Antusch, S.

Pintsuk, G.

Rieth, M.

Wirtz, M.

KITopen

Manufacturing and Characterization of PIM-W Materials as PFMs  Gerald Pintsuk1, Steffen Antusch2, M. Rieth2, M. Wirtz1  1 Forschungszentrum Juelich (FZJ) 2 Karsruhe Institute of Technology (KIT) G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 2  Motivation  DEMO divertor development within the EUROFusion program WPMAT  Pure and particle strengthened materials interesting characteristics: strength, fracture toughness, ductility, recrystallization resistance, and sufficiently high thermal conductivity  PIM: near net shape technology; materials with isotropic microstructure and properties; fast screening of different compositions  Qualification via e-beam testing (standardized method) vs. a reference W-grade Stress [MPa] Strain 1400 1200 1000 800 600 400 200 0 0 0.02 0.04 0.06 0.08 0.10 0.12 0.14 400 °C 300 °C 200 °C G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 3  Tungsten Powder Injection Molding @ KIT Mass production of components Materials development Time & cost effective  near-net-shape forming process  Shape complexity & high final density Tailoring new materials & Investigation of properties G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 4  Mass production of tungsten parts Green parts (dark), finished parts (bright) Filling simulation PIM-tool Debinding / Heat-treatment Injection molding of green parts Feedstock Binder Powder Mixing / Kneading / Extrusion G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 5  Mass production of tungsten parts Green parts (dark), finished parts (bright) Filling simulation PIM-tool Debinding / Heat-treatment Injection molding of green parts Feedstock Binder Powder Mixing / Kneading / Extrusion G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 6  Mass production of tungsten parts Green parts (dark), finished parts (bright) Filling simulation PIM-tool Debinding / Heat-treatment Injection molding of green parts Feedstock Binder Powder Mixing / Kneading / Extrusion G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 7  Development of new materials Rolled-W: [A] in rolling direction – e.g. high strength and bending toughness  [B] perpendicular to rolling direction  PIM-W: [C] fully isotropic C Texture analysis: EBSD Rolled W-plate (Plansee AG) vs. PIM-W G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 8  Top view, ∅ ~10 µm Side view, 5 × 25 µm2 50 µm 50 µm 12 × 12 × 5 mm³ longitudinal transversal recrystallized 1600 °C, 1 hour Reference W according to ITER specs („IGP“) G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 9  PIM: Investigated W materials  pure W: 2 grades with different powder sizes (W-170, W-5050)  W-2La2O3: initial composition; vaporization of La2O3 during sintering ⇒ pure W with “clean” grain boundaries  W-Y2O3: 3 grades with different Y2O3 content (W-0.5Y2O3, W-1Y2O3, W-2Y2O3)  W-TiC: 4 grades with different TiC content (W-1TiC, W-1.5TiC, W-2TiC, W-3TiC)   W-TaC: 3 grades with different TaC content (W-0.5TaC, W-1TaC, W-2TaC) Manufacturing according to shown PIM-process; final sintering at 2400 °C; particle sizes < 1 µm G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 10  Materials grain size reference, trans. reference, long.: 10 x 25 µm reference, rxx: 64 x 102 µm  Optimization potential by variation of raw materials (powder sizes) G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 11  Materials hardness reference reference, rxx  Pure PIM-W similar to recrystallized W; hardness increase only for W-TiC G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 12  Qualification via thermal shock: e-beam JUDITH 1 E-beam parameters acceleration voltage: 120 - 150 kV beam power:  ≤ 60 kW pulse length: 1 ms – cont. beam diameter: 1 mm scanning frequency: ≤ 100 kHz Test parameters power density: 0.19-0.38 GW/m2 pulse length: 1 ms pulse number: 100, 1000 base temperature: RT, 400 °C, 1000 °C G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 13  Reference W according to ITER specs („IGP“) n = 100 n = 1000 G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 14  Thermal shock response: reference W longitudinal recrystallized transversal  small crack formation  grain loss for transversal orientation  significant surface roughening for recryst. material G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 15  W-170 W-5050 W-(2La2O3)  Significant surface roughening – similar to recrystallized material!  Reduced crack formation compared to reference ELM-test at elevated temperature reference: transversal G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 16  ELM-test at elevated temperature reference: transversal W-0.5Y2O3 W-2Y2O3 W-1Y2O3  Local µ-cracks due to inhomogeneities  Reduced crack formation compared to reference G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 17  ELM-test at elevated temperature reference: transversal W-1TiC  Low surface roughening  Crack formation similar to reference W-1TiC G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 18  W-1.5TiC W-3TiC ELM-test at elevated temperature W-2TiC reference: transversal  Large crack formation  No improvement compared to reference G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 19  W-0.5TaC W-1TaC W-2TaC ELM-test at elevated temperature reference: transversal  Local µ-cracks due to inhomogeneities.  Reduced crack formation compared to reference G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 20  ELM-test at elevated temperature reference, rxx: 1.33 µm reference  Reduced roughening / plastic deformation for W-Y2O3 and W-TiC materials G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 21  Grain size vs. roughness  Less roughening with decreasing grain size  G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 22  Grain size vs. hardness  Increased hardness with decreasing grain size G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 23  Hardness vs. roughness  Decreasing roughness with increasing hardness G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 24  ELM-test at elevated temperature     Further investigation via 4pt-bending & disruption tests  crack network cracks cracks cracks µ-cracks µ-cracks cracks µ-cracks µ-cracks µ-cracks µ-cracks µ-cracks G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 25  Mechanical testing via 4pt-bending Sample geometry: 12 × 1 × 1 mm3 Strain rate: 0.033 mm/min W-1TiC, 453 HV      1400 0.140 400 °C pure W, 371 HV 200 °C 300 °C 100 °C 1200 0.160 W-2Y2O3, 454 HV 1200 0.160 W-2TaC, 408 HV 1400 0.160 Stress [MPa] Stress [MPa] Stress [MPa] Stress [MPa] Strain Strain Strain Strain G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 26  W-1.1TiC (H. Kurishita): Pabs = 0.38 GW/m2, t = 1 ms, n = 1000, T = 1000 °C ⇒ low roughness (Ra = 0.3 µm) ⇒ only small and localized crack formation Disruption test - Rationale No disruption on cool surface ⇒ disruption test will be done at 1000 °C! Pabs = 1.13 GW/m2, t = 5 ms, n = 10, T = RT G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 27  W-5050 W-2Y2O3 W-1TiC W-2TaC Loading conditions: n = 100 T = 1000 °C Δt = 5 ms Labs = 1.13 GW/m2 Crack formation vs. inhomogeneous melting! Disruption test Tm,Y2O3 = 2410 °C Tm,TiC = 3140 °C Tm,TaC = 3880 °C G. Pintsuk | PFMC 2015 | Aix en Provence, France | 18-22. May 2015 | 28  Summary Fabrication  Mass production of near-net-shape parts via PIM @ KIT  Brittle to ductile transition for pure PIM W at 200 °C (low strain rates)  High density (> 99 % T.D.)  Fully isotropic material properties  Qualification  Increased hardness and mechanical strength for W-Y2O3 and W-TiC materials ⇒ reduced roughening / plastic deformation  Reduced roughening ⇒ thermal fatigue induced crack formation (in view of > 106 ELM pulses) is slowed down  Disruption test: crack formation (≥ 1 mm) is still an issue even at 1000 °C  Disruption test: additives with relative low melting point may cause an inhomogeneous melt distribution 

Manufacturing and characterization of PIM-W materials as PFMs

https://publikationen.bibliothek.kit.edu/230100821/3816820

Manufacturing and characterization of PIM-W materials as PFMs

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