POWDER METALLURGY AND SOLID STATE PROCESSING OF ARMSTRONG TITANIUM AND TITANIUM ALLOY

POWDERS

William H. Peter (Bill), Craig A. Blue, Jim O. Kiggans, John D.K. Rivard*Oak Ridge National Laboratory, Oak Ridge, TN

Charlie Yu, Clive Scorey*, Joe Capone, and John McKernonAMETEK Specialty Metal Products, Wallingford, CT

Bill ErnstInternational Titanium Powder (ITP), Lockport, IL

T. James DorschBAE Systems, Santa Clara, CA

ITA Annual Conference 2007, Orlando, FLOctober 7-9 2007

* Formerly with Organization

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Land Combat Systems -P

IntroductionIntroduction• Ti Offers Many Attractive Properties.

PegasusBAE Systems

− High Specific Strength.− Good Elevated Temperature

Properties.− Excellent Corrosion Resistance.− Allows for Damage Tolerant

Design.• Cost and Availability Are a Concern

− Lead Times 12 to 18 MonthsLead Times 12 to 18 Months− Plate Prices of $35 to $50/Lb

• Cost Limits Application to Specific Markets. Critical Need for Basic Research

Heat Exchangershttp://www titanmf com• Critical Need for Basic Research

into Lower Cost Refining and Processing

• New Low Cost Titanium Powders Could Initiate a Paradigm Shift in

http://www.titanmf.com

Biomedical -Knee Replacement

Could Initiate a Paradigm Shift in Titanium’s Use in Industry

• Oak Ridge National Laboratory is Working with Industry to Develop the Necessary PM Technologies to

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787 Boeinghttp://www.boeing.com/commercial/787family/index.html

the Necessary PM Technologies to Consolidate the New Low Cost Ti Powders

Conventional Technology Compared to DARPA Funded Armstrong Processg

• Kroll Process− Mg Reduction of TiCl4

• Armstrong (ITP) Process− Reduction of TiCl4 in Na Liquid Loop

− Batch Process− Requires Acid Leaching and

Vacuum Arc Remelting− Finally Milled into Desired Product

− Continuous Process− Ability to Produce Prealloyed Powder− Price of Powder Competitive with Kroll

Sponge

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y− PM Approach Not Attractive

Except for Specialty Components

g− PM Approach Economically Attractive− Thousands of Pounds of Powder Have

Been Produced

International Titanium Powder (ITP),Armstrong Process Titanium Powder

A 100 lb Drum of ITP Powder Received by ORNL

• New 4 Million Pound Titanium Plant Under Construction in IL, U.S.

• Chemical Analysis of Powder Has Fallen within ySpecification− Grade 2 for CP Ti (e.g., 0.12 to 0.21 wt. % O)− Grade 5 for Ti-6Al-4V

• Typical Powder Particle Size Range: 150 to 2000 µm Armstrong Titanium Powder• Typical Powder Particle Size Range: 150 to 2000 µm with a mean size of 400 µm

• Energy Consumption for Reduction Process− 50 Year Old Conventional Kroll Process = 355

MBtu/ton [Batelle-Columbus Laboratories, (1975). Energy use

Armstrong Titanium Powder Morphology

[ , ( ) gypatterns in metallurgical and non-metallurgical mineral processing]

− Armstrong Process = 165 MBtu/ton− A 53.4% Reduction in Energy Consumption.

• “Low Cost” Powder Allows for:− Near Net Shape Consolidation− Compositing and Layered or Engineered

Structures− Ability to Use Beneficial Elements Not Possible

in Conventional Processing (E g Small

International Titanium Powder 4 Million Pound Per Year Plant to be Finished in 2008

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in Conventional Processing (E.g., Small Additions of Boron ))

Processing Processing –– Cost Break Down of Cost Break Down of F b i ti 1” Ti Pl tF b i ti 1” Ti Pl tFabricating 1” Ti PlateFabricating 1” Ti Plate

• ITP “Low Cost” Ti Powders Developed in DTi ProgramDeveloped in DTi Program Address 25% of 1” Plate Fabrication Costs

• The Secondary Processing y gor Processing into Finished Product (62% VAR and Milling) Needs to Be Add dAddressed

• Conventional Milling Operations, Scrap Generated: 40 to 60%

Cost Break Down to Produce 1” Thick Titanium Plate Using Kroll – VAR Melted Titanium

Generated: 40 to 60%• PM Approach with ITP

Powder Ability to Reduce Scrap to Less Than 10%

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Hartman, A.D. et al. JOM September 1998. pp. 16-19Scrap to Less Than 10%

Development of Multiple PM Processes for Economical ProductProcesses for Economical Product

PlateForged, PIF, Hot Roll, HIP

Near Net ShapesHot Pressed, Forged, Press+Sinter

Bars and RodSheetRoll CompactedBars and Rod

Extrusionp

Low Cost Ti Powder

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Vacuum Hot Pressing (VHP) of Vacuum Hot Pressing (VHP) of ITP CP Ti and TiITP CP Ti and Ti--6Al6Al--4V4V –– PlatePlateITP CP Ti and TiITP CP Ti and Ti 6Al6Al 4V 4V Plate Plate and Near Net Shape Productionand Near Net Shape Production

VHP CP Ti

As VHP microstructures

VHP Ti-6Al-4V

• Armstrong Ti and Ti-6Al-4V powder were vacuum hot pressed.

• Interstitial Levels of ITP CP Ti, VHP

As VHP microstructures

Sample YS [MPa]

UTS [MPa]

Ductility [%],

Produced Plate within Specification• Mechanical testing, microstructures,

and chemical analysis comparable to ti l ht ti

[MPa] [MPa] [%]

ITP VHP CP Ti900°C/30min

517 617 20.7

CP Ti Grade 2 345 448 20.0

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conventional wrought properties. • Rivard, J.D.K. et al. JOM 57, 11, 2005.

pp. 56-60

ITP VHP Ti-6Al-4V 950°C/60min 963 994 13.8

Ti-6Al-4V Grade 5 828 897 10.0

Fatigue Testing Procedure for VHPTi 6Al 4V Pl tTi-6Al-4V Plate• Ti-6Al-4V ITP Powder Pressed

at 1 050oC 1 hour in Vacuumat 1,050oC, 1 hour in Vacuum• Initial powder had slightly high

oxygen compared to ASTM G d 5 (O 0 23 t %)Grade 5 (O2 ~ 0.23 wt. %).

• Consolidated Plate: O2 ~ 0.25 wt. %, 200 ppm pickup, pp p p

• Hot Rolled VHP Plate (850oC, 50% reduction)

• Round Bar Specimen with 1/8”• Round Bar Specimen with 1/8 testing diameter, less than half hot rolled gauge thicknessR ti / 0 1

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• R ratio,smin/smax = 0.1• Frequency = 10 Hz

Ongoing Fatigue Results

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• Preliminary Results of Specimens Taken Normal to Rolling Direction Indicate ITP VHP Ti-6Al-4V Samples Are Comparable to Conventionally Pressed and Forged Powders

DTi “Low-Cost” Ti-6Al-4V Plates Show Comparable Ballistic Results to Conventional Wrought Plate

Distribution Statement "A" (Approved for Public Release, Distribution Unlimited)

• VHP Consolidated Plate (950oC and 1,050oC)•Ballistics testing performed at BAE Systems using MIL-DTL-46077G spec.

( pp , )

p– 0.30 cal APM2 (same as 7.62mm AP).– Velocity increased until 0.5” plate was penetrated.

• 1,050oC Plate - Estimated V50 ~2,037 fps, within 2% of conventional wrought Ti-6Al-4V properties for specific thickness of plate (ref: MIL-DTL-46077 spec).

– No cracking.G d d f ti /d tilit ( t #4 B k)– Good deformation/ductility (note: #4, Back).

– Extremely limited spalling.• 950oC Plate – Estimated V50 >2,097 fps, within 0.3% of specification for specific plate thickness WITHOUTspecification for specific plate thickness WITHOUTpenetration. V50 test could not be completed due to insufficient test area.•Low-cost Ti-6Al-4V plate exhibited comparable Front and back of V50 tested

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performance to wrought plate.f 50

1,050oC VHP Ti-6Al-4V Plate

Development of Cold Isostatic Pressing / Pneumatic Isostatic Forging (CIP/PIF) Process

CIP/PIF Near Net Shape Stainless Forging (CIP/PIF) Process

• Necessity for Cost Effective Method of Producing Plate and

Steel Components

CIP/PIF TubesgNear Net Shape Components

• PIF AMETEK Patented Process – Rapid Gas Pressurization (1 to 2 Minutes) VHP ITP Ti-6Al-4V CIP/PIF ITP Ti-6Al-4V

CIP/PIF Tubes

2 Minutes)• Very Preliminary CIP/PIF Work

Performed with AMETEK Shows PromiseB lli ti R lt H B• Ballistic Results Have Been Comparable to Wrought Plate

• Mechanical Evaluation OngoingDescription VHP CIP/PIFDescription VHP CIP/PIF

% of Theoretical Density

99.4% 99.6%

Oxygen Pickup 0.02 0.04

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(wt. %)

Microstructure Equiaxed Equiaxed

Hardness (VHN) 343 +/- 31.9 346 +/- 27.3 CIP/PIF ITP Ti-6Al-4VVHP ITP Ti-6Al-4V

Ti Processing Ti Processing –– ExtrusionExtrusion• Mechanical testing and microscopy

As-extruded Ti

ORNL, 1250 ton -extrusion press

Mechanical testing and microscopy

As-extruded Ti-6Al-4VExtruded CP Ti Tensile Bars

Sample* YS [MPa] UTS [MPa] Ductility [%]

Extruded Ti 407 552 17.0Ti Grade 2 345 448 20.0

* Insufficient Ti-6Al-4V powder was available at the time of initial extrusion demonstration. Recent Increase in ITP Ti-6Al-4V powder production will enable ORNL to produce Ti-6Al-4V extrusions and

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p ptest bars in the near future.

Roll Compaction of Armstrong (ITP) Derived Ti PowdersRoll Compaction of Armstrong (ITP) Derived Ti PowdersRoll Compacted Rolls of

Nickel Sheet CommerciallyNickel Sheet Commercially Produced at AMETEK with

over 50 years experience

• Collaborative Effort Between ORNL and AMETEK to Develop Roll Compaction Manufacturing Technology for Low Cost Titanium PowdersTechnology for Low Cost Titanium Powders

• Both Commercially Pure Ti and Ti-Al-V Alloys Have Been Roll Compacted

• ITP Powder Has Resulted in:− Green Densities of 60 to 70%

Diagram of Roll Compaction Sheet Production with AMETEK Roll

Compaction MillGreen Densities of 60 to 70%− Sheet Widths of 15” (or Greater) and Proof of

Continuous Production (Coils of 28’ in length)• Solid State Sheet Processing After Roll

Compaction: Sinter, Cold Roll, And Anneal Lead to Fully Consolidated Sheet (>99%)

Compaction Mill

Fully Consolidated Sheet (>99%)• Initial Trial Resulted in High Strength/Low Ductility

Due to High Oxygen• However, Further Development Has Led to

Acceptable Oxygen Levels: 200ppm Pickup or

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p yg pp pLess During Roll Compaction, and Less Than 800ppm Pickup After Full Consolidation –Mechanical Testing Ongoing

Distribution Statement “A” (Approved for Public Release, Distribution Unlimited) Roll Compacted Titanium Sheet

Results of ITP Ti Press+Sinter

ITP Ti-6Al-4V Press+ Sinter Samples with Microstructure

• ITP CP Ti and Ti-6Al-4V Powders − Pressed to Pressures of 100 ksiPressed to Pressures of 100 ksi− Sintered at Temperatures 1,100oC and 1,300oC

• Densities for given loads and temperatures:− Up to 90% theoretical for CP Ti− Up to 95% theoretical for ITP Ti-6Al-4V

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− Up to 95% theoretical for ITP Ti-6Al-4V • < 300 to 400 ppm pickup in oxygen• Further Work in Progress Low Cost Ti “Green” Near

Net Shape Component

ConclusionsConclusions• Low Cost Titanium Powders Are Now Produced That Could Cause a

P di Shift i th U f Tit i f I d t d Oth A li tiParadigm Shift in the Use of Titanium for Industry and Other Applications. • Further Development in Solid State Consolidation of the New Titanium

Powders Is Required to Realize the Most Economical Components and Penetrate New Markets.

• Vacuum Hot Pressed Plates and Extruded Bar of the Low Cost Titanium Have Been Produced with Tensile Properties that Meet ASTM Specifications.

• Very Preliminary Ballistic and Fatigue Results are Encouraging• Very Preliminary Ballistic and Fatigue Results are Encouraging.

Future WorkFuture Work• Further Development of Existing Work Shown

•Comprehensive Mechanical Testing for Various PM Approaches (CP Ti, Ti-6Al-4V)•PM Development of Other Low Cost PowdersPM Development of Other Low Cost Powders as Made Available

• Currently Fabricating 200lb Military Component from ITP PowdersW l A F th C ll b ti t All f

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• Welcome Any Further Collaboration to Allow for the Penetration of Titanium Into New Markets

Heat Treatment and Rolling of Ti-6Al-4V Plates for 200lb

Military Component

Acknowledgements• The Research Presented Was Made Possible by the y

Support of:− Department of Energy, Office of Energy Efficiency and

Renewable Energy, Industrial Technologies Program (DOE-EERE ITPEERE-ITP

− Department of Energy, Office of Energy Efficiency and Renewable Energy, FreedomCar & Vehicle Technologies Program- Weight Reduction of Heavy Vehicles Program (DOE-EERE F d CAR)EERE-FreedomCAR)

− Defense Advanced Research Programs Agency (DARPA), Defense Science Office (DSO), DARPA’s Initiative in Titanium Program (DTi)g ( )

• I would like to thank the following individuals:− Oak Ridge National Laboratory, Phil Sklad, Evan Ohriner, Steve

Nunn, David Harper, Donny McInturff, Ed Hatfield, and Kevin Harper− International Titanium Powder, Stanley S. Borys, Lance Jacobsen,

and Dariusz Kogut− AMETEK, Joe Capone, Greg Nelson

Taras Lyssenko

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− Taras Lyssenko

Questions?