WO2022208032A1 - Method for manufacturing metal parts and metal parts obtained using sps sintering - Google Patents
Method for manufacturing metal parts and metal parts obtained using sps sintering Download PDFInfo
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- WO2022208032A1 WO2022208032A1 PCT/FR2022/050614 FR2022050614W WO2022208032A1 WO 2022208032 A1 WO2022208032 A1 WO 2022208032A1 FR 2022050614 W FR2022050614 W FR 2022050614W WO 2022208032 A1 WO2022208032 A1 WO 2022208032A1
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- powder
- manufacturing process
- process according
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- size
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- 238000005245 sintering Methods 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 title claims description 15
- 239000002184 metal Substances 0.000 title claims description 12
- 239000000843 powder Substances 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000002019 doping agent Substances 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 239000000956 alloy Substances 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000002490 spark plasma sintering Methods 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000000889 atomisation Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000007769 metal material Substances 0.000 description 6
- 238000000280 densification Methods 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000002902 bimodal effect Effects 0.000 description 2
- 230000001427 coherent effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000001131 transforming effect Effects 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 238000001812 pycnometry Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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- C22C—ALLOYS
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- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0057—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0292—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with more than 5% preformed carbides, nitrides or borides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the present invention relates to the manufacture of metal parts by sintering, in particular the manufacture of parts having mechanical properties of particular hardness.
- a metallurgical material such as steel mainly comprises iron and carbon, the carbon being between 0.02% and 2% by mass.
- the carbon content In order to increase the hardness of a steel, it is known to increase the carbon content.
- some steels have carbon concentrations above 1.7% (ledeburitic steels).
- heat treatments these treatments being mainly surface treatments.
- Another object of the invention is to limit the number of operations and/or treatments.
- the invention proposes a method for manufacturing a metallurgical part characterized by the following steps:
- the part obtained according to the invention makes it possible to increase the hardness compared to the results of the prior art, while limiting the costs thanks in particular to the reduction in the number of operations and/or post-treatments. In addition, this makes it possible to limit the carbon content by compared to the results of the prior art.
- the metallurgical part obtained is thus intrinsically different from the results of the prior art.
- - SPS sintering acronym for "Spark Plasma Sintering"
- Spark Plasma Sintering a pressure sintering process based on the densification of a powder sample by applying a mechanical stress associated with the passage of a pulsed current to heat the sample; for example a sintering method related to hot isostatic pressing but using the Joule effect to heat the precompacted powder in a hollow cylindrical crucible between two graphite electrodes under an inert atmosphere or under vacuum, the assembly being subjected to a pressure of several megapascals under the action of a hydraulic press.
- a direct or alternating current of several kiloamperes, pulsed or not, is applied between the electrodes with a voltage of a few volts. ;
- any material making it possible to improve the densification and/or the final mechanical properties giving mechanical cohesion to the final part for example cobalt material or another sintering agent;
- grain size or grain size, or grain size, the size characterized by the values d10, d90, d50 in order to quantify the dispersion of this grain size distribution;
- - spheroidization, or spheroidize in particular concerning a powder, a method of transforming an angular ground metal powder by melting, most often plasma assisted, to make it spherical; - grinding or milling, in particular concerning a powder, a method of transformation by mechanical action, for example by balls, so as to reduce the size of the crystallites and/or the size of the grains of a powder;
- the grain size is measurable by an optical or electronic microscope or by a granulometer.
- the particle sizer it is possible to use a particle sizer of the laser or optical type, in the dry or liquid way.
- the metallurgical part or the metallurgical material comprises at least one metallic element.
- the part or material comprises at least 50% by mass of at least one metallic element.
- the powder of metallurgical material used has a particle size of less than 50 mna (micrometers).
- the powder of metallurgical material used comprises:
- the powder of metallurgical material may include doping agents to further increase the final hardness, in order to complete the composition of said powder and respectively:
- metal phase means a metallurgical or crystallographic phase which is a particular compound combining several chemical elements and having a particular microstructure.
- An alloy is an association of metallic elements mainly and optionally in a minority of ceramic elements.
- An alloy can comprise one or more metallurgical phases.
- the metallic phase is an iron-based alloy, such as steel or cast iron, or an aluminum-based alloy, or a titanium-based alloy, or a nickel-based alloy.
- the present invention deals with all alloys.
- the metallurgical material has a carbon content of less than or equal to 2% by weight relative to the total weight of the metallurgical material.
- the metallurgical material has a carbon content of less than or equal to 2%, preferably less than or equal to 1.75%, preferably less than or equal to 1.5%, preferably less than or equal to 1.25 %, preferably less than or equal to 1%, preferably less than or equal to 0.75%, preferably less than or equal to 0.5%.
- Each grain type has a predetermined grain size, a predetermined crystallite size, and a predetermined aspect ratio.
- the powder is reduced, in particular when the powder cannot be used as it is, so that:
- the aggregates have a characteristic size of less than 200 micrometers, and/or
- the average crystallite size is less than 100 nanometers.
- the reduction in the size of the grains and/or the crystallites of the powder comprises:
- the method comprises a step of atomizing the powder used so that the size of the grains has a size less than or equal to 150 micrometers.
- the reduction in the size of the grains and/or crystallites of the powder comprises:
- a step of grinding the metallurgical material so that the size of the agglomerates has a size of less than 1000 micrometers.
- the atomization step is carried out before the grinding step.
- d50 being between 0.1 and 100 m m ,
- One embodiment consists in using a monomodal particle size distribution before grinding of between 0.1 and 100 micrometers (jim).
- the powders have a bimodal distribution before grinding with d50 values separated by a decade, typically O. ⁇ iti and 1 m m or 1 mm m and
- the distribution is trimodal with d50 separated by a decade, typically O. ⁇ iti, 1 m m and IO iti. These examples are obviously non-limiting.
- the powder is used as is, raw from the supplier.
- this powder may have a d50 value, in particular a grain diameter, of less than 100 micrometers, preferably less than 50 micrometers, preferably less than 15 micrometers.
- the powder is ground in order to refine the size of the crystallites (coherent crystallographic domains) which is different from the distribution particle size.
- the size of the crystallites coherent crystallographic domains
- the powder is ground in order to refine the size of the crystallites (coherent crystallographic domains) which is different from the distribution particle size.
- the size of the crystallites is between 20 and 1000 nanometers (nm).
- the size of the crystallites is between 20 and 100 nm.
- the size of the crystallites is between 20 and 50 nm. In one embodiment, it is possible to associate several sizes of crystallites.
- the manufacturing method comprises a step of adding at least one doping agent with the metallurgical material, before the sintering step.
- the at least one doping agent is or comprises boron nitride BN, titanium carbide TiC, tungsten carbide WC, silicon carbide SiC, niobium carbide NbC, boron carbide B C, Silicon nitride SiN , aluminum oxide AlO , zirconium oxide ZrO , yttrium oxide Y0 or a mixture of these.
- the at least one doping agent is or comprises the doped variants of the preceding elements.
- the manufacturing process only comprises a step of atomizing the powder of the metallurgical material, and then the powder obtained, called intermediate powder, can be mixed, or not, with at least one doping agent.
- the manufacturing method only comprises a step of grinding the powder of the metallurgical material, and then the powder obtained, called intermediate powder, can be mixed, or not, with at least one doping agent.
- the sintering step is carried out until a piece of predetermined shape is obtained which is composed or consists of the sintered metallurgical material.
- the part of predetermined shape is composed or consists solely of sintered metallurgical material, the metallurgical material comprising one or more of the characteristics stated above.
- the sintering step is carried out until a part, called the starting part, is covered with a layer of sintered metallurgical material so as to obtain a part of predetermined shape.
- the manufacturing process further comprises the following steps:
- the starting part is obtained by the sintering step according to the first embodiment.
- the manufacturing method comprises a step of adding at least one substrate metal powder with the metallurgical material, before the sintering step.
- the height of each layer of sintered powder according to the need is the height of each layer of sintered powder according to the need.
- substrate metal powder means any alloy that is thermochemically compatible with the metallurgical powder resulting in metallic materials of high hardness.
- the substrate metal powder is 316L steel or nickel-free stainless steel.
- the manufacturing process further comprises a heat treatment step after the sintering step.
- the invention proposes a metallurgical part obtained according to one or more of the characteristics of the manufacturing process of the first aspect.
- the metallurgical part is for example, and in a non-limiting manner, a cutting tool for machining or drilling.
- the metallurgical part is obtained by SPS sintering of a powder of a metallurgical material characterized in that the powder has a grain size of less than 1000 micrometers and/or a crystallite size of less than 200 nanometers, so that the metallurgical part obtained has a Vickers hardness greater than 320Hv.
- the manufacturing process provides for taking into account only the grain size and/or the crystallite size.
- the manufacturing process provides for taking into account only the grain size and/or the crystallite size.
- the stress applied may be greater than 0 MPa, preferably greater than or equal to 5
- MPa and less than or equal to 150 MPa preferably less than or equal to 75 MPa, preferably less than or equal to 50 MPa, preferably less than or equal to 25 MPa, preferably less than or equal to 20 MPa, preferably less than or equal at 18 MPa, preferably less than or equal to 15 MPa;
- the duration of the SPS sintering stage can be greater than or equal to 2 minutes and less than or equal to 45 minutes.
- the temperature can be determined empirically by those skilled in the art depending on the nature of the metallic grade chosen.
- the densification parameters are to be adapted according to the metallic shade of the matrix.
- the determination of the sintering parameters described above can be defined by those skilled in the art via an empirical study.
- the choice of the sintering parameters may or may not induce a phenomenon of filler/matrix reactivity which may improve the final reinforcement of the formed material.
- the filler content is greater than a few mass %.
- the rate is greater than 1%, preferably greater than 5%, preferably less than 30%, preferably less than 25%.
- the step of grinding the metallurgical material, preferably the metallurgical powder, and/or the co-grinding of the metallurgical powder and the hardening filler, and/or the mixing of the metallurgical powders and the fillers hardeners can be carried out by dry or wet process. As part of the dry process, it can be carried out in air or in neutral gas depending on the nature of the metallic shade of the matrix. In the case of a wet route, the choice of solvent will be determined via empirical study known to those skilled in the art.
- said manufacturing method provides for a cryogenic grinding step.
- the quality of the sintering can be determined by measurement of geometric density, by buoyancy of Archimedes, by helium pycnometry, by porosimetry, by intrusion of mercury, and possibly by BET (measurement of specific surface area of materials measured by adsorption of a gas (nitrogen) with the BET method (Brunauer, Emett and Teller)), or image analysis in microscopy, or a combination of several methods.
- BET Brunauer, Emett and Teller
- FIG. 1 represents a flowchart presenting the various embodiments of the manufacturing method.
- the "Alloy" metallic material powder can be only atomized or only ground, see the first two lines,
- the "Alloy" metallic material powder can be atomized and mixed with an addition element or doping agent, see the fourth line,
- the "Alloy" metallic material powder can be ground and mixed with an addition element or doping agent, see the fifth line,
- the “Alloy” metallic material powder can be atomized, then ground and mixed with an addition element or doping agent, see sixth line.
- the hardness of the ex nihilo metallurgical part obtained or of the coating of the metallurgical part obtained is:
- the intermediate powder can be deposited before or after a metal substrate powder so as to form a superposition of layers. Adjust the height of each layer as needed.
- the coating can be applied, see “SPS D sintering”, on a part, called the starting part, for example a steel called 316L.
- the coating may have a thickness greater than or equal to one millimeter.
- the hardness of the parts obtained is thus increased until it reaches a value between 200 Hv and 1500 Hv with doping agents.
- the doping agent is for example silicon carbide.
- the aggregates have for example a size of between 100 and 500 micrometers.
- the grain size is for example between 50 and 150 nanometers. This example makes it possible to obtain a part with a hardness approximately equal to 1000 Hv.
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Abstract
The invention relates to a method for manufacturing a metallurgical part, characterized by the following steps: - using a powder of a metallurgical material having a particle size of less than 400 micrometers, - reducing the size of the grains and/or crystallites of the powder so as to obtain clusters having a characteristic size of less than 1000 micrometers, and a mean crystallite size of less than 200 nanometers, - sintering the reduced powder using an SPS sintering method, so that the metallurgical part obtained has a Vickers hardness of greater than 320 Hv.
Description
PROCEDE DE FABRICATION DE PIECES METALLIQUES ET PIECES METALLIQUES OBTENUES A BASE DE FRITTAGE SPS PROCESS FOR MANUFACTURING METALLIC PARTS AND METALLIC PARTS OBTAINED FROM SPS SINTERING
DOMAINE TECHNIQUE DE L’INVENTION TECHNICAL FIELD OF THE INVENTION
La présente invention concerne la fabrication de pièces métalliques par frittage, en particulier la fabrication de pièces présentant des propriétés mécaniques de dureté particulière. The present invention relates to the manufacture of metal parts by sintering, in particular the manufacture of parts having mechanical properties of particular hardness.
ETAT DE LA TECHNIQUE STATE OF THE ART
Un matériau métallurgique tel que l’acier comprend principalement du fer et du carbone, le carbone étant compris entre 0,02% et 2% en masse. Afin d’augmenter la dureté d’un acier, il est connu d’augmenter la teneur en carbone. Par exemple, certains aciers présentent des concentrations de carbone supérieures à 1,7% (aciers lédéburitiques). En outre, il est possible de réaliser des traitements thermiques, ces traitements étant principalement surfaciques. A metallurgical material such as steel mainly comprises iron and carbon, the carbon being between 0.02% and 2% by mass. In order to increase the hardness of a steel, it is known to increase the carbon content. For example, some steels have carbon concentrations above 1.7% (ledeburitic steels). In addition, it is possible to carry out heat treatments, these treatments being mainly surface treatments.
Il est ainsi désireux de proposer un matériau présentant une dureté équivalente ou supérieure à celles de l’état de la technique, et/ou une dureté homogène en volume. Un autre but de l’invention est de limiter le nombres d’opérations et/ou de traitements. It is therefore keen to offer a material with a hardness equivalent to or greater than that of the state of the art, and/or a uniform hardness in volume. Another object of the invention is to limit the number of operations and/or treatments.
L’INVENTION THE INVENTION
A cet effet, et selon un premier aspect, l’invention propose un procédé de fabrication d’une pièce métallurgique caractérisé par les étapes suivantes : To this end, and according to a first aspect, the invention proposes a method for manufacturing a metallurgical part characterized by the following steps:
- utiliser une poudre d’un matériau métallurgique présentant une granulométrie inférieure à 400 pim (micromètres), - use a powder of a metallurgical material with a particle size of less than 400 μm (micrometers),
- réduire la taille des grains et/ou des cristallites de la poudre de manière à obtenir des agrégats d’une taille caractéristique inférieure à 1000 pim (micromètres), et une taille moyenne de cristallites inférieure à 200 nm (nanomètres), - reduce the size of the grains and/or crystallites of the powder so as to obtain aggregates with a characteristic size of less than 1000 μm (micrometers), and an average crystallite size of less than 200 nm (nanometers),
- fritter en utilisant un procédé de frittage SPS la poudre réduite, de manière que la pièce métallurgique obtenue présente une dureté Vickers supérieure à 320Hv. - sintering the reduced powder using an SPS sintering process, so that the metallurgical part obtained has a Vickers hardness greater than 320Hv.
La pièce obtenue selon l’invention permet d’augmenter la dureté par rapport aux résultats de l’art antérieur, tout en limitant les coûts grâce notamment à la diminution du nombre d’opérations et/ou de post- traitements. En outre, cela permet de limiter la teneur en carbone par
rapport aux résultats de l’art antérieur. La pièce métalurgique obtenue est ainsi intrinsèquement différente par rapport aux résultats de l’art antérieur. The part obtained according to the invention makes it possible to increase the hardness compared to the results of the prior art, while limiting the costs thanks in particular to the reduction in the number of operations and/or post-treatments. In addition, this makes it possible to limit the carbon content by compared to the results of the prior art. The metallurgical part obtained is thus intrinsically different from the results of the prior art.
Pour ce qui précède et pour la suite de la description, on entend par : For the foregoing and for the remainder of the description, the following terms mean:
- frittage SPS, acronyme de « Spark Plasma Sintering », un procédé de frittage sous pression basé sur la densification d’un échantillon de poudre par application d’une contrainte mécanique associée au passage d’un courant pulsé permettant de chauffer l’échantillon ; par exemple une méthode de frittage apparentée au pressage isostatique à chaud mais utilisant l'effet joule pour chauffer la poudre précompactée dans un creuset cylindrique creux entre deux électrodes en graphite sous atmosphère inerte ou sous vide, l'ensemble étant soumis à une pression de plusieurs mégapascals sous l'action d'une presse hydraulique. Un courant continu ou alternatif de plusieurs kiloampères, pulsé ou non, est appliqué entre les électrodes avec une tension de quelques volts. ; - SPS sintering, acronym for "Spark Plasma Sintering", a pressure sintering process based on the densification of a powder sample by applying a mechanical stress associated with the passage of a pulsed current to heat the sample; for example a sintering method related to hot isostatic pressing but using the Joule effect to heat the precompacted powder in a hollow cylindrical crucible between two graphite electrodes under an inert atmosphere or under vacuum, the assembly being subjected to a pressure of several megapascals under the action of a hydraulic press. A direct or alternating current of several kiloamperes, pulsed or not, is applied between the electrodes with a voltage of a few volts. ;
- liant, toute matière permettant d’améliorer la densification et/ou les propriétés mécaniques finales donnant une cohésion mécanique à la pièce finale, par exemple le matériau cobalt ou un autre agent de frittage ; - binder, any material making it possible to improve the densification and/or the final mechanical properties giving mechanical cohesion to the final part, for example cobalt material or another sintering agent;
- taille de grains, ou granulométrie, ou granulométrie des grains, la taille caractérisée par les valeurs dlO, d90, d50 afin de quantifier la dispersion de cette distribution de taille de grains ; - grain size, or grain size, or grain size, the size characterized by the values d10, d90, d50 in order to quantify the dispersion of this grain size distribution;
- taille de cristallites, ou taille moyenne de cristallites, chaque grain pouvant présenter des cristallites, la taille se rapportant aux domaines cristallographiques cohérents et qui est mesurée par des techniques du type MEB, TEM, ...; - size of crystallites, or average size of crystallites, each grain possibly having crystallites, the size relating to the coherent crystallographic domains and which is measured by techniques of the SEM, TEM, etc. type;
- facteur de forme, le rapport entre deux longueurs caractéristiques, chaque longueur s’étendant selon une direction déterminée, lesdites longueurs caractéristiques présentant un angle non- nul l’une par rapport à l’autre, par exemple un angle de 90 degrés ; - form factor, the ratio between two characteristic lengths, each length extending in a determined direction, said characteristic lengths having a non-zero angle with respect to each other, for example an angle of 90 degrees;
- atomisation ou atomiser, en particulier concernant une poudre, une méthode de transformation d’un lingot métallique en poudre sphérique par fusion et projection des gouttes métalliques sous flux gazeux pour les rendre sphériques, - atomization or atomization, in particular concerning a powder, a method of transforming a metal ingot into spherical powder by melting and projecting metal drops under a gas stream to make them spherical,
- sphéroïdisation, ou sphéroïdiser, en particulier concernant une poudre, une méthode de transformation d’une poudre métallique broyée anguleuse par fusion le plus souvent assisté plasma pour la rendre sphérique ;
- broyage ou broyer, en particulier concernant une poudre, une méthode de transformation par action mécanique, par exemple par des billes, de manière à réduire la taille des cristallites et/ou la taille des grains d’une poudre ; - spheroidization, or spheroidize, in particular concerning a powder, a method of transforming an angular ground metal powder by melting, most often plasma assisted, to make it spherical; - grinding or milling, in particular concerning a powder, a method of transformation by mechanical action, for example by balls, so as to reduce the size of the crystallites and/or the size of the grains of a powder;
- agrégats, le résultat d’une réduction de la taille des grains et/ou de la taille des cristallites, par exemple par broyage, qui aboutit à une agglomération de petits grains pour former des agglomérats plus gros, mais chaque grain constituant les agglomérats présentent des tailles de cristallites plus petits ; - aggregates, the result of a reduction in the size of the grains and/or the size of the crystallites, for example by grinding, which results in an agglomeration of small grains to form larger agglomerates, but each grain constituting the agglomerates has smaller crystallite sizes;
- dureté, la résistance d'un matériau a être marqué par un autre, on utilisera ici la dureté Vickers. - hardness, the resistance of a material to being marked by another, here we will use the Vickers hardness.
De préférence, la taille de grain est mesurable par un microscope optique ou électronique ou par un granulomètre. Dans le cas du granulomètre, il est possible d’utiliser un granulomètre du type laser ou optique, en voie sèche ou liquide. Preferably, the grain size is measurable by an optical or electronic microscope or by a granulometer. In the case of the particle sizer, it is possible to use a particle sizer of the laser or optical type, in the dry or liquid way.
De préférence, la pièce métallurgique ou le matériau métallurgique comprend au moins un élément métallique. La pièce ou le matériau comprend au moins 50% en masse de l’au moins un élément métallique. Preferably, the metallurgical part or the metallurgical material comprises at least one metallic element. The part or material comprises at least 50% by mass of at least one metallic element.
De manière préférentielle, la poudre de matériau métallurgique utilisée présente une granulométrie inférieure à 50 mna (micromètres). Preferably, the powder of metallurgical material used has a particle size of less than 50 mna (micrometers).
Selon des variantes de réalisation, la poudre de matériau métallurgique utilisée comprend :According to variant embodiments, the powder of metallurgical material used comprises:
- au moins 98% d’une phase métallique, ou - at least 98% of a metallic phase, or
- au moins 95% d’une phase métallique, ou - at least 95% of a metallic phase, or
- au moins 85% d’une phase métallique, ou - at least 85% of a metallic phase, or
- au moins 80% d’une phase métallique, ou - at least 80% of a metallic phase, or
- au moins 75% d’une phase métallique. - at least 75% of a metallic phase.
En lien avec le paragraphe précédent, la poudre de matériau métallurgique peut comprendre des agents dopants permettant d’augmenter encore plus la dureté finale, afin de compléter la composition de ladite poudre et respectivement :In connection with the previous paragraph, the powder of metallurgical material may include doping agents to further increase the final hardness, in order to complete the composition of said powder and respectively:
- au plus 2% d’un ou plusieurs agents dopants, - at most 2% of one or more doping agents,
- au plus 5% d’un ou plusieurs agents dopants, - at most 5% of one or more doping agents,
- au plus 15% d’un ou plusieurs agents dopants,
- au plus 20% d’un ou plusieurs agents dopants, - at most 15% of one or more doping agents, - at most 20% of one or more doping agents,
- au plus 25% d’un ou plusieurs agents dopants. - at most 25% of one or more doping agents.
On entend par phase métallique, une phase métallurgique, ou cristallographique qui est un composé particulier associant plusieurs éléments chimiques et présentant une microstructure particulière. Un alliage est une association d’éléments métalliques principalement et optionnellement de manière minoritaire des éléments céramiques. Un alliage peut comporter une ou plusieurs phases métallurgiques. The term “metallic phase” means a metallurgical or crystallographic phase which is a particular compound combining several chemical elements and having a particular microstructure. An alloy is an association of metallic elements mainly and optionally in a minority of ceramic elements. An alloy can comprise one or more metallurgical phases.
De préférence, la phase métallique est un alliage à base de fer, tel que l’acier ou la fonte, ou un alliage à base d’aluminium, ou un alliage à base de titane, ou un alliage à base de nickel. La présente invention traite de tous les alliages. Preferably, the metallic phase is an iron-based alloy, such as steel or cast iron, or an aluminum-based alloy, or a titanium-based alloy, or a nickel-based alloy. The present invention deals with all alloys.
De préférence, le matériau métallurgique présente une teneur en carbone inférieure ou égale à 2% en poids par rapport au poids total du matériau métallurgique. De manière préférentielle, le matériau métallurgique présente une teneur en carbone inférieure ou égale à 2% , de préférence inférieure ou égale à 1,75%, de préférence inférieure ou égale à 1,5%, de préférence inférieure ou égale à 1,25%, de manière préférée inférieure ou égale à 1%, de préférence inférieure ou égale à 0,75%, de manière préférentielle inférieure ou égale à 0,5%. Preferably, the metallurgical material has a carbon content of less than or equal to 2% by weight relative to the total weight of the metallurgical material. Preferably, the metallurgical material has a carbon content of less than or equal to 2%, preferably less than or equal to 1.75%, preferably less than or equal to 1.5%, preferably less than or equal to 1.25 %, preferably less than or equal to 1%, preferably less than or equal to 0.75%, preferably less than or equal to 0.5%.
Chaque type de grains présente une taille de grain prédéterminée, une taille de cristallite prédéterminée et un facteur de forme prédéterminé. Each grain type has a predetermined grain size, a predetermined crystallite size, and a predetermined aspect ratio.
De préférence, la poudre est réduite, en particulier lorsque la poudre ne peut pas être utilisée telle quelle, de manière que : Preferably, the powder is reduced, in particular when the powder cannot be used as it is, so that:
- les agrégats présentent une taille caractéristique inférieure à 200 micromètres, et/ou- the aggregates have a characteristic size of less than 200 micrometers, and/or
- la taille moyenne des cristallites est inférieure à 100 nanomètres. - the average crystallite size is less than 100 nanometers.
Selon des variantes de réalisation pouvant, ou non, être combinées, la réduction de la taille des grains et/ou des cristallites de la poudre comprend : According to variant embodiments which may or may not be combined, the reduction in the size of the grains and/or the crystallites of the powder comprises:
- une étape d’atomisation du matériau métallurgique, et/ou - a step of atomization of the metallurgical material, and/or
- une étape de broyage du matériau métallurgique, de manière que la poudre utilisée présente une granulométrie inférieure à 1000 micromètres.
De préférence, le procédé comprend une étape d’atomisation de la poudre utilisée de manière que la taille des grains présente une taille inférieure ou égale à 150 micromètres. - a step of grinding the metallurgical material, so that the powder used has a particle size of less than 1000 micrometers. Preferably, the method comprises a step of atomizing the powder used so that the size of the grains has a size less than or equal to 150 micrometers.
Selon d’autres variantes de réalisation, pouvant, ou non, être combinées, la réduction de la taille des grains et/ou des cristallites de la poudre comprend : According to other variant embodiments, which may or may not be combined, the reduction in the size of the grains and/or crystallites of the powder comprises:
- une étape d’atomisation du matériau métallurgique, et/ou - a step of atomization of the metallurgical material, and/or
- une étape de broyage du matériau métallurgique, de manière que la taille des agglomérats présente une taille inférieure à 1000 micromètres. - a step of grinding the metallurgical material, so that the size of the agglomerates has a size of less than 1000 micrometers.
De préférence, et dans le cas de la combinaison des deux étapes, l’étape d’atomisation est réalisée avant l’étape de broyage. Preferably, and in the case of the combination of the two steps, the atomization step is carried out before the grinding step.
La microstructure de grains prédéterminée peut présenter les caractéristiques suivantes :The predetermined grain microstructure may have the following characteristics:
- Distribution granulométrique : d50 étant compris entre 0.1 et 100 m m , - Particle size distribution: d50 being between 0.1 and 100 m m ,
- Taille de cristallite : 20 à 1000 nm, - Crystallite size: 20 to 1000 nm,
- Facteur de forme : entre 1 et 5 (sphérique à anguleux, sans être cylindrique). - Form factor: between 1 and 5 (spherical to angular, without being cylindrical).
Un mode de réalisation consiste à utiliser une distribution granulométrique monomodale avant broyage comprise entre 0.1 et 100 micromètres (jim ). One embodiment consists in using a monomodal particle size distribution before grinding of between 0.1 and 100 micrometers (jim).
Selon un autre mode de réalisation, les poudres présentent une distribution bimodale avant broyage avec des valeurs d50 séparées d’une décade, typiquement O.ΐ iti et 1 m m ou 1 m m etAccording to another embodiment, the powders have a bimodal distribution before grinding with d50 values separated by a decade, typically O.ΐ iti and 1 m m or 1 mm m and
1 Om m ou encore 1 Om m et 1 ()()// m . Il se peut que cette distribution bimodale soit séparée de1 Om m or 1 Om m and 1 ()()// m . It may be that this bimodal distribution is separated from
2 décades, typiquement 0.1 et 1 Om m ou 1 et 1 ()()// m . 2 decades, typically 0.1 and 1 Om m or 1 and 1 ()()// m .
Selon encore un autre mode de réalisation, la distribution est trimodale avec des d50 séparées d’une décade, typiquement O.ΐ iti, 1 m m et IO iti. Ces exemples sont évidemment non limitatifs. According to yet another embodiment, the distribution is trimodal with d50 separated by a decade, typically O.ΐ iti, 1 m m and IO iti. These examples are obviously non-limiting.
Dans un mode de réalisation, la poudre est utilisée telle quelle, brute de fournisseur. Par exemple, cette poudre peut présenter une valeur d50, en particulier un diamètre, de grain inférieur(e) à 100 micromètres, de préférence inférieur(e) à 50 micromètres, de préférence inférieur(e) à 15 micromètres. In one embodiment, the powder is used as is, raw from the supplier. For example, this powder may have a d50 value, in particular a grain diameter, of less than 100 micrometers, preferably less than 50 micrometers, preferably less than 15 micrometers.
Dans un mode préférentiel, la poudre est broyée afin d’affiner la taille des cristallites (domaines cristallographiques cohérents) qui est différente de la distribution
granulométrique. Ainsi, après broyage, on constate une réduction de la taille des cristallites, mais pas nécessairement une réduction de la taille des grains. In a preferential mode, the powder is ground in order to refine the size of the crystallites (coherent crystallographic domains) which is different from the distribution particle size. Thus, after grinding, a reduction in the size of the crystallites is observed, but not necessarily a reduction in the size of the grains.
Préférentiellement, la taille des cristallites est comprise entre 20 et 1000 nanomètres (nm). Préférentiellement, la taille des cristallites est comprise entre 20 et 100 nm. Préférentiellement enfin, la taille des cristallites est comprise entre 20 et 50 nm. Dans un mode de réalisation, il est envisageable d’associer plusieurs tailles de cristallites. Preferably, the size of the crystallites is between 20 and 1000 nanometers (nm). Preferably, the size of the crystallites is between 20 and 100 nm. Finally, preferably, the size of the crystallites is between 20 and 50 nm. In one embodiment, it is possible to associate several sizes of crystallites.
Selon un mode de réalisation, le procédé de fabrication comprend une étape d’ajout d’au moins un agent dopant avec le matériau métallurgique, avant l’étape de frittage. According to one embodiment, the manufacturing method comprises a step of adding at least one doping agent with the metallurgical material, before the sintering step.
De préférence, l’au moins un agent dopant est ou comprend du nitrure de bore BN, du carbure de titane TiC, du carbure de tungstène WC, du carbure de silicium SiC, du carbure de niobium NbC, du carbure de bore B C, du Nitrure de silicium SiN , de l’oxide d’aluminium Al O , de l’oxyde de zirconium ZrO , de l’oxyde d’yttrium Y0 ou un mélange de ceux-ci. De manière préférentielle, l’au moins un agent dopant est ou comprend les variants dopés des éléments précédents. Preferably, the at least one doping agent is or comprises boron nitride BN, titanium carbide TiC, tungsten carbide WC, silicon carbide SiC, niobium carbide NbC, boron carbide B C, Silicon nitride SiN , aluminum oxide AlO , zirconium oxide ZrO , yttrium oxide Y0 or a mixture of these. Preferably, the at least one doping agent is or comprises the doped variants of the preceding elements.
Selon un mode de réalisation particulier, le procédé de fabrication comprend uniquement une étape d’atomisation de la poudre du matériau métallurgique, et ensuite la poudre obtenue, dite poudre intermédiaire, peut être mélangée, ou non, à au moins un agent dopant. According to a particular embodiment, the manufacturing process only comprises a step of atomizing the powder of the metallurgical material, and then the powder obtained, called intermediate powder, can be mixed, or not, with at least one doping agent.
Selon un autre mode de réalisation particulier, le procédé de fabrication comprend uniquement une étape de broyage de la poudre du matériau métallurgique, et ensuite la poudre obtenue, dite poudre intermédiaire, peut être mélangée, ou non, à au moins un agent dopant. According to another particular embodiment, the manufacturing method only comprises a step of grinding the powder of the metallurgical material, and then the powder obtained, called intermediate powder, can be mixed, or not, with at least one doping agent.
Selon un premier mode de réalisation, l’étape de frittage est réalisée jusqu’à l’obtention d’une pièce de forme prédéterminée est composée ou constituée du matériau métallurgique fritté. De manière préférentielle, la pièce de forme prédéterminée est composée ou constituée uniquement du matériau métallurgique fritté, le matériau métallurgique comprenant l’une ou plusieurs des carctéristiques énoncées précédemment. According to a first embodiment, the sintering step is carried out until a piece of predetermined shape is obtained which is composed or consists of the sintered metallurgical material. Preferably, the part of predetermined shape is composed or consists solely of sintered metallurgical material, the metallurgical material comprising one or more of the characteristics stated above.
Selon un deuxième mode de réalisation, l’étape de frittage est réalisée jusqu’à recouvrir une pièce, dite pièce de départ, d’une couche du matériau métallurgique fritté de manière à obtenir une pièce de forme prédéterminée.
Par exemple le procédé de fabrication comprend en outre les étapes suivantes : According to a second embodiment, the sintering step is carried out until a part, called the starting part, is covered with a layer of sintered metallurgical material so as to obtain a part of predetermined shape. For example, the manufacturing process further comprises the following steps:
- choisir une pièce, dite pièce de départ, - choose a piece, called the starting piece,
- fritter la poudre réduite sur la pièce de départ jusqu’à recouvrir ladite pièce de manière à obtenir la pièce métallurgique. - sinter the reduced powder on the starting part until the said part is covered so as to obtain the metallurgical part.
Selon une variante de réalisation, la pièce de départ est obtenue par l’étape de frittage selon le premier mode de réalisation. According to a variant embodiment, the starting part is obtained by the sintering step according to the first embodiment.
De préférence, selon n’importe quel mode de réalisation, le procédé de fabrication comprend une étape d’ajout d’au moins une poudre métallique de substrat avec le matériau métallurgique, avant l’étape de frittage. Preferably, according to any embodiment, the manufacturing method comprises a step of adding at least one substrate metal powder with the metallurgical material, before the sintering step.
De manière préférentielle, selon n’importe quel mode de réalisation, la hauteur de chaque couche de poudre frittée en fonction du besoin. Preferably, according to any embodiment, the height of each layer of sintered powder according to the need.
On entend par poudre métallique de substrat, Tout alliage, compatible thermochimiquement avec la poudre métallurgique aboutissant au matériaux métallique de dureté élevée. Par exemple, la poudre métallique de substrat est de l’acier 316L ou de l’inox sans nickel. The term “substrate metal powder” means any alloy that is thermochemically compatible with the metallurgical powder resulting in metallic materials of high hardness. For example, the substrate metal powder is 316L steel or nickel-free stainless steel.
De préférence, le procédé de fabrication comprend en outre une étape de traitement thermique après l’étape de frittage. Preferably, the manufacturing process further comprises a heat treatment step after the sintering step.
Selon un deuxième aspect, l’invention propose une pièce métallurgique obtenue selon l’une ou plusieurs des caractéristiques du procédé de fabrication du premier aspect. According to a second aspect, the invention proposes a metallurgical part obtained according to one or more of the characteristics of the manufacturing process of the first aspect.
La pièce métallurgique est par exemple, et de manière non limitative, un outil de coupe pour l’usinage ou le forage. The metallurgical part is for example, and in a non-limiting manner, a cutting tool for machining or drilling.
La pièce métallurgique est obtenue par frittage SPS d’une poudre d’un matériau métallurgique caractérisé en ce que la poudre présente une taille de grains inférieure à 1000 micromètres et/ou une taille de cristallites inférieure à 200 nanomètres, de manière que la pièce métallurgique obtenue présente une dureté Vickers supérieure à 320Hv. The metallurgical part is obtained by SPS sintering of a powder of a metallurgical material characterized in that the powder has a grain size of less than 1000 micrometers and/or a crystallite size of less than 200 nanometers, so that the metallurgical part obtained has a Vickers hardness greater than 320Hv.
De préférence, le procédé de fabrication prévoit de prendre en compte seulement la taille de grain et/ou la taille de cristallites.
Selon un ou plusieurs modes de réalisation, pouvant être combinable, lors de l’étape de frittage en utilisant un procédé de frittage SPS : Preferably, the manufacturing process provides for taking into account only the grain size and/or the crystallite size. According to one or more embodiments, which can be combined, during the sintering step using an SPS sintering process:
-la contrainte appliquée peut être supérieure à 0 MPa, de préférence supérieure ou égale à 5- the stress applied may be greater than 0 MPa, preferably greater than or equal to 5
MPa et inférieure ou égale à 150 MPa, de préférence inférieure ou égale à 75 MPa, de préférence inférieure ou égale à 50 MPa, de préférence inférieure ou égale à 25 MPa, de préférence inférieure ou égale à 20 MPa, de préférence inférieure ou égale à 18 MPa, de préférence inférieure ou égale à 15 MPa; MPa and less than or equal to 150 MPa, preferably less than or equal to 75 MPa, preferably less than or equal to 50 MPa, preferably less than or equal to 25 MPa, preferably less than or equal to 20 MPa, preferably less than or equal at 18 MPa, preferably less than or equal to 15 MPa;
- la durée de palier du frittage SPS peut être supérieure ou égale à 2 minutes et inférieure ou égale à 45 minutes. - the duration of the SPS sintering stage can be greater than or equal to 2 minutes and less than or equal to 45 minutes.
De préférence, la température peut être déterminée de manière empirique par l’homme du métier en fonction de la nature de la nuance métallique choisie. Preferably, the temperature can be determined empirically by those skilled in the art depending on the nature of the metallic grade chosen.
Ces caractéristiques permettent d’obtenir une pièce présentant un taux de densification souhaité, qui peut être égal ou supérieur à 70% et peut être égal à 100%. En particulier, l’association de la température, de la contrainte et de la durée du pallier permettent d’accéder à un taux de densification souhaité. These characteristics make it possible to obtain a part with a desired densification rate, which can be equal to or greater than 70% and can be equal to 100%. In particular, the combination of the temperature, the stress and the duration of the plateau allow access to a desired densification rate.
De préférence, les paramètres de densification (température, durée de pallier, contrainte) sont à adapter en fonction de la nuance métallique de la matrice. Par exemple, la détermination des paramètres de frittage décrit précédemment sont définissable par l’homme du métier via une étude empirique. Selon un mode de réalisation, en fonction de la nature des agents dopants, dit aussi charges durcissantes et la nature de la nuance métallique de la matrice, le choix des paramètres de frittage peuvent induire ou non un phénomène de réactivité charge/matrice qui pourra améliorer le renforcement final du matériaux formé. Par exemple, le taux de charges est supérieur à quelques % massiques. Par exemple, le taux est supérieur à 1%, de préférence supérieure à 5%, de préférence inférieur à 30%, de préférence inférieur à 25%. Preferably, the densification parameters (temperature, plateau duration, stress) are to be adapted according to the metallic shade of the matrix. For example, the determination of the sintering parameters described above can be defined by those skilled in the art via an empirical study. According to one embodiment, depending on the nature of the doping agents, also called hardening fillers and the nature of the metallic shade of the matrix, the choice of the sintering parameters may or may not induce a phenomenon of filler/matrix reactivity which may improve the final reinforcement of the formed material. For example, the filler content is greater than a few mass %. For example, the rate is greater than 1%, preferably greater than 5%, preferably less than 30%, preferably less than 25%.
Selon un mode de réalisation, l’etape de broyage du matériau métallurgique, de préférence de la poudre métallurgique, et/ou le co-broyage de la poudre métallurgique et de la charge durcissante, et/ou le mélangeage des poudres métallurgique et des charges durcissantes peut être réaliser en voie sèche ou en voie humide. Dans le cadre de la voie sèche, elle peut être réalisée sous air ou sous gaz neutre en fonction de la nature de la nuance métallique de la
matrice. Dans le cas d’une voie humide, le choix du solvant sera déterminé via étude empirique connue de l’homme du métier. According to one embodiment, the step of grinding the metallurgical material, preferably the metallurgical powder, and/or the co-grinding of the metallurgical powder and the hardening filler, and/or the mixing of the metallurgical powders and the fillers hardeners can be carried out by dry or wet process. As part of the dry process, it can be carried out in air or in neutral gas depending on the nature of the metallic shade of the matrix. In the case of a wet route, the choice of solvent will be determined via empirical study known to those skilled in the art.
De préférence, ledit procédé de fabrication prévoit une étape de broyage cryogénique. Preferably, said manufacturing method provides for a cryogenic grinding step.
De préférence, la qualité du frittage peut être déterminée par mesure de densité géométrique, par poussée d’Archimède, par pycnométrie hélium, par porosimétrie, par intrusion de mercure, et éventuellement par BET (mesure de surface spécifique des matériaux mesurée par adsorption d'un gaz (azote) avec la méthode BET (Brunauer, Emett et Teller)), ou analyse d’image en microscopie, ou une combinaison de plusieurs méthodes. Preferably, the quality of the sintering can be determined by measurement of geometric density, by buoyancy of Archimedes, by helium pycnometry, by porosimetry, by intrusion of mercury, and possibly by BET (measurement of specific surface area of materials measured by adsorption of a gas (nitrogen) with the BET method (Brunauer, Emett and Teller)), or image analysis in microscopy, or a combination of several methods.
Description de la figure Description of figure
La figure 1 représente un logigramme présentant les différents modes de réalisation du procédé de fabrication. FIG. 1 represents a flowchart presenting the various embodiments of the manufacturing method.
En référence à la figure 1 , il est prévu un procédé de fabrication d’une pièce métallique au cours duquel : Referring to Figure 1, there is provided a method of manufacturing a metal part during which:
- la poudre de matériau métallugique « Alliage » peut être seulement atomisée ou seulement broyée, voir les deux premières lignes, - the "Alloy" metallic material powder can be only atomized or only ground, see the first two lines,
- la poudre de matériau métallugique « Alliage » peut être atomisée puis broyée, voir la troisième ligne, - the "Alloy" metallic material powder can be atomized and then ground, see the third line,
- la poudre de matériau métallugique « Alliage » peut être atomisée et mélangée à un élément d’addition ou agent dopant, voir la quatrième ligne, - the "Alloy" metallic material powder can be atomized and mixed with an addition element or doping agent, see the fourth line,
- la poudre de matériau métallugique « Alliage » peut être broyée et mélangée à un élément d’addition ou agent dopant, voir la cinquième ligne, - the "Alloy" metallic material powder can be ground and mixed with an addition element or doping agent, see the fifth line,
- la poudre de matériau métallugique « Alliage » peut être atomisée, puis broyée et mélangée à un élément d’addition ou agent dopant, voir sixième ligne. - the “Alloy” metallic material powder can be atomized, then ground and mixed with an addition element or doping agent, see sixth line.
L’obtention de cette poudre dite poudre d’alliage intermédiaire est ensuite fritter en utilisant la méthode du frittage SPS, voir « frittage SPS A ». Obtaining this powder called intermediate alloy powder is then sintered using the SPS sintering method, see “SPS A sintering”.
La dureté de la pièce métallurgique ex nihilo obtenue ou du revêtement de la pièce métallurgique obtenu est : The hardness of the ex nihilo metallurgical part obtained or of the coating of the metallurgical part obtained is:
- supérieure à 200Hv dans les cas d’une atomisation seule ou d’un broyage seule,
- supérieure à 350Hv dans le cas d’une atomisation puis d’un broyage,- greater than 200Hv in the case of atomization alone or grinding alone, - greater than 350Hv in the case of atomization then grinding,
- supérieure à 450Hv dans les autres cas. - greater than 450Hv in other cases.
Selon un autre mode de réalisation, la poudre intermédiaire peut être déposée avant ou après une poudre de substrat métallique de manière à former une superposition de couches. On ajustera la hauteur de chaque couche en fonction du besoin. According to another embodiment, the intermediate powder can be deposited before or after a metal substrate powder so as to form a superposition of layers. Adjust the height of each layer as needed.
Ensuite cette superposition de couches est frittée en utilisant la méthode du frittage SPS, voir « frittage SPS B », permettant d’obtenir une pièce métallurgique ex nihilo obtenue. Then this superposition of layers is sintered using the SPS sintering method, see “SPS B sintering”, making it possible to obtain an ex nihilo metallurgical part obtained.
Selon une variante de réalisation par rapport au précédent mode de réalisation, il est possible de réaliser le procédé de fabrication précédent de manière à former un revêtement, voir « frittage SPS C », sur une pièce métallurgique obtenue ex nihilo, après « frittage SPS A » . According to an alternative embodiment compared to the previous embodiment, it is possible to carry out the previous manufacturing process so as to form a coating, see "SPS C sintering", on a metallurgical part obtained ex nihilo, after "SPS A sintering » .
Selon une autre variante, le revêtement peut être appliqué, voir « frittage SPS D », sur une pièce, dite pièce de départ, par exemple un acier dit 316L. According to another variant, the coating can be applied, see “SPS D sintering”, on a part, called the starting part, for example a steel called 316L.
Le revêtement peut présenter une épaisseur supérieure ou égale à un millimètre. The coating may have a thickness greater than or equal to one millimeter.
La dureté des pièces obtenues est ainsi augmentée jusqu’à atteindre une valeur comprise entre 200 Hv et 1500 Hv avec des agents dopants. The hardness of the parts obtained is thus increased until it reaches a value between 200 Hv and 1500 Hv with doping agents.
Selon un mode de réalisation, l’agent de dopage est par exemple du carbure de silicium. Les agrégats présentent par exemple une taille comprise entre 100 et 500 micromètres. La taille des grains est par exemple comprise entre 50 et 150 nanomètres. Cet exemple permet d’obtenir une pièce présentant une dureté environ égale à 1000 Hv.
According to one embodiment, the doping agent is for example silicon carbide. The aggregates have for example a size of between 100 and 500 micrometers. The grain size is for example between 50 and 150 nanometers. This example makes it possible to obtain a part with a hardness approximately equal to 1000 Hv.
Claims
1. Procédé de fabrication d’une pièce métallurgique caractérisé par les étapes suivantes : 1. Process for manufacturing a metallurgical part characterized by the following steps:
- Utiliser une poudre d’un matériau métallurgique présentant une granulométrie inférieure à 400 micromètres, - Use a powder of a metallurgical material with a particle size of less than 400 micrometers,
- réduire la taille des grains et/ou des cristallites de la poudre de manière à obtenir des agrégats d’une taille caractéristique inférieure à 1000 micromètres, et une taille moyenne de cristallites inférieure à 200 nanomètres, - reduce the size of the grains and/or crystallites of the powder so as to obtain aggregates with a characteristic size of less than 1000 micrometers, and an average crystallite size of less than 200 nanometers,
- Fritter en utilisant un procédé de frittage SPS la poudre réduite, de manière que la pièce métallurgique obtenue présente une dureté Vickers supérieure à 320Hv. - Sinter using an SPS sintering process the reduced powder, so that the metallurgical part obtained has a Vickers hardness greater than 320Hv.
2. Procédé de fabrication selon la revendication précédente, dans lequel la poudre de matériau métallurgique comprend au moins 98% d’une phase métallique. 2. Manufacturing process according to the preceding claim, in which the powder of metallurgical material comprises at least 98% of a metallic phase.
3. Procédé de fabrication selon la revendication précédente, dans lequel la poudre de matériau métallurgique comprend au moins 75% d’une phase métallique. 3. Manufacturing process according to the preceding claim, in which the powder of metallurgical material comprises at least 75% of a metallic phase.
4. Procédé de fabrication selon la revendication 2 ou 3, dans lequel la phase métallique est un alliage à base de fer, tel que l’acier, ou un alliage à base d’aluminium, ou un alliage à base de titane, ou un alliage à base de nickel. 4. Manufacturing process according to claim 2 or 3, in which the metallic phase is an iron-based alloy, such as steel, or an aluminum-based alloy, or a titanium-based alloy, or a nickel base alloy.
5. Procédé de fabrication selon l’une des revendications précédentes, dans lequel les agrégats présentent une taille caractéristique inférieure à 200 micromètres. 5. Manufacturing process according to one of the preceding claims, in which the aggregates have a characteristic size of less than 200 micrometers.
6. Procédé de fabrication selon l’une des revendications précédentes, dans lequel la taille moyenne des cristallites est inférieure à 100 nanomètres. 6. Manufacturing process according to one of the preceding claims, in which the average size of the crystallites is less than 100 nanometers.
7. Procédé de fabrication selon l’une des revendications précédentes, dans lequel la réduction de la taille des grains et/ou des cristallites de la poudre comprend une étape d’atomisation du matériau métallurgique de manière qu’il présente une granulométrie inférieure à 1000 micromètres. 7. Manufacturing process according to one of the preceding claims, in which the reduction in the size of the grains and/or crystallites of the powder comprises a step of atomizing the metallurgical material so that it has a particle size of less than 1000 micrometers.
8. Procédé de fabrication selon l’une des revendications précédentes, dans lequel la réduction de la taille des grains et/ou des cristallites de la poudre comprend une étape de broyage du matériau métallurgique de manière qu’il présente une granulométrie inférieure à 1000 micromètres.
8. Manufacturing process according to one of the preceding claims, in which the reduction in the size of the grains and/or crystallites of the powder comprises a step of grinding the metallurgical material so that it has a particle size of less than 1000 micrometers .
9. Procédé de fabrication selon l’une des revendications précédentes, comprenant une étape d’ajout d’au moins un agent dopant avec le matériau métallurgique, avant l’étape de frittage. 9. Manufacturing process according to one of the preceding claims, comprising a step of adding at least one doping agent with the metallurgical material, before the sintering step.
10. Procédé de fabrication selon la revendication précédente, dans lequel l’au moins un agent dopant est du nitrure de bore, du carbure de titane, du carbure de tungstène, du carbure de silicium, du carbure de niobium, du carbure de bore, du borure de silicium, de l’oxide d’aluminium, de l’oxyde de zirconium, de l’oxyde d’yttrium ou un mélange de ceux-ci. 10. Manufacturing process according to the preceding claim, in which the at least one doping agent is boron nitride, titanium carbide, tungsten carbide, silicon carbide, niobium carbide, boron carbide, silicon boride, aluminum oxide, zirconium oxide, yttrium oxide or a mixture thereof.
11. Procédé de fabrication selon l’une des revendications précédentes, dans lequel l’étape de frittage est réalisée jusqu’à l’obtention d’une pièce de forme prédéterminée composée du matériau métallurgique fritté. 11. Manufacturing process according to one of the preceding claims, in which the sintering step is carried out until a part of predetermined shape composed of the sintered metallurgical material is obtained.
12. Procédé de fabrication selon l’une des revendications 1 à 10, comprenant en outre les étapes suivantes : 12. Manufacturing process according to one of claims 1 to 10, further comprising the following steps:
- choisir une pièce, dite pièce de départ, - choose a piece, called the starting piece,
- fritter la poudre réduite sur la pièce de départ jusqu ’ à recouvrir ladite pièce de manière à obtenir la pièce métallurgique. - sinter the reduced powder on the starting part until the said part is covered so as to obtain the metallurgical part.
13. Procédé de fabrication selon la revendication précédente, dans lequel la pièce de départ est obtenue par l’étape de frittage selon la revendication 11. 13. Manufacturing process according to the preceding claim, in which the starting part is obtained by the sintering step according to claim 11.
14. Procédé de fabrication selon l’une des revendications précédentes, comprenant une étape d’ajout d’au moins une poudre métallique de substrat avec le matériau métallurgique, avant l’étape de frittage. 14. Manufacturing process according to one of the preceding claims, comprising a step of adding at least one metal substrate powder with the metallurgical material, before the sintering step.
15. Procédé de fabrication selon l’une des revendications précédentes, comprenant une étape de traitement thermique après l’étape de frittage. 15. Manufacturing process according to one of the preceding claims, comprising a heat treatment step after the sintering step.
16. Pièce métallurgique caractérisée en ce qu’elle est obtenue selon l’une des revendications précédentes.
16. Metallurgical part characterized in that it is obtained according to one of the preceding claims.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP22718747.3A EP4313446A1 (en) | 2021-03-31 | 2022-03-31 | Method for manufacturing metal parts and metal parts obtained using sps sintering |
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| FR2103304A FR3121374A1 (en) | 2021-03-31 | 2021-03-31 | Process for manufacturing metal parts and metal parts obtained based on SPS sintering |
| FRFR2103304 | 2021-03-31 |
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| WO2022208032A1 true WO2022208032A1 (en) | 2022-10-06 |
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| PCT/FR2022/050614 WO2022208032A1 (en) | 2021-03-31 | 2022-03-31 | Method for manufacturing metal parts and metal parts obtained using sps sintering |
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| Country | Link |
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| EP (1) | EP4313446A1 (en) |
| FR (1) | FR3121374A1 (en) |
| WO (1) | WO2022208032A1 (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120208045A1 (en) * | 2011-02-11 | 2012-08-16 | The Board Of Regents For Oklahoma State University | Method of fabricating amorphous coatings on crystalline substrates |
| JP2013181213A (en) * | 2012-03-01 | 2013-09-12 | Hokkaido Univ | Oxide dispersion strengthening type nickel-based superalloy |
| US20170314097A1 (en) * | 2016-05-02 | 2017-11-02 | Korea Advanced Institute Of Science And Technology | High-strength and ultra heat-resistant high entropy alloy (hea) matrix composites and method of preparing the same |
| CN107475564A (en) * | 2017-08-22 | 2017-12-15 | 东北大学 | A kind of preparation method of high-strength compact titanium alloy ceramics Biocomposite material |
| CN110257684A (en) * | 2019-07-22 | 2019-09-20 | 合肥工业大学 | A kind of preparation process of FeCrCoMnNi high-entropy alloy-base composite material |
| CN110735063A (en) * | 2019-08-27 | 2020-01-31 | 江苏大学 | Preparation method of high-performance high-temperature titanium alloy-based composite material |
-
2021
- 2021-03-31 FR FR2103304A patent/FR3121374A1/en active Pending
-
2022
- 2022-03-31 EP EP22718747.3A patent/EP4313446A1/en active Pending
- 2022-03-31 WO PCT/FR2022/050614 patent/WO2022208032A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120208045A1 (en) * | 2011-02-11 | 2012-08-16 | The Board Of Regents For Oklahoma State University | Method of fabricating amorphous coatings on crystalline substrates |
| JP2013181213A (en) * | 2012-03-01 | 2013-09-12 | Hokkaido Univ | Oxide dispersion strengthening type nickel-based superalloy |
| US20170314097A1 (en) * | 2016-05-02 | 2017-11-02 | Korea Advanced Institute Of Science And Technology | High-strength and ultra heat-resistant high entropy alloy (hea) matrix composites and method of preparing the same |
| CN107475564A (en) * | 2017-08-22 | 2017-12-15 | 东北大学 | A kind of preparation method of high-strength compact titanium alloy ceramics Biocomposite material |
| CN110257684A (en) * | 2019-07-22 | 2019-09-20 | 合肥工业大学 | A kind of preparation process of FeCrCoMnNi high-entropy alloy-base composite material |
| CN110735063A (en) * | 2019-08-27 | 2020-01-31 | 江苏大学 | Preparation method of high-performance high-temperature titanium alloy-based composite material |
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| ALLAHAR KERRY N ET AL: "Ferritic oxide dispersion strengthened alloys by spark plasma sintering", JOURNAL OF NUCLEAR MATERIALS, ELSEVIER B.V, NETHERLANDS, vol. 443, no. 1, 16 July 2013 (2013-07-16), pages 256 - 265, XP028770651, ISSN: 0022-3115, DOI: 10.1016/J.JNUCMAT.2013.07.019 * |
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| Publication number | Publication date |
|---|---|
| FR3121374A1 (en) | 2022-10-07 |
| EP4313446A1 (en) | 2024-02-07 |
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