ADDITIVE MANUFACTURING OF COPPER ALLOYS IN POWDER …

T. BAFFIE, C.SALVAN, P.LASSEGUE, M.ROUMANIE, L.BRIO TTET, L.GUETAZ, E. DE VITO, PE. FRAYSSINES, G.ROUX, L.AIX ALA

CEA-LITEN, Grenoble, France

ADDITIVE MANUFACTURING OF COPPER ALLOYS IN POWDER FORM

Colloque i3D Métal, December 13-14 th 2018, Orsay, France

[email protected]

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CEA – LITEN

Additive Manufacturing of Copper alloys in powder form | T.BAFFIE et al.

• Part of the Technological Research Direction of CEA• Dedicated to Renewables Energies (Solar, Hydrogen production & storage,

Fuel Cells, Batteries for Electric Cars, Heat exchangers)

• 80% of our funding comes from:• Industrial Bilateral projects• National or European projects

• A few CEA internal collaborations with DEN, LIST/AF H & IRFU-IRFM• Contribution to FADIESE AM database project

• Experience in Metal AM• Team of 20 persons• Al alloys (3 PhD, 2 projects), 316L (4 projects, 1PhD), Ni alloys (2 projects),

HEA (1 PhD), Magnetics (FeSi, NdFeB, FeCo, SmCo) and Cu alloys (1 PhD, 1 post-doc)

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POUDRINNOV PLATFORM DEDICATED TO POWDERS


• Opened in 2012 • Investment ≈ 2,5 M€

• An area of more than 800 m 2 focused on • Near net shape manufacturing technologies

• MIM, SPS, HIP• Polymers, Ceramics & Metals• New materials & feedstocks development

• Extended area in 2014• Additive Manufacturing (L-PBF, SLA, Jetting, FDM)• Permanent Magnets manufacturing pilot line

• Three new L-PBF machines in 2018-2019

1st L-PBF 2014

2nd L-PBF 2018

3rd L-PBF 2019

1st SLA 2014

1st FDM 20181st Jetting 2018

4th L-PBF 2019

2nd SLA 2015

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POWDER METALLURGY PROCESSES


@ CEA-LITEN

LMD

10 100 100k1 1 000 1Mk

0,1

1

10

100

Production

Volume

Parts Mass (kg)

MIM

1 000

PMD

HIP

M-BJ

M-FDM, M-SLA

EBM

L-PBF

MIM = Metal Injection MoldingHIP = Hot Isostatic PressingPMD = Plasma Metal DepositionLMD = Laser Metal DepositionL-PBF = Laser Powder Bed FusionM-BJ = Metal Binder JettingM-FDM = Metal Fusion Deposition ModelingM-SLA = Metal StereolithographyEBM = Electron Beam Melting

AM

Traditional

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AM PROCESSES BASED ON METAL POWDERS


Powder-based MetalAM Technologies

Small parts, high complexity

Powder bed

M-BJ L-PBF EBM

Powders in feedstocks,

resins or inks

M-FDM M-Jetting M-SLA

Large parts, lowcomplexity

Powder feed

DED (LMD, PMD) Cold spray

Direct process

Indirect process

Metal Binder Jetting

Laser Powder Bed Fusion

Electron Beam Melting

Metal Fusion Deposition Modeling

MetalStereolithography

Direct EnergyDeposition

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DESCRIPTION OF METAL-POWDERS AM PROCESSES


Laser Powder

Bed Fusion (L-PBF)

Electron Beam

Melting(EBM)

MetalBinder Jetting(M-BJ)

MetalFusion

DepositionModeling(M-FDM)

[HP]

[Bose 2018]

[Arcam]

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DESCRIPTION OF METAL-POWDERS AM PROCESSES


Metal Stereolithography (M-SLA) M-Jetting

Nanoparticles ink

Ink droplets Jetting

Solventevaporation @ each layer

Part sintering at HT°

DED Cold Spray

[XJET]

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COMPARISON OF METAL-POWDERS AM PROCESSES


Processes capabilities Largest parts with L-PBF, SLA+Electroless Smallest parts with M-Jetting Most complex parts with M-BJ, L-PBF Limited complexity with Cold Spray, DED Highest building speed with Cold Spray, M-BJ Highest accuracy M-Jetting, M-SLA Lowest accuracy with M-FDM

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MOTIVATION FOR STUDYING CU ALLOYS BY AM


AGENDA

Needs for several industrial applications

Quite limited data available in literature

No commercial offers in 2016

Interest of Cu alloys Cu alloys by traditional processes Cu powders atomisation Cu parts by powder AM processes Cu alloys by powder-based AM processes L-PBF & M-SLA on Cu @ CEA-LITEN L-PBF on CuCrZr @ CEA-LITEN

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INTEREST OF CU ALLOYS


Large number of grade alloys available in wrought forms Bronze, Cupro-aluminium, Cupro-Nickel, Brass Precipitation-Hardening Cu alloys

Focus on those with High electrical/thermal conductivities and YS > 200 MPa Experience at CEA-LITEN on wrought CuCrZr

[Zinkle 2016]

SA = solutionized and aged

TMT = thermomechanically treated

CW = cold-workedCWA = cold-worked and aged

PM = powder metallurgy (PM)

ann. = annealed

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CU ALLOYS BY TRADITIONAL PROCESSES


Properties Wrought Pure Cu → High σ and λ in annealed state, but low YS Wrought CuAg & CuZr → Lower σ but higher YS Wrought CuCr1Zr & Cu-Al2O3 → Much higher mech. Properties Hipped CuCr1Zr powder → heat treatment suited to ITER specifications MIM → only Cu powder available; low density impacts mech.properties

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CU ALLOYS BY TRADITIONAL PROCESSES


CuCr1Zr shows relatively high mechanical strength at 200-300°C Microstructure after heat treatment

finely dispersed Cu5Zr and pure chromium precipitates Traditional processes limited to relatively low complexity parts

CuCr1Zr solutionized, water quench and aged 475 °C/1 h

[Zinkle 2016]

[Zinkle 2016]

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CU POWDERS ATOMISATION


GA powder producers ECKA TLS (EIGA) UTBM Sandvik Osprey

Grades commercially available Cu-8Sn, Cu-10Sn, Cu-15Sn Cu-10Al, Cu-10Al-5Ni Cu-10Mn-3Ni HC Cu, OFHC Cu CuCrZr CuAg

Main processes Electrolytic process Reduction of Copper oxide Water atomization Gas atomization (GA, VIGA, EIGA)

GA [Erasteel] VIGA [Erasteel] EIGA [Erasteel]

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CU PARTS BY POWDER AM PROCESSES


M-BJ+Sintering: Cu first demonstrators

M-FDM+Sintering: Cu first prototypes; tries to improve final density

Cold-spray: « more than coating » with several demos

P-SLA + Cu Electroless: several large parts for RF applications tested

Spline-Profiled Smooth Horn RF Ku-band Antenna and waveguide transitions [Vorst 2016]

M-Jetting+Sintering: only Ag available; copper under development

M-SLA+Sintering: first pure Cu parts

M-BJ (SS)+Sintering+ Cu Electroless: Cu still under development

EBM: mainly pure Cu for coils and RF devices

More than 1200 induction coils produced [Portoles 2018]

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CU ALLOYS BY POWDER AM PROCESSES


EBM, M-Jetting, M-SLA, M-BJ, Cold Spray, M-FDM: Propertiesavailable from suppliers and literature EBM Cu: The highest σ and λ M-BJ+Sintering Cu: HIP required to reach 90%IACS & 330 W/m.K M-FDM Cu: density needs to be improved M-Jetting & M-SLA Cu: no data in literature yet DED Cu: Cu alloys difficult to process Cold Spray CuCrZr & CuAg: first IACS over 90%

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CU PARTS BY POWDER AM PROCESSES


L-PBF: more and more applications (molds inserts, combustion chambers, coils) and suppliers, but still very little scientific publications

Induction coil (GKN)

Mold insert with channels (Schmelzmetal)

CuCrNb Rocket Thrust Chamber (NASA)

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CU ALLOYS BY POWDER AM PROCESSES


L-PBF: Properties available from suppliers and literature Commercial CuCrZr: data from datasheets (need to be checked); no data

on powder characteristics; data on as-build or on heat-treated samples; no data on heat treatments; σ > 75% IACS and λ > 250 W/m.K

CuCrZr in literature: data on HT° but limited data on properties Cu-0.1Ag: still under developement CuCrNb: Few data available but combustion chamber successfully tested

at NASA

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L-PBF OF CU ALLOYS


Main difficulties with Cu-rich alloys High optical reflectivity at standard laser wavelength High thermal conductivity → Requires high energy densities for melting

Cu alloy Cu

References[Ikeshoji

2018]

[Uhlmann

2018]

[Buchmayr

2017]

Laser power (W) 800 350 370

Part density (%) 96.6 99.99 99.96

CuCrZr

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L-PBF ON PURE CU @ CEA-LITEN


Cu powder Atomised under N2 gas PSD < 45 µm Many satellites

Aspect ratio : D50 = 0.91 Good flowability

Mean avalanche angle = 44° Coherent with Hausner ratio

Densities : True D = 8.88 g/cm3

AD = 5.61 g/cm3

TD = 5.74 g/cm3

Supplier CEA

D10 9.2 µm 10.0 �0.5 µm

D50 26.2 µm 22.5 �0.6 µm

D90 47.8 µm 44.3 � 1.6 µm

Composition (wt%) P O B C Cu

Cu DHP Standard0.015-0.04

99.90

Supplier 0.02 0.02 0.01 <0.05 >99.9

CEAWt.% 0.026 0.021 0.020 0.011 99.92

Std deviation 0.004 0.004 0.002 0.002

[Lassègue 2018]

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L-PBF ON PURE CU @ CEA-LITEN


Cu L-PBF process development P & S variations effect P limited to 480 W Highest density = 8.54 g/cm3 (95.3%)

Outlook Effect of spot size Microstructure and hardness

� ��

�. �. ��

[Lassègue 2018]

BD ρ = 88%

Den

sity

(Arc

him

edes

) %

Volumic Energy Density Ev (J/mm 3)

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M-SLA ON CU @ CEA-LITEN


Same Cu powder as L-PBF study Photoreticulable resin formulation

Able to reticulate under UV LED 365nm 55-56%vol Cu (close to MIM: 55-60%vol) Include dispersant, thixotropic agent & PP Resin stable and suitable viscosity

η = 5-10 Pa.s @ 100 s-1

SLA printing step Layer thickness = 30µm Good adhesion between layers Real printing time = 0.42s Printing speed = 50-100 µm/s

Debinding step DOE on temperature, soaking time & atmosphere Aim: optimize density and C/N/O contents

Sintering step 1050°C - 2h under H2 Shrinkage : 30% in Z; 25% in XY Final density = 94 % C, N, O contents controled

[Roumanie 2018]

Resin formulation SLA printing Debinding & sintering

Part with fiber sections and openings 0.4x0.4mm

C (wt%) N (wt%) 0 (wt%)

Cu powder 0.011 0.001 0.021

Sintered part 0.018 0.002 0.018

SinteredAs-printed

Opt

ical

abs

orba

nce

(%)

Wavelength (nm)

Effect of %PP

| 22Additive Manufacturing of Copper alloys in powder form | T.BAFFIE et al.

L-PBF ON CUCRZR ALLOY @ CEA-LITEN

CuCrZr powder Wrought alloy EIGA-atomised under N2 gas PSD 10-45µm Composition agreed to standard except for Fe

0.02wt% Fe → reduce σ of 5% IACS Mainly spherical particles; a few satellites

Aspect ratio: D50 = 0.96 Bad flowability

Mean avalanche angle = 64° Uncoherent with Hausner ratio

Densities: True D = 8.928 g/cm3

AD = 5.05 g/cm3

TD = 5.68 g/cm3

Wt% Cr Zr Fe Si Other Cu

Supplier 0.742 0.097 O:0.0139 Bal.

CEA 0.723 0.084 0.021 � 0.001 0.038 Bal.

CEA Std dev. (�) 0.045 0.005 0.001 0.0005 0.005

Standard PN-EN10204:2006P

0.5– 1.2 0.03-0.3 0– 0.008 0– 0.1 0.2 Bal.

Supplier CEA

D10 11.4 µm 12.7 �1.3 µm

D50 31.2 µm 25.9 �1.2 µm

D90 48.1 µm 47.5 � 2.0 µm

[Salvan 2018]

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L-PBF ON CUCRZR ALLOY @ CEA-LITEN


CuCrZr L-PBF process development P, S & h variations effect P limited to 270 W Layer thickness = 30µm Highest density = 8.868 g/cm3 (99.4%) Minimum wall thickness = 0.2 mm Columnar grains

Outlook Effect of humidity on powder

XPS analyses vs different storage atmospheres Mechanical, thermal, electrical parts Comparison to forged and HIP

� � 100μ�Building

direction

[Salvan 2018]

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OUTLOOK ON CU ALLOYS BY AM


Two driving technologies: EBM & L-PBF Choice will depend on applications

First Cu-industrial L-PBF parts in 2016

First L-PBF machines with green laser in 2018 Highly expensive But first parts visually convincing

Lack of studies on Links between process parameters, microstructures and properties Post-treatments

Heat treatement effect on properties Surface roughness

Round-robin tests among machines Fatigue, creep and fracture toughness

No standard on Cu AM parts

Commissariat à l’énergie atomique et aux énergies alternatives17 rue des Martyrs | 38054 Grenoble Cedexwww-liten.cea.fr

Établissement public à caractère industriel et commercial | RCS Paris B 775 685 019

Many thanks to :

- CEA/IRFU, CEA/IRFM and Institute CARNOT/EF for financial

support- C.Salvan, P.Lassègue, N.Tissot& M.Roumanie for supplying their

data.

THANKS FOR YOUR ATTENTION !

[email protected]

CEA-LITEN « Metal Additive Manufacturing » team

We are opened to collaborate or work with you !

CEA-LITEN « Metal Additive Manufacturing » team

We are opened to collaborate or work with you !

ADDITIVE MANUFACTURING OF COPPER ALLOYS IN POWDER …

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