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Mitglied der Helmholtz-Gemeinschaft Powder metallurgically produced tungsten fiber reinforced tungsten composites 15 th November 2017 | Y.Mao a , J.W.Coenen a , J.Riesch b , S.Sistla c , J.Almanstötter d , B.Jasper a , L.Raumann a , A.Litnovsky a , F.Klein a , M.Rasinski a , A.Terra a , T.Höschen b , H.Gietl b,e , M. Bram f , J. Gonzalez-Julian f , Ch.Linsmeier a and C.Broeckmann c a Institut für Energie und Klimaforschung Plasmaphysik, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany b Max-Planck-Institut für Plasmaphysik, 85748 Garching b. München, Germany c Institut für Werkstoffanwendungen im Maschinenbau (IWM), RWTH Aachen University, 52062 Aachen, Germany d OSRAM GmbH, SP PRE PLM DMET, Mittelstetter Weg 2, 86830 Schwabmünchen, Germany e Technische Universität München, Boltzmannstrasse 15, 85748 Garching, Germany f Institut für Energie und Klimaforschung - Materials Synthesis and Processing, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
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Page 1: Powder metallurgically produced tungsten fiber reinforced ...

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Powder metallurgically produced tungsten fiber reinforced tungsten

composites

15th November 2017 | Y.Maoa, J.W.Coenena, J.Rieschb, S.Sistlac, J.Almanstötterd, B.Jaspera, L.Raumanna, A.Litnovskya, F.Kleina, M.Rasinskia,

A.Terraa, T.Höschenb, H.Gietlb,e, M. Bramf, J. Gonzalez-Julianf, Ch.Linsmeiera and C.Broeckmannc

a Institut für Energie und Klimaforschung – Plasmaphysik, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany b Max-Planck-Institut für Plasmaphysik, 85748 Garching b. München, Germany c Institut für Werkstoffanwendungen im Maschinenbau (IWM), RWTH Aachen University, 52062 Aachen, Germany dOSRAM GmbH, SP PRE PLM DMET, Mittelstetter Weg 2, 86830 Schwabmünchen, Germany eTechnische Universität München, Boltzmannstrasse 15, 85748 Garching, Germany f Institut für Energie und Klimaforschung - Materials Synthesis and Processing, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany

Page 2: Powder metallurgically produced tungsten fiber reinforced ...

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20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Tungsten in fusion reactor

Extreme conditions • High ion/neutron flux,

• high heat load (≥ 10 MW/m2)

• temperature

• thermal stresses/cycling

• …

Tungsten features unique property combination • High melting point, Tmelt = 3380 °C

• High thermal conductivity, λ = 167 W/mK,

• High temperature strength and creep resistance, • Low sputter yield, …

ITER Organization ITER Organization

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Crack formation

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

• Intrinsic brittleness of tungsten material

• Thermal heat load at the divertor: thermal

stress and thermal fatigue

G. Pintsuk et al. / Fusion Engineering and Design 88 (2013) 1858– 1861 1861

Neutron embrittlement

ITER Material Properties Handbook, ITER Document No.G74 MA 16, 2005.

A damage resilient material is required

H Bolt, et al; Journal of Nuclear Materials, Volumes 307–311, Part 1, 2002, Pages 43-52

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Fiber reinforced composites

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Energy dissipation mechanisms:

a – pull-out of fibers

b – pull-out of matrix elements

c – crack deflection at interface

d – crack bridging by fiber

e – crack meandering at interf.

Pseudo ductile behavior

[based on Chawla 1993]

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20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Tungsten fiber reinforced tungsten composites

(Wf/W)

Fiber

• High strength/ductility, temperature stability

commercial, drawn tungsten wire (Osram GmbH)

Interface

• Optimum bonding, stability: e.g. oxide ceramic (Yttria)

Matrix

• Interface/fiber integrity, fiber architecture, density

Chemical vapor deposition (CVD-Wf/W)

Powder metallurgy (PM-Wf/W)

Mature industrial production route High production rate Easy to apply alloy production

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Manufacturing process and microstructure

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

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20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Raw materials

Powders:

5 µm average

particle size

Fibers:

- length: 2.4 mm

- diameter: 0.24 mm

Ductile fiber with extremely high

tensile strength up to ~3000 Mpa

1 µm

Elongated grain structure

-Zhao, Microstructure, mechanical behaviour and fracture of pure

tungsten wire after different heat treatments, 2017

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20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Process

Tungsten fiber coating with

2.5 µm Y2O3 thin film by Magnetron sputtering

Fiber and powder mixing with 30%

fiber volume fraction

PM process

Consolidation:

Field assisted sintering technology (FAST)

Hot Isostatic Pressing (HIP)

Tungsten fiber reinforced tungsten

composite

FAST

HIP

2µm

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20.11.2017

Parameter and microstructure

Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

FAST HIP

Parameter FAST HIP

Temperature 1900°C 1600°C

Pressure 60 MPa 200 MPa

Time 4min 2h

Heating rate 200K/min 10K/min

Relative

density ~94% ~98%

7

• Dense material • Random fiber distribution • Yttria interface between fiber and matrix

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Pseudo ductile behavior of the PM produced Wf/W

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

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Pseudo ductile behavior

-pre-notched 3 point bending test

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Qualitative measurement of the fracture behavior

Diamond wire cutting →razor blade polishing

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20.11.2017

Pseudo ductile behavior

Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Pure W FAST HIP

The PM produced Wf/W samples are able to show a pseudo-ductility behavior at RT. The improved resistance against

fracture relies on the energy dissipation mechanisms like fiber pull-out, crack bridging by the fibers and crack deflection.

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Carbon influence on Tungsten fiber after FAST process

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

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Brittle tungsten fiber

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

• Cleavage transgranular fracture

• Tungsten fibers after FAST process are brittle fibers

Our principle works, even with brittle fibers and matrix, the material still behave pseudo ductile. We have fiber embrittlement during the production of the composite.

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Carbon embrittlement

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Ductile fiber Brittle fiber 1220 °C

annealing on graphite sheet

annealing on Mo bed plate

Ductile fiber Ductile fiber 1220 °C

-Marine Ilg, Diplomarbeit, 2016

• Very small amount (Dozens of ppm) of

carbon impurities will increase DBTT of

tungsten.

• “carbon embrittlement results from an

interaction between carbon atoms and

dislocations within the tungsten lattice”

Carbon content (ppm) 8 36 60

DBTT (°C) 232 368 415

-Stephens JR. Effects of interstitial impurities on the low-temperature

tensile properties of tungsten; 1964.

1900 °C

Using W foil to separate the

tungsten and the graphite

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Wf/W with ductile fiber

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Displacement (a.u.)

Forc

e (a

.u.)

Displacement (a.u.)

Forc

e (a

.u.)

• Fiber necking; knife edge shape fracture surface Wf/W with brittle fiber

Wf/W with Ductile fiber Wf/W with brittle fiber

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Conclusion

20.11.2017

• High density Wf/W composites are able to

be produced by powder metallurgy

process.

• The optimized Wf/W show significant

increasing of crack propagation

resistance; even with brittle fibers

• Tungsten is very sensitive to carbon

contamination; very little amount of C can

cause fiber embrittlement.

Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

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Monoblock

20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

Coenen PSI, 2016 Rome

ITER Material Properties Handbook, ITER Document No.G74 MA 16, 2005.

G. Pintsuk et al. / Fusion Engineering and Design 88 (2013) 1858– 1861 1861

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20.11.2017 Yiran Mao – Second Technical Meeting on Divertor Concepts, 13-16 Nov, Suzhou

200 µm

Self passivating tungsten alloy (smart alloy)

pure W sample W-11.6Cr-0.6Y alloy

Oxidation test: 80 vol.% Ar + 20 vol. % O2 at 1 bar and 1000oC

Normal operation →

Tungsten (W)

•High melting point

•Low erosion yield

Accident:

•Loss of cooling

•Air ingress

•No W

evaporation/sublimation

W, Cr, Y


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