontechnocrats. This lobbying was made considerablymore difficult by the need to explain technicalissues to non-technical members of the Europeanparliament. The battle to make substitution ofhigh-danger substances advisable but not manda-tory was lost, as was the attempt to exclude sec-ondary raw materials. However, it was agreed thatores and concentrates should be exempt. Mostother metal-specific issues were ignored.

LEGAL AND TECHNICAL ASPECTSRegistration:

All M/Is intending to register have to inform theREACH authorities before December 2008 ("Pre-Registration"); this will be without charge. Afterthat date it will be illegal for an M/I to place asubstance on the market without first having pre-registered. In order to preserve continuity of sup-ply, their customers—the downstream users—willbe advised to ensure that their key suppliers havepre-registered as required. Lists of pre-registrantswill then be published, and are intended to helpthe formation of SIEFs for exchange of data.

REACH requires M/Is of chemical substancesto demonstrate to the new REACH agency thattheir products are safe down the complete supplychain. This requires the production of dossiersincluding full assessment of risks for each identi-fied use including data on exposures and compar-isons with stated known safe limits, andmeasures to manage any risks. The level of detailrequired for a chemical substance depends on thetonnage placed on the market and on its hazardclassification. The prime responsibility for thisdossier is with the original producer of the chemi-cal—in the case of metals typically the smelter orrefiner, or importer for metals produced outside

THE NEW EUROPEAN REACH REGULATION: A MAJOR CHALLENGE TO MANUFACTURERS AND IMPORTERS

Alloy: Under REACH an alloy is treated as a "preparation" of its constituents; it is therefore not a substance. For calculation of exposurean alloy can be treated as a "special" preparationArticle: "An object which during production is given a special shape, surface or design which determines its function to a greater degree thandoes its chemical composition"Downstream User: Uses substance in EuropeIdentified Use: Use of a substance on its own or in a preparation that isintended by an actor in the supply chainImporter: Imports substance produced outside Europe; a Europe-basedlegal entity who signs the customs declaration formManufacturer: Refines and produces a substance in EuropePreparation: A mixture of two or more chemical substancesSIEF: Substance Information Exchange ForumSubstance: Element (e.g., Fe) or stoichiometric chemical compound (e.g., MnS, WC)

BOX 2: Some REACH Definitions (for full definitions see Article 3 of theREACH Regulation)


the European Union (EU). However, they will relyon customers and their users to supply informa-tion on uses, exposure for each use, and approvalfor risk-management measures to be proposed inthe registration dossier. Downstream users willnot be permitted to process substances for useswhich have not been identified in the RegistrationDossier

Downstream users that have uses which theywish to keep confidential from their suppliers maywithhold the information, but must provide a fullchemical safety assessment of this use to theauthorities.

The authorities expect M/Is of the same chemi-cal to share and generate data (e.g., through con-sortia or SIEFs). Target dates for the submission ofthe dossiers depend on tonnages placed on themarket, except that known hazards have to be reg-istered first, irrespective of tonnage (Box 3). Thecore of the dossier are data on exposure. In thepast this has proved to be the most difficult andthe most time consuming to complete. It includes:

• historical data on emissions to air, water, andsoil (local factory, local region, state)

• data to be related to each use down the com-plete supply chain including disposal

• data to differentiate between exposure andabsorption (failure to provide this will resultin the use of 100% as a default absorptionfactor)

Finished articles placed on the market areexempt from REACH, unless hazardous chemicalsare released to humans or the environment dur-ing normal handling and use. Certain chemicalsare exempt from REACH, either because they arenaturally occurring, or because they are judged tobe controlled adequately by other legislation.

Authorization—Adequate Control andEventual Replacement

In REACH chemical substances classified ashighly dangerous to human health or the environ-ment are covered by a separate authorizationprocess. Irrespective of tonnage these have to reg-ister within 3.5 years of EIF.

In the first instance all such chemicals will beplaced on published lists (the public candidaturelist). From this list about 25 chemicals per year willbe selected for detailed investigation by the author-ities depending upon intrinsic hazard and risk ofexposure. This list may include some metals.

M/Is wishing to obtain consent for the contin-


BOX 3: Registration TimescalesEntry into Force (EIF) = June 1, 2007

CMR 1, 2 = Carcinogenic, Mutagenic, or Reproductive Hazards 1 or 2. tpa = annual tonnage*R50/53 = very toxic to aquatic organisms, may cause long-term adverse effects to the environment


ued use of such chemicals may be required tosubmit a dossier separate from the RegistrationDossier. Irrespective of tonnage these authoriza-tion dossiers could be required to be completedwithin 42 months of REACH coming into force,and should contain:

• analysis of non-hazardous substitutes or anR&D plan for product re-design if no safesubstitutes exist

• socio-economics of risk management of con-tinued use

It is possible that authorization will only begiven for certain uses and for limited time periods,after which the authorities will expect non-haz-ardous substitutes to have been developed.

IMPLICATIONS FOR EUROPEAN PMREACH has been drafted by lawyers with the

control of liquid organic chemicals primarily inmind. Hence several of the definitions in Article 3are difficult to interpret for metals (e.g., alloy, arti-cle, identified use, importer, preparation).Additionally, complications arise from the treat-ment of scrap, polymers in oils, waxes, and lubri-cants, and companies that decide to M/I chemicalsubstances after the registration deadlines forsound commercial reasons.

Companies that have taken out accreditationunder ISO 14000 and 18000 will find the datacollection and feedback procedures highly rele-vant to REACH.

In the context of PM, other important issuesinclude:

Pre-Registration:It is now clear that this is of first importance,

since chemical substances that are not pre-regis-tered by the deadline will no longer be available toEuropean manufacturers.

Comment: Manufacturers of powders and sin-tered parts based in Europe should carry out a fullinventory of all metals and chemicals purchased,and should contact their suppliers, to ensure thatthe constituent chemical substances will be pre-registered.

Importer or Downstream User:European parts makers who currently import

chemical substances faced with the requirementto undertake full registration may decide to con-vert to downstream user status by discontinuingimport in favor of local supply.


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Consortia Formation:Although, for antitrust reasons, the EU legisla-

tors decided to withdraw the consortia concept inthe final form of the regulation, M/Is of the samesubstance are encouraged to cooperate to mini-mize duplication of effort and legislative time.There is currently no obvious mechanism for anM/I to find out which consortia are being formed,or contact details. However, the Brussels lobbyingorganization Eurometaux (www.eurometaux.org)has the intention of starting a "REACH Gateway."

Comment: Trade associations will be key initialcontacts here.

Identified Uses:Chemical substances display different risks

according to use. For example, a preservative canbe safe to humans when painted on with a brush,but lethal if applied by aerosol without respira-tors. In this respect it will be important to differ-entiate the risks posed by sieve-size powders(20–250 µm) from those posed by sub-sieve-sizepowders (such as metal injection molding (MIM)powders).

Comment: It will be important to identify a fewgeneric uses for PM, bearing in mind the dangerthat the most precautionary approach (worst case)will be taken by the legislators in developing risk-management methods.

Exposure:By their intrinsic nature, liquids are "bioavail-

able" in that they can readily be taken up in thehuman body (skin, eyes, inhalation, mouth) orenvironment (soil, air, water). In contrast, thebioavailability of solids depends on release rate(surface area, surface chemistry, etc.).

Comment: The OECD2 Transformation andDissolution Protocol and derivatives will be usefulhere.

Hardmetals Industry:A survey of EPMA members in 2005 revealed,

among other things, a multiplicity of substancesinvolved in the manufacture of hardmetals (TiC,TiN, TaC, NbC, etc.). All these will be required toregister.

Comment: This will be a high priority for thehardmetals industries.

Metal Injection Molding:On MIM feedstock, component manufacturers

will need to ensure that both the constituent pow-ders and their binders are fully identified and pre-registered. The fine powder particle sizes inherentto MIM present potential risks of inhalation aswell as enhanced bioavailability (high specific sur-face). Data on aerodynamics and dissolution ratesmay be required, as well as data on safe operatinglimits.

Secondary Raw Materials:Scrap (such as recycled defective components)

that is not defined as waste is treated as a down-stream use and must be included in the registra-tion packages for its constituent chemicalsubstances.

Treatment of Alloys:REACH treats dangerous substances from two

aspects. The hazard of a substance is regarded asan intrinsic property of that substance (equivalentto specific gravity, boiling point, for example), andtherefore a substance is classified purely on thebasis of its chemical name. The risk the sub-stance poses to humans or the environment, how-ever, takes into account exposure routes andlevels. In shorthand:

Risk = Hazard × Exposure (1)

For classification purposes alloys are treated aspreparations. Under European legislation, if apreparation contains more than 1 w/o of a dan-gerous substance, it is classified as if it contains100% of that substance. If it contains over 0.1w/o of a highly dangerous substance, it is classi-fied as if it contains 100 w/o of that substance.

In the final version of REACH the metals indus-tries obtained a concession in that alloys aretreated as "special" preparations. By this the leg-islation recognizes that in establishing the risksfor each use, the fact that in an alloy a dangeroussubstance could be in solid solution in a "safe"matrix could greatly reduce its bioavailability andtherefore its exposure. The objective on alloys,therefore, will be to demonstrate this by bioavail-ability or equivalent test data using methods thatreplicate the worst case in each identified use.

IMPLICATIONS FOR IMPORTERS OF POWDERSAND PM PARTS

Under REACH, Europe-based manufacturerscurrently importing preparations (such as powderpremixes) will have to pre-register the constituent



substances. Depending on tonnage they will thenhave to register and supply the full technicaldossier.

Manufacturers of powders based outsideEurope will need to discuss with the importer howbest to supply the information for registration.

As articles are exempt from REACH, manufac-turers of sintered parts based outside Europe willbe allowed to continue to import these withoutundergoing registration. The possible exceptionhere is sintered parts which emit dangerous sub-stances during normal handling and use. Thusoil-filled bearing and brake pads may need todemonstrate that substances emitted (oils, copperparticles) are safe.

CONCLUSIONSIt is clear that REACH will be a major but

unavoidable burden for European M/Is at a timewhen (a) cost pressures (energy, raw materials)and global competition are squeezing profit mar-gins to the limits, and (b) the metals industrieshave long ago established risk-managementmeasures to protect human health and the envi-ronment. The fact that such legislation has comeinto law demonstrates the danger that industryfaces in ignoring the political process for too long,and in failing to publicize its safety record.

Conforming to the requirements of REACH willnot be easy, especially for smaller organizations.Each M/I needs to appoint a REACH specialistwithout delay, whose first task should be to carryout an audit of all chemicals and metals pur-chased to ensure continuity of supply against theunrealistically tight deadlines of the higher-ton-nage substances.

While many consultancy organizations willundoubtedly offer expensive training workshops,the availability of personalized help will beextremely limited. Trade associations (such as theEPMA) will have a vital role to play in helpingmembers to prepare, to facilitate cooperation, andto minimize duplication.

REFERENCES1. Regulation (EC) No. 1907/2006 of the European

Parliament and of the Council of 18, December 2006.2. Organisation for Economic Cooperation and Development.


ijpm

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While the powder metallurgy(PM) industry’s growth mayhave leveled off during thepast few years, our futureremains very positive. Newtechnologies, improved PMmaterial properties andinnovative processing areopening up new applicationsfor growth. The world hastapped PM as an importantglobal technology.

STATE OF THE PMINDUSTRY IN NORTHAMERICA—2007Edul M. Daver* and C. James Trombino, CAE**

ENGINEERING &TECHNOLOGY

*President, MPIF and President and CEO, ACuPowder International, LLC, 901 Lehigh Avenue, Union, New Jersey 07083-7632, USA, **ExecutiveDirector/CEO, Metal Powder Industries Federation, 105 College Road East, Princeton, New Jersey 08540-6692, USA; E-mail: [email protected]

Figure 1. North American iron powder shipments. 1 mt = 1.102 st

First, a review of metal powder shipments within North America forlast year and for the first quarter of 2007.

2006 iron powder shipments declined about five percent to 378,396mt (416,828 st), Figure 1. The PM share of this amount also declinedabout 5 percent, to 342,244 mt (377,004 st). Astute industry observersattribute this decline to the North American Big 3 automakers’ steadyloss of market share to transplants and the shift in product mix awayfrom SUVs and light trucks to passenger cars and the popularcrossover vehicles.

Shipments of copper and copper-base powders declined 9.4 percentin 2006 to 19,780 mt (21,789 st), Figure 2. The PM share of thisamount dropped 6.4 percent to 16,547 mt (18,228 st). These declinescan be attributed to the previously cited reasons, in addition to lossesof the domestic bearing business to manufacturers in Southeast Asia,and the very high price of commodity copper, which exceeded $8.8/kg($4.00/lb.) last year.

The unabated rises in commodity prices, especially copper and nick-el, have begun to force a substitution trend. For example, some stain-less steel users are switching to lower-nickel 304 stainless or movinginto non-nickel-containing stainless steels. Similarly, fabricators ofbronze bearings are lowering the copper content in PM bearings by

Presented atPowderMet2007 inDenver, Colorado.


utilizing diluted bronze bearings or iron–graphitebearings. Observers expect the prices of nickeland copper to stay high, at least through 2008when new mining capacity is targeted to hit themarket.

Tin powder shipments declined slightly to 885mt (975 st) but, once again, prices rose steadilythrough the year due to production disruptions inIndonesia.

Stainless steel powder shipments rose by anestimated 5 percent to 9,246 mt (10,185 st).

Nickel powder imports into the United Statesrose about 11 percent to an estimated 9,078 mt(10,000 st).

The domestic aluminum powder market is esti-mated at about 45,390 mt (50,000 st).

The tungsten and tungsten carbide markets areestimated at 4,085 mt (4,500 st) and 5,900 mt(6,500 st), respectively. Tungsten and molybde-num prices also increased appreciably.

Despite the challenges of coping with spiralingcommodity prices, PM as a net-shape or near-net-shape technology has an important story to tell.The PM process saves raw materials by eliminat-ing or reducing costly scrap, a fact that should beturned into a marketing advantage. But have we,as an industry, promoted this benefit sufficiently?

Equipment makers rebounded somewhat in2006 with compacting press shipments up 27percent to more than $19 million. However, presssales are still way off from historic highs duringthe 1998 through 2000 timeframe. Conventionalsintering furnace makers reported weak sales lastyear; overcapacity among parts makers as well asa large inventory of used equipment have beencited as reasons that overshadow the equipmentmarket.

The metal injection molding market is a brightspot, enjoying a consistent double-digit growth

rate. The Metal Injection Molding Association(MIMA) estimates the 2006 international MIMmarket at $435 million, according to the followingsales breakdown: Europe—$130 million, Asia—$130 million, and North America—$175 million.Some observers claim the global market is muchhigher, approaching $1 billion in sales. MIMA’stop growth markets for 2007 are medical, auto-motive, and electronic. Another source puts the2007 worldwide MIM market at over 4,085 mt(4,500 st) of metal powder, excluding hard metals.

We entered 2007 facing a somewhat negativeeconomic outlook, mostly related to automotiveproduction cuts spilling over from a soft fourthquarter of 2006. However, iron powder shipmentsfor the first quarter of this year have increased by3.9 percent to 98,307 mt (108,291 st), while cop-per has declined again, impacted by the steadilyrising price of commodity copper. At best, theNorth American iron powder market will end upflat or increase by two to three percent in 2007.

However, we need to note that the numbers col-lected and reported by MPIF are strictly for NorthAmerica, that is, the U.S., Canada, and Mexico. Intoday’s global economic environment many NorthAmerican companies have started operationsabroad. Powders and some PM parts are beingshipped to these and other independent compa-nies. As such, some or all of the decrease in ship-ments in North America is perhaps being made upby shipments abroad. So, for MPIF’s numbers tobe more meaningful in today’s global businessenvironment, we should be collecting and report-ing total shipments, rather than just for NorthAmerica.

Now a consideration of other PM issues.Although the acquisition trend has ebbed duringthe last few years, consolidations are still takingplace. Three companies were acquired in 2006,

STATE OF THE PM INDUSTRY IN NORTH AMERICA—2007

Figure 2. North American shipments of copper and copper-base powders.1 mt = 1.102st


down from six acquisitions in 2005. And duringthe first quarter of this year, three more compa-nies have been acquired, bringing the total ofacquisitions since 1990 to 124. It is distinctlypossible that more will be announced in themonths ahead.

The outlook for PM parts makers is mixed. Non-automotive niche product companies seem to bedoing well when delivering higher-density andhigher-performance parts. On the other hand,companies focused on the automotive market mayor may not be holding their own, depending onwhether or not they are making parts for so-called“hot” platforms. Without a doubt, the vehicleproduct mix is changing drastically away fromlarge SUVs and light trucks to passenger cars andcrossover models, adversely affecting PM partsmakers. A substantial cut in vehicle productionalso has a negative impact on PM parts makers,who share their pain with other North AmericanOEM parts suppliers. With North American auto-motive production forecast to stay flat at about15.3 million light vehicles, perhaps 2007 could belabeled a “bottom out” year for the PM automotivemarket..

The Big 3 (or the Detroit 3, as Automotive Newshas taken to labeling them), are no longer trulythe Big 3, based on Toyota’s dynamic growth. TheDetroit 3’s first-quarter market share dipped 3.7percent from their 2006 level to 52.1 percent.

Because of production cuts and shifts in OEMmarket shares, the average content of PM parts inNorth American vehicles will experience its firstdecline in decades, dipping 2 to 3 percent toslightly below 19.5 kg (43 lb.) in the 2007 modelyear.

Depending upon who you talk with, there issome good news, though. New program launches,such as the Ford Edge, are going very well. OnePM automotive supplier claims they cannot makeparts fast enough for this model. And the new2008 Cadillac CTS and STS sedans, both hot-sell-ing models, will use the new 300-horsepower 3.6liter V6 engine with variable valve timing (VVT)and direct fuel injection (DI). The new DI versionof the engine, which is about to debut, containsan estimated 14.5 kg (32 lb.) of PM parts.

To survive and grow in the turbulent automo-tive market, the North American PM industrymust sell its benefits more aggressively to thetransplant OEMs. Contributing to this endeavor,the MPIF Technical Board is conducting an ambi-

tious project to identify every known automotivepart that is being manufactured by our industry.With this information we can better promote PM’sadvantages for new automotive applications, aswell as provide examples for conversions. We canthen also promote PM automotive usage by num-ber of parts and applications, as opposed to onlyby weight per vehicle.

We must also think more globally and become aserious player in the worldwide marketplace. ThePM parts market in China, Korea, and India isenjoying double-digit annual growth rates. Manyof the major international OEMs have establishedproduction and procurement sites in these coun-tries. For example, GM CEO Rick Wagoner report-ed in a New York Times interview in New Delhithat GM planned to create a local base in India. Hesaid GM planned to take advantage of India’s high-quality, low-cost supply base to source more partsthere, which could mean buying up to $1 billionworth of automotive parts annually in India.

MPIF learned first-hand about the growing PMindustry in India during its recent successfultrade mission there. The Indian PM parts industryis growing at more than 15 percent annually.Currently the average PM parts content in pas-senger cars made in India is an estimated 5.5 to6.6 kg (12.1 to 14.5 lb.). This signals a significantgrowth potential for additional applications.

The automotive components industry is project-ed to sustain a 17 percent compound annualgrowth through 2014. Automotive production isgrowing at 15 to 20 percent annually. TataMotors, India’s largest automaker, forecasts build-ing 2 million vehicles annually by 2010. Thesedizzying statistics spell opportunities for theNorth American PM industry. Should we beginbuilding technical and business bridges to India,projected to be world’s third largest economy by2020? The answer is definitely “yes.”

Other areas of the world are also experiencingexciting growth. PM parts production in China isgrowing at least 10 to 15 percent annually.Officials from Chinese associations report that thePM parts market in China ranges from 78,070 mt(86,000 st) to over 90,780 mt (100,000 st) a year.The typical passenger car built in China containsabout 4.54 kg (10 lb.) of PM parts. And while onlya handful of companies there are capable of mak-ing parts of world-class quality, it is a given thatChina will catch up to the West sooner ratherthan later.



Korea is still another growing PM country witha PM parts market exceeding 45,390 mt (50,000st). The average weight of PM parts in a Korean-built vehicle is 8.0 kg (17.6 lb.).

While North America remains, by far, thelargest single market for iron powder shipments,at 378,400 mt (416,828 st), Japan and Europeare not far behind at 224,200 mt (246,968 st) and161,700 mt (196,241 st), respectively. The rest ofAsia and other regions of the world could easilyaccount for another 249,600 mt (275,000 st),which puts the estimated global iron powder mar-ket at about 1.03 million mt (1.135 million st).

Our industry must take on a more global per-spective to survive and grow in the 21st century.Following customers overseas with greenfieldplants or establishing joint ventures is a viablestrategy that must be reviewed continually.Another strategy is to maintain technologicalleadership through investment in innovative tech-nologies to improve the properties of PM parts andproducts.

Metal powder makers have been hard at workdeveloping new high-density steels and processesto achieve a density of 7.5 g/cm3 by single pressingand sintering. Achieving densities of 7.5 g/cm3 andabove will certainly open up new markets, with PMgears and sprockets for automotive transmissionsbeing but two such potential applications.

Diffusion-alloyed master alloys that provide per-formance and stability benefits, while containingless nickel, molybdenum and copper, have beenintroduced along with prealloyed chromiumgrades. Taking advantage of chromium’s lower andmore-stable cost, these grades can provide bend-ing-fatigue strengths exceeding 297 MPa (43,000psi) with conventional sintering. Leaner and lower-priced alloys are being developed for sinter hard-ening. New premixes are being offered to providevery close apparent density and dimensional sta-bility for high-performance applications such asvariable valve timing parts for automobile engines.

Nonferrous powder producers are also develop-ing new materials such as super high-strengthbronze alloys for PM gears. Some other new appli-cations for copper-base powders include coldspraying, lead-free brazing alloys and specialmaterials for frangible bullets. Compacting pressbuilders are developing improved warm com-paction systems that can process up to 13.6 kg(30 lb.) of powder per minute. One system is beingdesigned that can process parts with densities

above 7.5 g/cm3. The Center for Powder Metallurgy Technology

(CPMT) has launched its most ambitious program,focusing on achieving “full density” in a singlepressing operation. This program is funded byCPMT and through a consortium of companiesthat have raised over $200,000. The first phase ofthe program is targeting high-velocity compacting,warm compaction, and ultra-high-pressure com-paction. A corollary program focusing on admixedlubrication and die-wall lubrication has also beenlaunched.

MPIF recently published the revised and largestedition of Standard 35, Materials Standards forPM Structural Parts. It contains new informationon many of the 93 industry-approved ferrous andnonferrous materials. It covers chemical composi-tions and mechanical properties of 11 new materi-als, such as hybrid low-alloy steels,sinter-hardened steels, diffusion-alloyed steels,and prealloyed steels. A new section on the steamoxidation of ferrous PM materials has been added,as well as new guidelines for specifying PM parts.The new Standard 35 has the most comprehen-sive information on PM materials released by theindustry thus far.

The revised Materials Standards for MetalInjection Molded Parts was also published andcontains new materials, such as MIM-F-15 con-trolled-expansion alloys and MIM 420 stainlesssteel. New guaranteed maximum coercive forcevalues have been added for all the soft magneticalloys, along with new typical densities for all thematerials listed.

In addition, the newly published 2007 edition ofMPIF Standard Test Methods for Metal Powdersand Powder Metallurgy Products contains threenew standards. Developing up-to-date standardsthat reflect the most current industry practices isessential for PM’s continuing growth. In 2007MPIF has budgeted well over $200,000 for itsstandards development programs.

A new distance learning program is in develop-ment and will be launched in October this year.

PM trade associations all over the world alsohave a major role to play. Countries in Asia—notably Japan, Korea, China, and India—areworking towards an Asian PM federation.Similarly, EPMA and MPIF, respectively, need tobroaden their reach in order to represent theentirety of Europe and the Americas. It is time forAsia, Europe, and the Americas to collaborate



even more effectively to promote and grow PMworldwide, quite possibly through a global PMfederation.

Like never before, our industry is being tested.The changing automotive market, globalization,and competition from lower-cost countries, are alltesting PM’s resilience and future opportunity. Asin the past, the industry will meet and overcomechallenges to its continuous growth. We representa wealth of industrial and technical talent, as evi-denced by the technical papers presented here inDenver. We can be confident that our PM industrywill continue to grow as we invest in new technol-ogy and are not afraid of new ideas and approach-es to innovation. Let us not fear the challenges ofglobalization and competition. We must take on amore global perspective to continue growing in the21st century. Our long-term competition is notother PM companies; it is other fabricating tech-nologies and materials. We have to work togetherworldwide to grow the total PM pie so that each ofus can have a bigger slice. This can only happenby collaboration, by technological innovation, andpossibly through a worldwide federation as a cat-alyzing force.

We can and must become stronger and better.PM’s future, forged in the fires of a competitivestruggle, will be bright indeed. ijpm



INTRODUCTIONNickel is an important alloying additive in PM steels. It increases

strength and allows for improved control of dimensional change (DC)during sintering, particularly in PM steels that contain copper. At thenormal sintering temperature of 1,120°C, the diffusion of nickel isincomplete and this results in PM steels with nonuniform microstruc-tures, containing nickel-rich areas (NRAs). While these NRAs can bebeneficial in relation to toughness and fatigue properties,1 nickel mustbe diffused completely in the steel matrix for maximum hardenabilityand to maximize solution hardening. Higher sintering temperatures2

and/or longer sintering times promote nickel diffusion. However, theseapproaches are not used widely in the PM industry due to the atten-dant cost. Recent studies3 have shown that the use of extra-fine nickelpowder (D50 1.5 µm), instead of standard PM nickel powder (D50 8 µm)offers an attractive alternative to increasing the diffusion of nickel inPM steels. In addition to improving the nickel distribution, the use ofextra-fine nickel powder in nickel–copper-based PM steels alsoimproves the distribution of copper by increasing the interactionbetween these elements during sintering.4,5

Alloying additions can be admixed, diffusion-alloyed, or prealloyed insteel powders. While prealloying leads to homogeneous microstructuresand higher mechanical properties, it is usually detrimental to powdercompressibility. For this reason, in applications requiring high densi-ties, alloying additions such as copper and nickel are usually admixedwith steel powders. However, this can lead to segregation if particleswith different sizes and densities are mixed together. Admixing can alsolead to flow and dusting problems in which case binding the alloyingadditions to the surface of the base steel powder can be beneficial. Twotypes of bonding technique are used in PM, namely, partial alloying andbinder treatments. In partial alloying, the additives are partially dif-fused into the iron powders forming a strong metallurgical bond. Inbinder treatments, an organic binder, usually a polymer or wax, acts asan adhesive. The bonding strength of binder-treated mixes is lowerthan that of diffusion-alloyed mixes. However, this approach is relative-

Distribution of the alloyingadditives in powder metallurgy (PM) steels is akey element in achievingoptimum sintered properties.Segregation must be avoided in order to ensureconsistent part-to-part properties. Recent studiesindicate that extra-fine nickel powders have a beneficial impact on theoverall properties of nickel–copper–carbon PM steels.Therefore, the use of extra-fine nickel powder in segregation-free PM mixescould be an efficient way tooptimize properties. To thisend, the effect of the sizeand size distribution of twonickel powders on the physical and mechanicalproperties of two binder-treated steel powder premixes processed on apilot scale has beenassessed. The properties ofthese two mixes are compared with those of a diffusion-alloyed mix of thesame composition.Mechanical properties anddimensional change of thebinder-treated mixes areshown to be superior tothose of the diffusion-alloyed mix. The physicaland sintered properties ofthe binder-treated mixescan be further improved byusing extra-fine nickel powder (D50 1.5 µm) insteadof a standard size (D50 8 µm) nickel powder.

HIGH-PERFORMANCE PM STEELS UTILIZINGEXTRA-FINE NICKEL Lhoucine Azzi*, Tom Stephenson**, Sylvain Pelletier*** and S. St-Laurent****

RESEARCH &DEVELOPMENT

*Research Associate, ***Group Leader, Industrial Materials Institute, National Research Council Canada, Boucherville, Québec; E-mail:[email protected], **Technology & Development Manager, INCO Special Products, 2101 Hadwen Road, Mississauga, Ontario, Canada, L5K 2L3,****R&D Manager, Quebec Metal Powders Limited, 1655 Marie Victorin, Tracy, Québec, Canada, J3R 4R4


ly inexpensive and has the advantage over diffu-sion-alloying treatments that it can bind the lubri-cant and graphite. Binder-treated mixes usuallyexhibit acceptable flow properties, reduced segre-gation, and, as a result, improved part-to-partdimensional consistency.

Using extra-fine nickel powder in bonded PMmixes offers an efficient way to optimize the prop-erties of nickel–copper PM steels. In this study,the effect of two nickel powders with differentsizes and size distributions on the physical andmechanical properties of two binder-treated nick-el–copper–molybdenum steel powder premixeswas evaluated. The properties obtained utilizingthe two binder-treated mixes processed on a pilotscale are compared with those of a diffusion-alloyed mix of the same composition. Each of theeight components of the study is presented as astand-alone entity in terms of experimental proce-dures, results/observations, and implications/discussion.

POWDER MIXESTwo base powders were used in the study:

ATOMET 4001, a water-atomized prealloyed steelpowder containing 0.5 w/o Mo and ATOMET DB46, a diffusion-alloyed powder containing 0.5 w/oMo, 1.75 w/o Ni, and 1.5 w/o Cu. Three 68 kgpilot-size mixes (two binder-treated mixes and onediffusion-alloyed mix) were prepared in a twin-shell V-Type blender/dryer. All three powdermixes had the same composition: Fe-0.5 w/o Mo-1.5 w/o Cu-1.75 w/o Ni-0.6 w/o graphite (0.5w/o sintered carbon).

The diffusion-alloyed mix was prepared byadding and dry mixing 0.6 w/o natural graphite

(SW 1651) and 0.75 w/o lubricant (Acrawax C) tothe ATOMET DB46 diffusion-alloyed powder. TheATOMET DB46 powder was obtained by partiallydiffusing copper and nickel to ATOMET 4001powder (a prealloyed powder containing 0.5 w/oMo and 0.15 w/o Mn). The regular mix (graphiteand lubricant not bonded) was identified as AT-DB40A in this study.

The two binder-treated mixes of nominal com-position FLN2C-4005 were prepared in the twinshell V-Type blender/dryer by means of a patentedbinder technology.6 These mixes were prepared byadmixing 1.75 w/o Ni, 1.5 w/o Cu (D50~15 µm), 0.6 w/o natural graphite (SW 1651), and0.65 w/o wax lubricant (Acrawax C) with theATOMET 4001 powder for 30 min. A solution con-taining the binder at a concentration of 0.2 w/o ofthe powder mix was then injected into the blenderand rotated for an additional 10 min. The powderswere dried by vacuum extraction of the solvent.Two different carbonyl nickel powders, INCO T123PM and INCO T110 D, and a fine commercial cop-per powder (D50 ~15–20 µm) were used in thesemixes. The binder-treated mixes containing theINCO T123 PM and T110 D nickel powders wereidentified in this study as F40A-123 and F40A-T110, respectively. The particle-size distribution ofthese two nickel powders, as measured by laserdiffraction particle-size analysis, is given in TableI. The characteristics of the 68 kg steel mixes usedin the study are summarized in Table II.

PARTICLE BONDING AND DISPERSIONFigure 1 shows representative scanning electron

micrographs (SEM) of bonded powders in thebinder-treated and regular diffusion-alloyed pow-der mixes. It can be seen that, in the case of theregular non-bonded mix, a significant proportionof the graphite and lubricant particles are free andnot attached to the iron particles. Nevertheless,dry-bonding of graphite is observed. This is dueprimarily to the presence of the lubricant that actsas a binder. In the case of the binder-treated pow-

HIGH-PERFORMANCE PM STEELS UTILIZING EXTRA-FINE NICKEL

TABLE I. PARTICLE-SIZE DISTRIBUTION OF FINE ANDEXTRA-FINE NICKEL POWDERS

Type D10 (µm) D50 (µm) D90 (µm)

INCO 123 1.25 8 20INCO T110 0.5 1.5 4.7

TABLE II. MIX CHARACTERISTICS

Mix Identification Type of Mix Prealloyed Additives Diffusion Additives Admixed Additives(w/o) (w/o) (w/o)

Mo Mn Ni Cu Ni Cu C

AT-DB40A Regular/Diffusion-Alloyed 0.5 0.15 1.75 1.5 0.6F40A-123 Binder-Treated 0.5 0.15 1.75 (T123 PM) 1.5 0.6F40A-T110 Binder-Treated 0.5 0.15 1.75 (T110 D) 1.5 0.6


der, the graphite and lubricant particles are essen-tially all bonded to the iron particles. The size ofthe nickel particles has a significant impact ontheir bonding and dispersion. The extra-fine nickelparticles were more efficiently bonded and distrib-uted on the surface of the iron particles than werethe standard-size nickel particles. This is attrib-uted to the increase of the adhesion forces as thedifference in size between the iron particles andthe nickel particles increases.

The nickel distribution was also examined aftercompaction. Green compacts were pressed to a

density of 7.0 g/cm3 and partially sintered at600°C in argon for 30 min. Sintering at this tem-perature provides sufficient green strength toallow for polishing, while limiting diffusion of thealloying additives. The nickel distribution wasevaluated by energy dispersive spectrometry(EDS) mapping, Figure 2. It can be seen that, inthe green compacts, the extra-fine nickel particlesare more uniformly distributed than are the stan-dard-size nickel particles. This is attributeddirectly to the enhanced bonding efficiency anddispersion of the nickel particles during thebinder treatment.

DUSTING RESISTANCEThe bonding efficiency of the three bonded

mixes was evaluated by measuring the level ofretention of graphite, lubricant, nickel, and cop-per after the powder mixes were subjected to a


Figure 1. Representative SEM images of powder mixes.(a) F40A-123, (b) F40A-T110, (c) AT-DB40A. C = graphite or lubricant. BS = back-scattered electron image.

Figure 2. EDS mapping of nickel in powder mixes. (a) F40A-123, (b)F40A-T110

(a)

(a)

(b)

(b)

(c)


strong flow of air. The dusting test consisted ofpouring 25 g of powder into a 25 mm cylindricaltube and flowing an air stream into the tube at arate of 6 L/min for 5 min. The flow of air wasstrong enough to partially fluidize the powder. Thepowder was analyzed before and after the test andthe dusting resistance of a specific element deter-mined by means of the relation:

Dusting Resistance = [(w/o after test) / (w/o before test)] x 100 (1)

Figure 3 shows the dusting resistance factor forgraphite, copper, and nickel of the powder mixesAT-DB40A, F40A-123 and F40A-T110.

As expected, the dusting resistance of copperand nickel in the diffusion-alloyed mix is high. Themean dusting resistance of graphite is around90% in the binder-treated mixes. It could be readi-ly increased to >95% by selecting appropriatebinding parameters. The dusting resistance of cop-per is between 45% and 50% in the two binder-treated mixes, which is typical of binder-treatedmixes containing commercial copper powders. Itshould be noted that the dusting resistance of cop-per in regular non-bonded mixes is ~20% to 25%.The dusting resistance of graphite in the regulardiffusion-alloyed mix is higher than that of copperin the binder-treated mixes (60% vs. ~50%).

Fine natural graphite powders have large flatsurfaces with the ability to adhere to large parti-cles by van der Waals–type forces. The nickeldusting resistance was ~60% for mix F40A-123,compared with ~25% in the regular mixes.Essentially no nickel dusting loss was recordedfor the fine nickel mix. Several iron powder manu-facturers have independently confirmed this ten-

dency.1,7 However, contrary to the study byNichols and Sawayama,7 we conclude that theextra-fine nickel powder was not only more effi-ciently bonded, but was also more uniformly dis-persed in the powder mix. These different findingsmay be related to the different binders, base pow-der and/or processing methods used to preparethe binder-treated mixes. The use of extra-finenickel in binder-treated mixes is an efficient wayto improve industrial hygiene in relation to nickeldusting at a reduced cost compared with diffu-sion-alloyed mixes.

POWDER FLOW AND GREEN PROPERTIESThe flow rate, apparent density, green strength,

and compressibility of the powder mixes AT-DB40A, F40A-123, and F40A-T110 were evaluat-ed in compliance with MPIF standards 03, 04, 41,and 45. These properties are reported in Table IIIand Figure 4.

The flow rates of the two binder-treated mixeswere higher than that of the regular diffusion-alloyed mix. The flow rate of the regular diffusion-alloyed mix is typical and is attributed to thestrong adhesion introduced by wax-type lubri-cants.8 Binding the wax lubricant reduces the“stickiness” of the powder mix, resulting in


Figure 3. Dusting resistance of powder mixes AT-DB40A, F40A-123, and F40A-T110. 100% = no dusting loss; 0% = total loss of additive

Figure 4. Compressibility of powder mixes AT-DB40A, F40A-123, and F40A-T110

TABLE III. FLOW AND GREEN PROPERTIES

Mixture Apparent Flow Rate Green StrengthIdentification Density (g/cm3) (s/50 g) (7 g/cm3)

MPa psi

AT-DB40A 3.19 35 8.7 1,270F40A-123 3.19 27 9.4 1,360F40A-T110 3.14 27 9.8 1,420


improved flow behavior. The binder-treated mixesand the regular mix exhibited similar low greenstrengths. This is typical of green compacts con-taining wax-type lubricants and is associated withthe lack of metal-to-metal contact due to smear-ing of the lubricants during mixing. Partial alloy-ing appears to affect the compressibility of thediffusion-alloyed mix at compacting pressures<550 MPa (40 tsi). However, at pressures >690MPa (50 tsi) the diffusion-alloyed mix exhibited ahigher compressibility than the binder-treatedmixes. This is related to the lower level of organicsin the diffusion-alloyed mix.

TRANSVERSE RUPTURE AND TENSILEPROPERTIES

Transverse rupture strength (TRS) was evaluat-ed on sets of 10 samples compacted on a double-acting floating die. Tensile properties wereevaluated on sets of 40 samples taken at randomduring runs of 250 dog-bone specimens pressedon an industrial 150 mt mechanical press at astroke rate of 10 parts per min. All the sampleswere sintered for 30 min at 1,120°C in a nitrogen-base atmosphere, containing 5 v/o hydrogen uti-lizing a commercial mesh-belt furnace. The coolingrate in the range 650°C–400°C was ~0.9°C/s. Onehalf of all the test specimens were tempered at205°C for 1 h in air before mechanical testing.

Results of the transverse rupture (TR) tests arereported in Figure 5. The TRS of the binder-treatedmixes was found to be higher than that of the dif-fusion-alloyed mixes, especially at low sintereddensities. The TRS of the fine-nickel mix was foundto be slightly higher (4%) than that of the standard-nickel mix, and 5% to 10% higher than that of thediffusion-alloyed mix. The apparent hardness of

the binder-treated mixes was found to be slightlyhigher than that of the diffusion-alloyed mix.

The results of the tensile tests are reported inTables IV and V. As was the case with the TRtests, the tensile properties of the binder-treatedmixes were found to be higher than those of thediffusion-alloyed mixes. For specimens pressed to7.0 g/cm3, the as-sintered UTS and yield strengthof the fine-nickel mix were found to be ~5% higherthan those of the binder-treated mix containingthe standard nickel powder, and ~20% higher thanthose of the diffusion-alloyed mix. At 7.2 g/cm3,the as-sintered UTS of the F40A-T110 mix was 7%higher than that of the F40A-123 mix and ~13%higher than that of the diffusion-alloyed mix.

Tempering increased the yield stress of all threepowder mixes at all the sintered densities evaluat-ed. This effect was more pronounced in the fine-


Figure 5. Sintered TRS as a function of compaction pressure in as-sintered andtempered conditions

TABLE IV. AS-SINTERED TENSILE PROPERTIES*

Mix Green UTS Yield at 0.2% Maximum ApparentIdentification Density (MPa) Plastic Strain Elongation Hardness

(g/cm3) (MPa) (%) (HRA)

Average Standard Average Standard Average Standard AverageDeviation Deviation Deviation

AT-DB40A 7.00 560 28 420 13 1.8 0.13 507.20 650 9 485 4 1.8 0.12 54

F40A-123 7.00 660 16 490 9.6 1.7 0.13 507.20 690 41 520 13 1.6 0.32 55

F40A-T110 7.00 690 23 510 8.7 1.7 0.11 547.20 740 13 545 6.7 1.7 0.12 56

*Average of 20 samples


nickel mix (7% increase vs. 4.5% increase for theother mixes) except for specimens pressed to 7.0g/cm3 where an increase of 9% was recorded inthe dif fusion-alloyed mix. The elongationremained essentially unchanged in all the mixes,which is typical for formulations with ~0.50 w/osintered carbon. UTS was also increased by tem-pering the fine-nickel mix at all sintered densities.However, this gain in strength was more modestthan the gain in yield strength (4% vs. 7%). Theeffect of tempering on UTS for the other mixeswas marginal. Apparent hardness was also basi-cally unchanged by tempering for all three mixes.Similar behavior has been reported in other stud-ies9 and was explained in terms of a reduction inthe residual stresses during tempering. The factthat tempering affected the tensile properties ofthe fine-nickel powder mix more positively andmore consistently is an indication of a more uni-form microstructure containing more martensitecompared with the coarser-nickel powder mix.Dimensional change (DC) after tempering of theTR specimens also supports this claim.

DIMENSIONAL CHANGE AFTER SINTERINGTR Specimens

Figure 6 shows that DC from die size was posi-tive in all the powder mixes. DC from green sizewas negative, showing that shrinkage actuallyoccurred during sintering. The net positive DCwas due to spring-back after ejection of the parts.DC in the binder-treated mixes (from green size)was more negative than in the diffusion-alloyedmix at all compacting pressures. The fine-nickelmix exhibited a more negative DC than mix F40A-123. In addition, the difference in DC betweenmix F40A-T110 and the other two powder mixes

was more pronounced as the compaction pres-sure increased. The more negative DC (from greensize) in the F40A-T110 mix compared with mixF40A-123 is associated with enhanced nickel dif-fusion in the iron matrix. As density increases,this shrinkage effect also increases. The morepositive DC recorded in the diffusion-alloyed mixmight be due to slight differences in the copperpowder size and/or distribution, due to agglomer-ation of copper during annealing.

The partial diffusion of nickel and copper in theiron matrix that occurs during annealing of theiron–copper–nickel mixture is also a contributingfactor. The diffusion-bonded (DB) material and thebinder-treated mix utilizing the 123 nickel powdercontain the same nickel type (particle size). Theshape of the DC curves (Figure 6) of these twomixes is similar but offset. In contrast, the shapeof the DC curve of the mix containing 110 nickelis dif ferent and close to the 123 material.Therefore, it is concluded that size of the nickelpowder controls the DC response (shape of thecurves in Figure 6), while the bonding type (par-tial alloying vs. binder) controls the curve offset.

Evidence of enhanced nickel diffusion in thefine-nickel mix can be seen in Figure 7 where thedensity variation after sintering is reported. Thesamples containing fine nickel powder resulted ina higher density; this is attributed to the swellingeffect of the copper negated by the increasedshrinkage due to the extra-fine nickel powder.Figure 8 shows that dimensional change is affect-ed by tempering. DC was slightly more negativeafter tempering in all the powder mixes. The effectof tempering on DC has been monitored in otherstudies and was related to the levels of martensiteand carbon in the alloys.10


TABLE V.TENSILE PROPERTIES*

Mix Green UTS Yield at 0.2% Maximum ApparentIdentification Density (MPa) Plastic Strain Elongation Hardness

(g/cm3) (MPa) (%) (HRA)

Average Standard Average Standard Average Standard AverageDeviation Deviation Deviation

AT-DB40A 7.00 589 20 462 9 1.9 0.11 507.20 643 25 505 8 1.8 0.13 54

F40A-123 7.00 665 26 511 10 1.8 0.19 517.20 711 22 544 9 1.9 0.31 55

F40A-T 110 7.00 723 10 551 6.3 1.9 0.17 537.20 770 19 586 10 1.9 0.19 55

*Average of 20 samples


Dimensional Change—Ring SpecimensIn order to compare part-to-part consistency of

the two binder-treated mixes, DC and distortionwere measured on ring specimens (OD 51 mm, ID43 mm, height 6.35 mm) compacted to a green

density of 7.2 g/cm3 on a 150 mt mechanicalpress. Limited runs of 250 parts were carried outfor each powder. DC and distortion after sinteringof the rings were measured on 30 specimensselected at random during the runs. The sinteringconditions were identical to those used for the TRand tensile specimens. Measurements were carriedout on the green and as-sintered samples utilizingthe coordinate measuring machine (CMM) tech-nique. CMMs are mechanical systems designed tomove a measuring probe to determine coordinatesof points on the surface of the workpiece. By meas-uring the coordinates of these points before andafter sintering, DC and distortion can be evaluated.

The wall thickness (OD – ID) of the rings wasmeasured before and after sintering at 40°, 80°,160°, 200°, 280°, and 320° from a reference pointmarked on the rings. For each ring an averagewall thickness was calculated as the mean of themeasured (OD – ID) values obtained at each of thesix angles. This procedure was applied to eachring in the green and as-sintered states. DC onthe wall thickness was calculated as the differ-ence of the mean values in the green and as-sin-tered states. Mean DC values for mix F40A-123and mix F40A-T110 were calculated as the meanDC from 30 different samples. The standard devi-ation from the 30 samples was used a measure ofDC consistency.

For the determination of out-of-roundness, theODs of the green rings were measured at 40°, 80°,160°, 200°, 280°, and 320° from the referencemark and the difference between the maximumOD and the minimum OD calculated. The sameprocedure was used for the sintered rings. Valuesreported in Table VI refer to the difference in out-of-roundness before and after sintering (i.e., dis-tortion due to sintering).

The out-of-roundness variation was marginaland similar for the two powder mixes evaluated.However, the results show that, as for the TRspecimens, more shrinkage occurred in powder


Figure 6. Mean dimensional change as a function of compaction pressure

Figure 7. Density variation after sintering as a function of compaction pressure

Figure 8. DC associated with tempering (205°C/1h) for specimens pressed to 7.0 g/cm3

TABLE VI. DC OUT-OF-ROUNDNESS VARIATION IN RINGS*

Wall Thickness Out-of-Roundness(∆D/DO)

Powder Mix Average Standard Average Standard(%) Deviation (%) Deviation

F40A-123 -0.002 0.14 0.00056 0.0004F40A-T110 -0.036 0.05 0.00057 0.0004

*Green density 7.2 g/cm3, D = wall thickness = (OD – ID)


mix F40A-T110 containing the extra-fine nickel.In addition to being more negative, the DC wasmore consistent for the binder-treated mix con-taining the extra-fine nickel. The use of the extra-fine nickel powder, instead of the standard nickelpowder, reduced the standard deviation in thewall thickness variation by a factor of 3.

MICROSTRUCTURE The phases constituting the microstructure of

the three powder mixes under study were similar.A representative optical micrograph (OM) isshown in Figure 9(a) where areas of fine pearlite(300 HV 10 gf), divorced pearlite (180 HV 10 gf),martensite (500 to 740 HV 10 gf), and retainedaustenite (150 to 200 HV 10 gf) are evident. Ahigh-magnification scanning electron micrograph(SEM) of the fine pearlite (backscattered image(BSI)) in mix F40A-123 is shown in Figure 9(b).Figure 10 shows representative OMs of three sintered mixes confirming that the fine-nickel

powder mix contained more martensite and lessretained austenite than the other two mixes. Themicrostructure of the standard-nickel mix wasless homogeneous than that of the DB mix(Figures 10–13) but the proportions of the differ-ent phases were similar in the two mixes.

EDS mapping revealed obvious differences inthe distribution of the NRAs in the microstructureof the three powder mixes (Figures 11–13).


Figure 9. (a) Representative microstructure showing fine pearlite(FP) bordered by divorced pearlite (DP), martensite (M), and nickel-rich retained austenite. OM (b) high magnification of black area (FP). Mix F40A-123 pressed to 7.0 g/cm3. SEM/BSI

Figure 10. Representative microstructures of sintered mixes. (a)F40A-T110, (b) F40A-123, and (c) AT-DB40A. OM

(a)

(a)

(b)

(c)

(b)


Figures 11 and 12 show that the NRAs are moreevenly distributed in the microstructure of thefine-nickel powder mix. NRAs with a high nickelcontent are observed in the microstructure of mixF40A-123. In the fine-nickel powder mix, NRAswere usually more uniformly distributed and

smaller in size, indicating that more nickel wentinto solution in the iron matrix. The nickel-richareas in mix F40A-123 were frequently found to


Figure 11. Dispersion of copper and nickel in powder mix F40A-T110after compaction to 7.2 g/cm3 and sintering at 1,120°C for 30 min.(a) back-scattered electron image, (b) EDS map for copper, and (c) EDS map for nickel

(a)

(b)

(c) Figure 12. Dispersion of copper and nickel in powder mix F40A-123after compaction to 7.2 g/cm3 and sintering at 1,120°C for 30 min.(a) back-scattered electron image, (b) EDS map for copper, and (c) EDS map for nickel. Agglomerates of copper and nickel evidentnear pores (white circles). In dense areas, agglomerated nickel doesnot associate with copper

(a)

(b)

(c)


be associated with copper-rich areas. As a result,the copper distribution was less uniform in thesemixes. NRAs located around large pores containeda high level of copper, while NRAs located indense (pore-free) areas contained almost no cop-

per. This result is explained by the fact that whencopper melts, it leaves behind pores that corre-spond to the initial particle size of the copper. Theenhanced mechanical properties, and the reducedswelling of the fine-nickel powder mix, are attrib-uted primarily to: (i) the more-uniform dispersionof both NRAs and copper, (ii) more solution hard-ening due to the increased amount of nickel dif-fused in the iron matrix, and (iii) the higherpercentage of martensite.

NRAs in the diffusion-alloyed mix were alsofound to be concentrated preferentially in thenickel compared with the NRAs in the fine-nickelmix (Figures 11–13). Qualitative line scansshowed that the concentration of nickel in theNRAs of the DB and the standard material is simi-lar. However, contrary to mix F40A-123, copperagglomeration was not obvious in concentratedNRAs. The copper distribution was virtuallyimmune to the nickel distribution in the diffu-sion-alloyed mix. This result suggests that partialalloying of copper occurred during annealing ofthe iron–nickel–copper mixture. This phenomenonmight also explain the more positive DC exhibitedby the DB material.

The reasons why the mechanical properties ofthe DB material are lower than those of the stan-dard-nickel material are not obvious. This behav-ior has been observed in premixes of similarcomposition of diffusion-alloyed grades of similarmaterials.10 The fact that nickel and copper donot interact in a similar fashion in these twomixes could be a factor. The difference in thenature of the organics in the two mixes could alsohave an impact on the final mechanical propertiesof the two mixes. Indeed, even if the same lubri-cant were used for both the DB and the binder-treated mixes, the presence of a binder mightchange the properties. While the effect of theextra-fine nickel powder in the fine-nickel mix canexplain the higher performances of this materialcompared with the DB material, further studiesare needed to explain the differences between theDB and the standard-nickel materials.

CONCLUSIONS• The use of extra-fine nickel powders signifi-

cantly reduced nickel dusting in binder-treat-ed mixes to levels as low as the nickel dustinglevels in diffusion-alloyed mixes.

• TRS and tensile properties of the two binder-treated mixes were superior to those of their


Figure 13. Dispersion of copper and nickel in powder mix AT-DB40Aafter compaction to 7.2 g/cm3 and sintering at 1,120°C for 30 min.(a) back-scattered electron image, (b) EDS map for copper, and (c) EDS map for nickel. Agglomeration of nickel does not result inagglomeration of copper

(a)

(b)

(c)


diffusion-alloyed counterparts. The binder-treated mix containing extra-fine nickel pow-der showed the largest improvements. TRSwas 5% to 10% higher than that of the diffu-sion-alloyed mix while UTS and yield stresswere 15% to 20% higher.

• Increased densification occurred in thebinder-treated mix containing extra-fine nick-el powder. As density increased, this shrink-age effect also increased and the density aftersintering of the binder-treated mix containingextra-fine nickel powder was higher than ofthe diffusion-alloyed mix and the binder-treated mix containing the standard nickelpowder.

• DC measurements indicate that, in additionto being more negative, DC is more consistentin the fine-nickel mix.

• NRAs were more evenly distributed and lessconcentrated in nickel in the microstructureof the fine-nickel powder mix compared withthe diffusion-alloyed mix. As a result, thecopper distribution was improved in themicrostructure of the fine-nickel powder mix.

This study has shown that the properties ofbinder-treated mixes can be improved over thoseof equivalent diffusion-alloyed mixes. The use ofextra-fine nickel powders, instead of standard-sizePM nickel powders, can further extend theseimprovements. In binder-treated mixes containingnickel, copper, carbon, and molybdenum, theseimprovements are associated with (i) a more uni-form dispersion of NRAs and the presence of cop-per in the steel microstructure, and (ii) enhancedsolution hardening due to increased nickel diffu-sion. The results suggest that the beneficialimpact of the extra-fine nickel powder on theproperties of PM parts increases with density.

REFERENCES1. T.F. Stephenson, T. Singh and S.T. Campbell,

“Performance Benefits in Sintered Steels with Extra-FineNickel Powder”, Euro PM 2004, edited by H. Danningerand R. Ratzi, European Powder Metallurgy Association,Shrewsbury, UK, 2004, vol. 7, pp. 105–115.

2. J.A. Hamill, R.J. Causton and S.O. Shah, “HighPerformance PM Materials Utilizing High TemperatureSintering”, Advances in Powder Metallurgy & ParticulateMaterials, compiled by J.M. Capus and R.M. German,Metal Powder Industries Federation, Princeton, NJ, 1992,vol. 5, pp. 193–214.

3. S.T. Campbell, T. Singh and T.F. Stephenson, “ImprovedHardenability of PM Steels Using Extra-Fine NickelPowder”, Advances in Powder Metallurgy & ParticulateMaterials, compiled by R.A. Chernenkoff and W.B. James,Metal Powder Industries Federation, Princeton, NJ, 2004,part 7, pp. 105–115.

4. T. Singh, T.F. Stephenson and S.T. Campbell, “Nickel-Copper Interactions in PM Steels”, ibid. reference no. 3,pp. 93–104.

5. T.F. Stephenson, T. Singh and S.T. Campbell, “Influence ofExtra-Fine Ni Powder on PM Steel Properties”, Advances inPowder Metallurgy & Particulate Materials, compiled by R.Lawcock and M. Wright, Metal Powder IndustriesFederation, Princeton, NJ, 2003, part 7, pp. 111–121.

6. F. Gosselin, “Segregation-Free Metallurgical PowderBlends using Polyvinyl Pyrrolidone Binder”, U.S. PatentNo. 5,069,714, December 3, 1991.

7. B. Nichols and T. Sawayama, “Investigation of PowderProperties in a FN-0208 Binder-Treated Powder”, ibid. ref-erence no. 1, pp. 1–9.

8. S. Uenosono, Y. Ozaki and H. Sugihara, “Development ofa High Flowable Segregation-Free Iron Based Powder Mixwith Wax Lubricant”, Journal of the Japan Society ofPowder and Powder Metallurgy, vol. 48, no. 4, 2001, pp.305–310.

9. S. St-Laurent and F. Chagnon, “Dynamic Properties ofSintered Molybdenum Steels”, Advances in PowderMetallurgy & Particulate Materials, compiled by V.Arnhold, C-L Chu, W.F. Jandeska, Jr. and H.I. Sanderow,Metal Powder Industries Federation, Princeton, NJ, 2002,part 5, pp. 121–133.

10. F.J. Semel, “Ancorloy Premixes: Binder-Treated Analogsof the Diffusion Alloyed Steels”, Advances in PowderMetallurgy & Particulate Materials, compiled by C.L. Roseand M.H. Thibodeau, Metal Powder Industries Federation,Princeton, NJ, 1999, part 7, pp. 93–115. ijpm



INTRODUCTIONPrecipitation hardening (commonly called age hardening) occurs

when two phases precipitate from a supersaturated solid solution.1 Forexample:

Precipitation: Solid A → Solid A1 + Solid B. (1)

The primary requirement of an alloy for precipitation hardening isthat the solubility of B in A decreases with decreasing temperature sothat a supersaturated solid solution forms on rapid cooling.

Strengthening as a result of precipitation hardening takes place inthree steps,2 illustrated in Figure 1 for the Al-Cu system:1

(1) Solution treatment, in which the alloy is heated to a relativelyhigh temperature that allows any precipitates or alloying ele-ments to form a superstaurated solid solution.

(2) Quenching, in which the solution-treated alloy is cooled to createa supersaturated solid solution. The cooling can be achievedusing air, water, or oil. In general, the faster the cooling rate the

Applications requiring high-strength stainlesssteels are growing rapidally.Precipitation-hardeningstainless steels have seenlimited use in powder metallurgy (PM) despite their high strength. Thestrengthening of thesealloys is achieved byadding elements such ascopper and niobium, whichform intermetallic precipitates during aging.The precipitation-hardeninggrades exhibit corrosionresistance levels comparable with those ofthe chromium–nickel (300 series) grades. Thephysical properties andmicrostructures of two precipitation-hardening PMstainless powders are presented: 17-4 PH, a high-chromium, martensiticprecipitation-hardeningstainless steel, has beenoptimized for use in PMapplications; and a newlow-chromium (12 w/o)alloy that utilizes copper inthe precipitation reaction.This alloy (410LCu), is considered to be a cost-effective alternative in applications that requirehigh strength and moderatecorrosion resistance.

PRECIPITATION-HARDENING PM STAINLESS STEELSChristopher T. Schade*, Patrick D. Stears**, Alan Lawley*** and Roger D. Doherty****

RESEARCH &DEVELOPMENT

*Manager, Pilot Plants & Process Engineer, Hoeganaes Corporation, 1001 Taylors Lane, Cinnaminson, New Jersey 08077, USA; E-mail:[email protected], **Process Engineer, Hoeganaes Corporation, 1315 Airport Road, Gallatin, Tennessee 37066, USA, ***Emeritus Professor, ****A.W. Grosvenor Professor, Drexel University, Philadelphia, Pennsylvania 19104, USA

Presented at PowderMet2006and published in Advances in Powder Metallurgy &Particulate Materials—2006,Proceedings of the 2006International Conference onPowder Metallurgy &Particulate Materials, whichare available from thePublications Department ofMPIF (www.mpif.org).

Figure 1. Precipitation hardening sequence1: (a) Partial Al-Cu equilibrium phase diagram, (b) heattreatment and resulting microstuctures


finer the grain size which can lead toimproved mechanical properties. Regardlessof the method of cooling, the cooling ratemust be sufficiently rapid to create a super-aturated solid solution.

(3) Precipitation or age hardening, in which thequenched alloy is heated to an intermediatetemperature and held for a period of time. Atthe intermediate temperature the supersat-ured solid solution decomposes and the alloy-ing elements form small precipitate clusters.The precipitates hinder the movement of dis-locations and consequently the metal resistsdeformation and its strength increases.

Austenitic, semiaustentic, and martensitic pre-cipitation-hardening stainless steels currentlyexist. The austenitic and semiaustenitic composi-tions were originally designed for aerospace appli-cations involving high temperatures (>704°C(>1,300°F)) where high strength is required. Themartensitic precipitation-hardenable alloys aremore widely used than the austenitic and semi-austenitic grades, and are the focus of this study.

BACKGROUNDTwo alloys were examined in this study. The

first alloy, 17-4 PH (UNS S17400), is a chromi-um–nickel–copper precipitation-hardening alloyused for applications in the aerospace, chemical,petrochemical, and food processing industries.Common wrought products made from 17-4 PHstainless steel include valves, fittings, springs,fasteners, and boat shafts. 17-4 PH powder hasbeen widely studied for metal injection molding(MIM) applications.3–5

The second alloy examined was a variation ofUNS J91151, primarily a casting-grade alloy. Inthe PM version, the composition was adjusted toallow for precipitation hardening via copper. Thisalloy also contains a unique balance of elementsthat strengthen the martensitic matrix, while pro-viding a high level of ductility. UNS J91151 finds

applications in pump impellers and casings dueto its resistance to cavitation; this property is typ-ically a function of the hardness of the alloy.6 Thechemical compositions of the two stainless steelgrades are shown in Table I.

ALLOY PREPARATION AND TESTINGThe powders used in this study were produced

by water atomization with a typical particle size(100 w/o) <150 µm (-100 mesh) and with 38 to 48w/o <45 µm (-325 mesh). All the alloying elements were prealloyed in the melt prior toatomization.

The prealloyed powders were mixed with 0.75w/o Acrawax C lubricant. Samples for transverserupture (TR) and tensile testing were compacteduniaxially at 690 MPa (50 tsi). All the test pieceswere sintered in a high-temperature Abbott con-tinuous-belt furnace at 1,260°C (2,300°F) for 45min in hydrogen with a dewpoint of -40°C (-40°F),unless otherwise noted.

Prior to mechanical testing, green and sintereddensity, dimensional change (DC), and apparenthardness were determined on the tensile and TRsamples. Five tensile specimens and five TR speci-mens were tested for each composition. The den-sities of the green and sintered steels weredetermined in accordance with MPIF Standard42, while tensile testing followed MPIF Standard10. Impact specimens were tested in accordancewith MPIF Standard 40. Apparent hardness meas-urements were conducted on tensile, TR, andimpact specimens following MPIF Standard 43.

Rotating bending-fatigue (RBF) specimens weremachined from test blanks that were pressed at690 MPa (50 tsi) and sintered at 1,260°C(2,300°F). The dimensions of the test blanks were12.7 mm × 12.7 mm × 100 mm. RBF tests wereperformed using rotational speeds in the range of7,000–8,000 rpm at R = -1 using four fatiguemachines simultaneously. Thirty specimens weretested for each alloy composition, utilizing thestaircase method to determine the 50% survivallimit and the 90% survival limit for 107 cycles inaccordance with MPIF Standard 56.

Metallographic mounts of the test materialswere examined by optical microscopy (OM) in thepolished and etched (Glyceregia) conditions.Etched specimens were used for microindentationhardness testing, following MPIF Standard 51.

Salt-spray testing on TR bars was performed inaccordance with ASTM Standard B 117-03. Five

PRECIPITATION-HARDENING PM STAINLESS STEELS

TABLE I. COMPOSITION OF MARTENSITIC PRECIPITATION-HARDENINGCAST AND WROUGHT STAINLESS STEELS (w/o)

AlloyUNS No. C S P Si Cr Ni Cu Mn Nb + Ta

S174000.07 .030 .040 1.0 15.0 3.0 3.0 1.0 0.15Max. Max. Max. Max. 17.0 5.0 5.0 Max. 0.45

J911510.15 .030 .040 1.5 11.5 1.0 3.0 1.0Max. Max. Max. Max. 14.0 Max. 5.0 Max.

—


TR bars per alloy (prepared as previouslydescribed) were tested. The percent area of thebars covered by red rust was recorded as a func-tion of time and the level of corrosion documentedphotographically.

RESULTS AND DISCUSSIONAlloy Development: 17-4 PH

The physical properties and processing condi-tions of 17-4 PH produced by conventional press-and-sinter PM techniques are not well documented.Work by Reinshagen et al.7 indicated that 17-4 PHhas not seen wide usage due to low powder com-pressibility. These authors also showed that, withan increase in the -45 µm (-325 mesh) fraction, theatomized powder sintered to higher densities andnegated the lower compressibility. However, withthe advent of new stainless steel processingroutes,8 it is now possible to produce a powderwith both low carbon and nitrogen levels that canbe compacted to reasonable green densities.Simultaneously, through a new high-performanceatomizing process, it is possible to produce a finersieve distribution, resulting in a higher sintereddensity. The use of high-temperature sintering isalso useful when processing 17-4 PH.

Table II gives the composition of the 17-4 PHused in this study. The notation CA refers tomaterial produced by conventional water atomiza-tion and the notation HPA refers to material pro-duced using the new high-per formancewater-atomization process.

The advanced high-performance processingroute for stainless steel powders utilizes an argonoxygen decarburization unit that removes bothcarbon and nitrogen from the melt. The mostcommon method for producing stainless steelpowders, induction melting, does not provide ameans to control the carbon and nitrogen levels.

It is well known that both carbon and nitrogenhave a negative impact on green density. Thegreen density of 17-4 PH is compared with con-ventional stainless steels 304L and 434L in Figure2. Over the range of compaction pressures shownin Figure 2, it can be seen that, while the greendensity is generally lower than other highly

alloyed stainless steels, 17-4 PH exhibits reason-able compressibility.

In general, lower green densities translate intolower sintered densities. It has been shown7 thatthe sintering of 17-4 PH is enhanced by highertemperatures, and in a pure hydrogen atmos-phere. The sintered density can also be improvedby increasing the -45 µm (-325 mesh) fraction ofthe powder or by sintering for longer times. Paststudies7 have focused on increasing the -45 µm (-325 mesh) fraction in the powder distribution.Using the HPA route, a melt was atomized inwhich the total distribution was finer, including a-45 µm (-325 mesh) fraction of 44 w/o. This pow-der and the powder with the standard distributiondescribed earlier were sintered in a 100 v/ohydrogen atmosphere at 1,260°C (2,300°F) for 20,35, 40, and 60 min, as shown in Figure 3.

Results show that, even with moderate times attemperature (20 min), sintered densities near 7.0g/cm3 can be achieved. As the time at tempera-ture is increased the sintered density increasesand reaches 7.40 g/cm3 after 60 min at 1,260°C(2,300°F). The material produced by HPA leads toa finer powder and higher sintered densities thanthe CA powder. The corresponding mechanicalproperties are increased, compared with materialproduced by CA. Figure 4 shows the transverse


TABLE II. COMPOSITION OF PM 17-4 PH STAINLESS STEEL (w/o)

Alloy C S O N P Si Cr Ni Cu Mn Mo Cb

17-4PH CA 0.023 0.006 0.25 0.020 0.008 0.78 17.43 4.67 3.84 0.06 0.03 0.2517-4PH HPA 0.011 0.005 0.23 0.018 0.009 0.86 17.34 4.61 3.92 0.20 0.02 0.26

Figure 2. Comparison of green density of 17-4 PH and two conventional stainless steels


rupture strength and apparent hardness of theHPA powder, over a range of sintered densities. Asexpected, the mechanical properties increase withincreasing sintered density.

The effect of aging can also be seen in Figure 4.Mechanical property data for wrought steels indi-cate that precipitation hardening can increase themechanical properties by as much as 15% to 20%.Although the thermal profile of the PM materials isslightly different to that of the wrought material, asimilar response is predicted. The wrought gradesof precipitation-hardening alloys are aged at tem-peratures from 482°C to 621°C (900°F to 1,150°F)for time periods ranging from 1 to 4 h. In order tooptimize the mechanical properties of PM 17-4 PH,test coupons were aged at various temperaturesand times in a nitrogen atmosphere. The effects ofthis aging treatment are illustrated in Figure 5. Itis seen that the optimum aging temperature for

maximum strength and apparent hardness in thisalloy occur at about 538°C (1,000°F) for 1 h.Higher temperatures led to over-aging (coarserprecipitates) and lower mechanical properties.Similar to the wrought grades, mechanical proper-ties increased from 15% to 20%. The tensile prop-erties, apparent hardness, and impact energyvalues for 17-4 PH aged at 538°C (1,000°F) for 1 hare given in Table III.

17-4 PH is widely used in environments where alevel of corrosion resistance comparable with thatof the austenitic grades is needed, but in applica-tions that require higher strength and hardnessthan the austenitic grades can provide, Table III. Amore realistic comparison of mechanical propertiesand corrosion resistance would be provided by aduplex stainless steel (22 w/o chromium, 5.5 w/onickel, 3.5 w/o molybdenum), which has excellenttoughness and strength, Table III. Typically, duplexstainless steels are used in applications where thestrength of the austenitic stainless steel is inade-quate. The high levels of chromium, nickel, andmolybdenum account for the excellent corrosionresistance of the duplex alloy.

These three alloys were compacted at 690 MPa(50 tsi) and sintered at 1,260°C (2,300°F) in 100v/o hydrogen. Salt-spray testing, performedaccording to ASTM Standard B 117-03, was con-ducted for 240 h; the results can be seen visuallyin Figure 6. This test is intended as a generalguideline on the performance of the alloys. Allthree alloys exhibited similar levels of rust. Sincethe mechanism(s) of corrosion varies by applica-tion, specific testing must be undertaken toensure the satisfactory performance of the alloyunder a given set of conditions.


Figure 3. Sintered density of HPA and CA atomized powders as afunction of time at temperature

Figure 4. Properties of HPA 17-4 PH as a function of sintered density: (a) transverse rupture strength, and (b) apparent hardness



Figure 5. Mechanical properties of 17-4 PH as a function of aging temperature: (a) ultimate tensile strength, (b) yield strength, (c) elongation, and(d) apparent hardness

Figure 6. Photographic documentation of salt-sprayspecimens: (a) 304L, (b) Duplex, and (c) 17-4 PH

TABLE III. MECHANICAL PROPERTIES OF CORROSION-RESISTANT PM STAINLESS STEELS

Alloy 0.20% Offset UTS Apparent Hardness Elongation Impact Energy(103 psi) (MPa) (103 psi) (MPa) (HRA) (%) (J) (ft.·lb.f)

304L 31 213 52 358 36 14 42 31DUPLEX 50 344 84 578 50 10.8 120 89

17-4 PH Aged 100 688 119 819 60 1.7 26 19


ALLOY DEVELOPMENT: 410LCUThere are many applications in which stainless

steels with only moderate corrosion resistance(compared with 17-4 PH) but with excellentmechanical properties are required. A widely usedexample is MPIF SS-410-90HT. This is a PM 410Lstainless steel in which graphite is added to theatomized powder and the alloy is sintered in anitrogen-rich atmosphere. When carbon andnitrogen are added to 410L stainless steel, themicrostructure becomes martensitic, therebyincreasing both hardness and strength. Thisgrade of stainless steel is used in applicationswhere high hardness and strength are required.The disadvantage of using carbon and nitrogen isthat they decrease corrosion resistance and alsoreduce impact strength and ductility. Many fabri-cators request this alloy because there are fewalternative compositions. In the casting industry,UNS J91151 (Table I) exhibits many of the proper-ties exhibited by SS-410-90HT. This alloy can bemodified by copper to form a martensitic precipi-tation-hardening stainless steel.6

Based on UNS J91151, a series of PM copper-containing stainless steel alloys was fabricated.All the powders were produced by CA with 100w/o <150 mm (-100 mesh) and 38 to 48 w/o <45mm (-325 mesh). All the alloying elements wereprealloyed in the melt prior to atomization. TableIV cites the chemical composition of the precipita-tion-hardening 410LCu alloys examined.

The copper content was varied to determine theamount needed for optimum precipitation-hard-ening response. The nickel and molybdenum lev-els were varied to harden and strengthen themartensite in the alloy. Previous studies haveshown that there is a synergistic effect betweenmolybdenum, copper, and nickel on sintered den-sity.9 One alloy was made with the addition ofcolumbium to determine if this element wouldenhance the precipitation reaction.

Compressibility data over a range of com-

paction pressures show that the addition of cop-per (Alloy A) reduces green density slightly, whencompared with SS-410-90HT, but is substantiallyhigher than 17-4 PH (Figure 7). Even when nickeland molybdenum are added with increasing levelsof copper, the compressibility of the experimentalalloys exceeded that of 17-4 PH.

The static mechanical properties of these alloysare compared in Table V. It is apparent that thealloys with small additions of nickel and molybde-num result in higher strength and apparent hard-ness. The microindentation hardness of Alloy Awas 214 HV (50 gf) while that of Alloy C (identicalcopper level but with nickel and molybdenum)was 309 HV (50 gf). The microstructure of Alloy Erevealed a fully ferritic structure, which explainsthe lower mechanical properties of this alloy.Columbium, which was added to aid in the pre-cipitation reaction, is also a strong ferrite stabiliz-er and its addition resulted in a fully ferriticmicrostructure. Because of their excellentmechanical properties, Alloy C and Alloy F werechosen as the optimum alloys and were subjectedto further testing.

From a detailed study of aging temperaturesand times, similar to the study performed on 17-4PH, it was concluded that optimal aging for the


TABLE IV. CHEMICAL COMPOSITION OF PM 410LCU HIGH-STRENGTHSTAINLESS STEEL GRADES (w/o)

Alloy P Si Cr Ni Cu Mn Mo Cb

410LCu-A 0.011 0.65 12.10 0.08 1.35 0.09 0.01 —410LCu-B 0.007 0.50 12.81 0.30 2.23 0.06 0.01 —410LCu-C 0.007 0.83 12.65 0.97 2.13 0.05 0.33410LCu-D 0.008 0.77 13.00 0.40 1.50 0.05 0.34 —410LCu-E 0.011 0.71 12.72 0.40 1.48 0.05 0.36 0.36410LCu-F 0.008 0.73 12.77 1.08 3.06 0.06 0.35 — Figure 7. Comparison of green density of experimental alloys


410LCu alloy was 1 h at 538°C (1,000°F). A com-parison of as-sintered and aged tensile properties,apparent hardness, and impact energy is given inTable VI. As expected, aging led to improvementsin hardness and tensile strength of approximately15% to 20%. Both alloys also exhibit unusualbehavior during the aging process. As the strengthand hardness increase during aging, the ductility

and impact toughness of the two alloys improves. An examination of the microstructures of

410LCu-C and 410LCu-F in the aged conditionreveals that both are a mixture of ferrite andmartensite (Figure 8). In an earlier paper it wasshown that a dual phase microstructure is formedwith the correct balance of austenite and ferritestabilizers.9 At the normal sintering temperatures


TABLE V. MECHANICAL PROPERTIES OF SINTERED HIGH-STRENGTH PM STAINLESS STEELS

Alloy 0.20% Offset UTS TRS Apparent Hardness Elongation(103 psi) (MPa) (103 psi) (MPa) (103 psi) (MPa) (HRB) (%)

410LCu-A 57 392 80 550 182 1,252 84 7.5410LCu-B 58 399 79 544 186 1,280 82 5.2410LCu-C 81 557 105 722 243 1,672 94 3.2410LCu-D 55 378 75 516 193 1,328 84 8410LCu-E 59 406 65 447 146 1,004 75 10410LCu-F 87 599 113 777 318 2,188 102 2.8

TABLE VI. SINTERED AND AGED PROPERTIES OF 410LCU PM STAINLESS STEELS


410LCu-C Sintered 81 557 105 722 52 3.2 82 61410LCu-C Aged 100 688 121 832 57 5.1 93 69

410LCu-F Sintered 87 599 113 777 54 2.8 40 30410LCu-F Aged 116 798 137 943 60 3.7 48 36

Figure 8. Representative microstructures:(a) Alloy C (microindentation hardness ofmartensite 372 HV (50 gf)), (b) Alloy C, (c) Alloy F (microindentation hardness ofmartensite 250 HV (50 gf)), and (d) Alloy F. OM

(a) (b)

(c) (d)


for stainless steels (~1,260°C (2,300°F)), when thechemistry is correctly balanced, the microstruc-ture consists of a mixture of ferrite and austenite.Upon cooling to room temperature, the austenitetransforms to martensite and the finalmicrostructure consists of ferrite and martensite.Copper in the alloy should promote the formationof high-temperature austenite, which, upon cool-ing, transforms to martensite. However, as thecopper precipitates, it leaves areas in the matrixdepleted of copper and it is in these areas thatferrite can form. During aging, the precipitatesharden and strengthen the alloys and the ferriteis tempered, improving both ductility and impacttoughness, and imparting a unique set ofmechanical properties to this alloy.

The properties of the two new 410LCu alloysare compared with SS-410-90HT in Table VII. Ithas been shown that stainless steels with a dual-phase microstructure (martensite+ferrite) havehigher tensile properties than SS-410-90HT.9 Inaddition, the ferrite in the microstructure pro-motes ductility, and precipitation from the copperadds additional strength. In effect, the develop-mental alloys are superior in mechanical proper-ties because they are dual-phase precipitation-hardening alloys.

In the wrought stainless steel industry, dual-phase stainless steels were developed as areplacement for weathering steels. The UNS

J91151 alloy was developed for moderate corro-sion resistance, and the addition of copper was, ingeneral, thought to be beneficial in terms of corro-sion resistance. There are numerous applicationsthat are compatible with less-severe corrosiveconditions, and, in such cases, ferritic stainlesssteels are preferred over the more expensiveaustenitic stainless steels.

SS-410-90HT and Alloy C were subjected tosalt-spray testing following ASTM Standard B117-03. Figure 9 shows the condition of the testspecimens after 240 h of exposure. Clearly the410LCu alloy shows superior performance in thistest. Although both alloys exhibit rust (within thefirst 24 h), 410LCu appeared to remain unalteredafter the initial coating of rust was formed. Incontrast, SS-410-90HT continued to rust at aconstant rate.

FATIGUE BEHAVIOR OF PM 17-4 PH AND410LCU ALLOYS

Fatigue tests were performed using PM 17-4 PHand the two new PM 410LCu grades (Alloy C andAlloy F). The results of these tests, in terms of the90% survival limit, are compared with other stain-less steel fatigue data by Shah et al.10 in Figure10. The latter study compared the fatiguestrength of various stainless steels as a function


TABLE VII. PROPERTIES OF PM 410LCU AND PM 22-410-90HT


SS-410-90HT 52 358 92 633 49 4.9 39 29410LCu-C Aged 100 688 121 832 57 5.1 93 69410LCu-F Aged 116 798 137 943 60 3.7 48 36

Figure 9. TR bars subjected to salt-spray testing: (a) SS-410-90HTand (b) Alloy C

Figure 10. Fatigue-endurance limit (for 90% survival) as a function of tensilestrength for various PM stainless alloys


of tensile strength. 17-4 PH at a sintered density of 6.98 g/cm3

exhibited a fatigue strength comparable to that ofSS-410-90HT. With high sintering temperatures,and a finer particle-size distribution, it can beexpected to out-perform this alloy. The excellentfatigue response of the PM 410LCu alloy appearsto be related to its high tensile strength. In gener-al, fatigue-crack propagation rates in PM steelsare high and the fatigue limit is dictated by crackinitiation rather than by crack propagation. Thus,resistance to crack initiation increases as the ten-sile strength increases. Both the 410LCu alloyshave high tensile strengths, and therefore highfatigue-endurance limits. It appears that the addi-tion of copper, along with the addition of nickeland molybdenum, leads to harder martensite,which in this case has a positive effect on fatiguestrength. Table VIII lists the fatigue-endurancelimits for 50% and 90% survival.

CONCLUSIONS• 17-4 PH stainless steel parts, which have his-

torically been produced by metal injectionmolding, can be produced by conventional PMpress-and-sinter operations.

• The mechanical properties of PM 17-4 PH canbe improved by utilizing a finer particle-sizedistribution, high sintering temperatures andlong sintering times.

• The corrosion resistance of PM 17-4 PH issimilar to that of 304L, when processedunder similar conditions.

• A lean precipitation-hardening grade, PM410LCu, has been developed for applicationsthat require high strength and toughness,but moderate corrosion resistance.

• The PM 410LCu alloy has a unique combina-tion of high strength, high toughness and

fatigue resistance. This is attributed to itsmicrostructure, which is dual phase and pre-cipitation hardened.

• PM 410LCu is a cost-effective alloy for appli-cations that require high strength and moder-ate corrosion resistance, such as pump partsand pump housings.

REFERENCES1. L.H. Van Vlack, Elements of Materials Science and

Engineering, Sixth Edition, Addison Wesley PublishingCompany, Reading, MA, 1989, pp. 304–309.

2. L. Zubek, “A Technical Review of Precipitation HardeningGrades”, Spring Manufacturers Institute, Oak Brook, IL,2006, pp.14–16,

3. K.A. Green, “PIM 17-4PH Actuator Arm for AerospaceApplications”, Advances in Powder Metallurgy andParticulate Materials, compiled by C.L. Rose and M.H.Thibodeau, Metal Powder Industries Federation,Princeton, NJ, 1999, vol. 5, pp. 119–130.

4. M.K. Bulger and A.R. Erickson, “Corrosion Resistance ofMIM Stainless Steels”, Advances in Powder Metallurgy andParticulate Materials, compiled by A. Neupaver and C.Lall, Metal Powder Industries Federation, Princeton, NJ,1994, vol. 4, pp. 197–215.

5. H. Kyogoku, H. Nakayama, H. Jinushi and K. Shinohara,“Microstructures and Mechanical Properties of SinteredPrecipitation Hardening Stainless Steel Compacts byMetal Injection Molding”, Advances in Powder Metallurgyand Particulate Materials, compiled by R. McKotch and R.Webb, Metal Powder Industries Federation, Princeton, NJ,1997, vol. 3, part 18, pp. 135–144.

6. J.A. Larson and R.B. Fischer, “Precipitation HardeningChromium Steel Casting Alloy”, U.S. Patent No.4,326,885, April 27, 1982.

7. J.H. Reinshagen and J.C. Witsberger, “Properties ofPrecipitation Hardening Stainless Steel Processed byConventional Powder Metallurgy Techniques”, ibid. refer-ence no. 4, vol. 7, pp. 313–323.

8. R.J. Causton, T. Cimino-Corey and C.T. Schade,“Improved Stainless Steel Process Routes”, Advances inPowder Metallurgy and Particulate Materials—2003, com-piled by R. Lawcock and M. Wright, Metal PowderIndustries Federation, Princeton, NJ, 2003, part 2, pp.1–13.

9. A. Lawley, E. Wagner and C.T. Schade, “Development of aHigh-Strength Dual-Phase P/M Stainless Steel”, Advancesin Powder Metallurgy and Particulate Materials—2005,compiled by C. Ruas and T. Tomlin, Metal PowderIndustries Federation, Princeton, NJ, 2005, part 7, pp.78–89.

10. S.O. Shah, J.R. McMillen, P.K. Samal and L.F. Pease,“Mechanical Properties of High Temperature Sintered P/M409LE and 409LNi Stainless Steels Utilized in theManufacturing of Exhaust Flanges and Oxygen SensorBosses”, SAE Paper No. 2003-01-0451, SAE International,Warrendale, PA, USA, 2003. ijpm


TABLE VIII. ROTATING BENDING-FATIGUE PROPERTIES: 50%AND 90% ENDURANCE LIMITS

Alloy Fatigue-Endurance Limits

50% 90%MPa (103 psi) MPa (103 psi)

410LCu-C Aged 337 (49) 324 (47)410LCu-F Aged 310 (45) 303 (44)


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The new Standard 35, Materials Standards for Metal Injection Molded Parts – 2007 Edition is themost comprehensive standard to date encompassing all facets of the MIM industry. Make sure that yourquality assurance/laboratory staff and your sales and marketing personnel/representatives have the lat-est edition of this standard. Order enough for your own company use and for free distribution to yourexisting and potential customers. Keep a supply handy for future trade shows, plant visits, etc.

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MPIF STANDARD 35, MATERIALS STANDARDS FOR METAL INJECTION MOLDEDPARTS—2007 EDITION

NEW

To Order: FAX:609-987-8523, Phone: 609-945-0009, E-mail: [email protected] or visit www.mpif.org


ADVERTISERS’INDEX

Need more information on products or services seen in this issue? Complete the form below and fax to the advertiser(s) of your choice. Fax numbers are listed in the advertisers’ index above.

To:___________________________________ Fax #: ____________________________________________________________________

Company: _______________________________________________________________________________________________________

Please send me more information on: __________________________________________________________________________

__________________________________________________________________________________________________________________

as advertised in the __________ issue of the International Journal of Powder Metallurgy.

Please send information to:

Name: Title:______________________________________________________________________________________________________

Company: _______________________________________________________________________________________________________

Address: _________________________________________________________________________________________________________

City:____________________________ State:_______________ Postal Code: ____________________________________________

Country: _________________________________________________________________________________________________________

Phone:___________________ Fax:___________________ E-Mail: ______________________________________________________

ADVERTISER’S REQUEST FOR INFORMATION FAX FORMinternational journal of

powdermetallurgy

ACUPOWDER INTERNATIONAL, LLC________________(908) 851-4597 ______www.acupowder.com ______________________32

AMETEK SPECIALTY METAL PRODUCTS_____________(724) 225-6622 ______www.ametekmetals.com ___________________13

ARBURG GmbH + Co KG _________________________(860) 667-6522 ______www.arburg.com __________________________4

ASBURY CARBONS _____________________________(908) 537-2908 ______________________________________________30

CLEVELAND VIBRATOR COMPANY/HK TECHNOLOGY __(216) 241-3480 ______www.clevelandvibrator.com_________________25

CM FURNACES, INC. ____________________________(973) 338-1625 ______www.cmfurnaces.com ______________________7

HOEGANAES CORPORATION ______________________(856) 786-2574 ______www.hoeganaes.com______INSIDE FRONT COVER

INCO SPECIAL PRODUCTS _______________________(201) 848-1022 ______www.incosp.com _________________________16

NORILSK NICKEL _______________________________(+ 7 495) 785 58 08___www.norilsknickel.com _____________________8

NORTH AMERICAN HÖGANÄS INC._________________(814) 479-2003 ______www.nah.com_____________________________2

OSRAM SYLVANIA ______________________________(570) 268-5157 ______www.sylvania.com ________________________10

OSTERWALDER POWDER COMPACTING SYSTEMS ____(513) 936-9008 ______www.osterwalder.com ______________________6

PRINCETON ONE _______________________________(440) 243-4868 ______www.princetonone.com ____________________14

PVA MIMtech, LLC, ELNIK SYSTEMS DIVISION _______(973) 239-6066 ______www.elnik.com___________________________37

SCM METAL PRODUCTS, INC. ____________________(919) 544-7996 ______www.scmmetals.com _______INSIDE BACK COVER

QMP _________________________________________(734) 953-0082 ______www.qmp-powders.com ___________BACK COVER

ADVERTISER FAX WEB SITE PAGE

Manufacturing Sites

• Research Triangle Park, North Carolina USA• Suzhou, China

Tel: 919-544-8090 • www.SCMmetals.com

SCM's products include:

• Copper, Tin and Bronze Premix Powders • Prealloyed Bronze and Brass Powders • Copper Base Infiltrating Powders • High Green Strength Copper Powders• Copper Oxides • Copper Base Catalyst Powders• Cubond® Furnace Brazing Pastes

North CarolinaUSA

SuzhouChina

e-ijpm: vol. 43/4s3. · pdf filep.k. samal h.i. sanderow d.w. smith, fapmi j.e. smugeresky r....

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