WO2014187867A1 - Procédé de fabrication d'une poudre contenant du métal - Google Patents
Procédé de fabrication d'une poudre contenant du métal Download PDFInfo
- Publication number
- WO2014187867A1 WO2014187867A1 PCT/EP2014/060462 EP2014060462W WO2014187867A1 WO 2014187867 A1 WO2014187867 A1 WO 2014187867A1 EP 2014060462 W EP2014060462 W EP 2014060462W WO 2014187867 A1 WO2014187867 A1 WO 2014187867A1
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- WO
- WIPO (PCT)
- Prior art keywords
- powder
- metal
- hydride
- mixture
- atmosphere
- Prior art date
Links
- 239000000843 powder Substances 0.000 title claims abstract description 170
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 74
- 239000002184 metal Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 239000012298 atmosphere Substances 0.000 claims abstract description 36
- 239000008187 granular material Substances 0.000 claims abstract description 33
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 29
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 29
- 239000011575 calcium Substances 0.000 claims abstract description 27
- 229910052987 metal hydride Inorganic materials 0.000 claims abstract description 24
- 150000004681 metal hydrides Chemical class 0.000 claims abstract description 24
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 14
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 23
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 229910052804 chromium Inorganic materials 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 9
- 150000002739 metals Chemical class 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- 229910012375 magnesium hydride Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 2
- RSHAOIXHUHAZPM-UHFFFAOYSA-N magnesium hydride Chemical compound [MgH2] RSHAOIXHUHAZPM-UHFFFAOYSA-N 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 34
- 239000002245 particle Substances 0.000 description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 238000010438 heat treatment Methods 0.000 description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 239000010936 titanium Substances 0.000 description 22
- 239000007789 gas Substances 0.000 description 21
- 239000001257 hydrogen Substances 0.000 description 19
- 229910052739 hydrogen Inorganic materials 0.000 description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 16
- 239000012467 final product Substances 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- 229910001092 metal group alloy Inorganic materials 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 239000011651 chromium Substances 0.000 description 13
- 229910052786 argon Inorganic materials 0.000 description 12
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 12
- 150000004678 hydrides Chemical class 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 10
- 239000000956 alloy Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 10
- 239000007858 starting material Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 9
- 239000010955 niobium Substances 0.000 description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 8
- -1 hydride compound Chemical class 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 229910000048 titanium hydride Inorganic materials 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 229910000765 intermetallic Inorganic materials 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000006356 dehydrogenation reaction Methods 0.000 description 4
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 3
- 229910002335 LaNi5 Inorganic materials 0.000 description 3
- 229910052776 Thorium Inorganic materials 0.000 description 3
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 2
- 238000009838 combustion analysis Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010165 TiCu Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
-
- 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
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/11—Argon
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/05—Light metals
- B22F2301/052—Aluminium
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
- B22F2301/205—Titanium, zirconium or hafnium
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/30—Low melting point metals, i.e. Zn, Pb, Sn, Cd, In, Ga
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/45—Rare earth metals, i.e. Sc, Y, Lanthanides (57-71)
-
- 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
- B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
- B22F2302/45—Others, including non-metals
-
- 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 concerns a new method for producing metal powders, metal alloy powders, intermetallic powders and/or their hydride powders, by a simplified, cost efficient process, preferably by performing the reduction reaction of metal oxides under hydrogen gas protection, using specific reducing agents and specific reduction conditions.
- Powder metallurgical (PM) techniques are well established routes for efficient production of complex metal based components. These techniques are commonly used in applications where alloys based on iron, stainless steel, copper or nickel are required. However, the use of PM techniques where material such as titanium, chromium and tantalum are required has so far been limited due to lack of availability of corresponding powders of high quality. Titanium metal base alloys and non-titanium metal base alloy powders are amongst the advanced materials, which are key to performance improvements and have many favorable properties such as high strength to weight ratio, good ductility and fracture toughness, high corrosion resistance and high melting point, making them important engineering materials for many applications in aerospace, chemical processing industry, architecture, and terrestrial systems. However, a major concern with titanium-based materials is high cost compared to competing materials.
- the present invention relates to a cost effective production of metal powders, metal alloy powders, intermetallic powders and/or their hydride powders, resulting in high levels of purity.
- the conventional method of producing titanium alloy powder today involves producing titanium sponge by the Kroll process, vacuum arc melting the sponge
- the Kroll process involves the reaction of T1O2 and carbon under chlorine gas at temperatures around 800°C, thus forming titanium chloride, TiCI 4 .
- TiCU produced in the reaction is in the form of liquid and must first be purified by distillation. This means that this process is complex and uses products difficult to handle, such as Mg and/or chlorine.
- US 6,264,719 discloses a method of producing a titanium-alumina composite, which results in the formation of AI2O3 particles in a Ti-rich metallic or intermetallic phase.
- JP 05299216 relates to the preparation of rare earth based alloy magnetic material, and describes a method in which a rare earth oxide, a reducing agent, and a metal are mixed, a reduction-diffusion reaction treatment is conducted in a hydrogen- containing reducing atmosphere, and the obtained cake-like reaction product is cooled.
- the reducing atmosphere is switched to an inert gas atmosphere when the cake-like reaction product is cooled.
- This switch is conducted in the temperature window of 770 to 870 °C. Conducting the switch in this specific temperature window is said to lead to the rare earth alloy product having good magnetic characteristics. In particular, conducting the switch in this temperature window is said to be important to ensure that the product does not contain any undesirable metal hydride product. There is no suggestion that any intermediate metal hydride product that may form during the reduction step would have any useful attributes.
- WO2008/010733 describes a process for producing titanium alloy powders.
- T1O2 and Al powder are mixed and heat-treated to form a
- T1AI/AI2O3 metal matrix ceramic composite material Said composite is further reduced in a second heat treatment step using CaH 2 .
- Attempts have also been made to produce various metal powders from their metal oxides by using the so-called self-ignition synthesis method. (Akiyama et al). These methods usually lead to products which suffer from low purity. Consequently, there is still a need for a more cost efficient process to produce high quality metal powders, metal alloy powders, intermetallic powders and/or their hydride powders, with high purity.
- the present invention is based on the realization that it is possible to completely reduce metal oxides under hydrogen atmosphere, using calcium and/or calcium hydride granules or powders, at a specified temperature to obtain pure metal or metal alloy powders at a high rate.
- the process of the invention particularly in the context of the preferred metal oxides discussed herein, enables excellent control over the reaction conditions, meaning that there is no need to take extra steps that may have been employed in previous methods.
- extra steps may include the provision of "buffer" substances that do not contribute to the reaction step, to act as a buffer during heat absorption/generation in order to avoid sharp rises/falls in temperature.
- the process of the invention also enables the preparation of metal powders, metal alloy powders, intermetallic powders and/or their hydride powders, which are of a very high quality, particularly in terms of purity and particle size distribution.
- the process may be applied to the production of a wide range of metal containing powders, such as metal powders, metal hydride powders, and/or metal alloy powders.
- metal oxides in powder form, are mixed with a reducing agent, such as calcium or magnesium in powder form or in the form of granules.
- a reducing agent such as calcium or magnesium in powder form or in the form of granules.
- the powder mixture should preferably not be compacted.
- the powder mixture is heated to a temperature in the range of 1000°C to 1500°C, and kept under a hydrogen atmosphere. This results in the formation of metal hydrides which are optionally subsequently dehydrated under a vacuum, or under an inert gas atmosphere (e.g. argon).
- an inert gas atmosphere e.g. argon
- the final product is of a higher purity than what is achieved with previously known technologies. This makes it possible to use the resulting metal powder in a variety of different applications within the powder metallurgy industry.
- Figure 1 is an SEM micrograph of the final product powder from T1O2 + 1 .3XCa granules at 1 100°C, 2 hr under argon gas atmosphere.
- Figure 2 shows an EDS spectrum of the final product powder from T1O2 + 1 .3XCa granules at 1 100°C, 2 hr under argon gas atmosphere.
- Figure 3 shows an XRD pattern of the final product material for the reduction of T1O2 and 1 .2XCa granules heat treated at 1 100°C for 2hrs under argon gas protection.
- the above XRD pattern showed that titanium was the first major phase of material, but in the same time showed calcium titanium oxide as the second phase of material. This means that the reduction reaction process was not successfully processed under the above mentioned conditions.
- Figure 4 is an SEM micrograph of the final product powder from T1O2 + 1 .3X Ca granules at 1 100°C, 2 hr under H 2 then switched to Ar gas.
- Figure 5 shows an EDS spectrum of the final product powder from T1O2 + 1 .3X Ca granules at 1 100°C, 2 hr under H 2 then switched to Ar gas
- Figure 6 shows the XRD pattern of the final product powder from T1O2 + 1 .3xCa granules at 1 100°C, 2hr under H 2 gas then switched to argon gas.
- the XRD pattern shows that titanium metal is the major constituent in the final product, with little or no contaminants.
- Figure 7 is an SEM micrograph of the Cr from the Cr2O3 and 1 .3X CaH 2 powder at 1 100°C for 2hrs under H 2 gas for both heating and cooling sessions.
- the particles have a spheroidal shape.
- Figure 8 shows the EDS spectrum of the final product powder from the Cr 2 O3 and 1 .3X CaH 2 powder at 1 100°C for 2hrs under H 2 gas for both heating and cooling sessions.
- Figure 9 shows the XRD of the final product of chromium powder from the Cr 2 O3 and 1 .3X CaH 2 powder at 1 100°C for 2hrs under H 2 gas for both heating and cooling sessions.
- Figure 10 is an SEM micrograph of Nb metal powder from Nb 2 O 5 +1 .2CaH 2 - heating Ar for both heating and cooling sessions.
- Figure 1 1 shows an EDS spectrum of the final product powder Nb 2 O 5 +1 .2CaH 2 - heating Ar for both heating and cooling sessions.
- Figure 12 is an SEM micrograph of tantalum powder made according to Example 12.
- the invention concerns a cost-efficient method of producing metal powders and their hydrides or alloys consisting or comprising the following steps:
- the present invention provides a process for manufacturing metal containing powder, the process comprising the steps of:
- the metal containing powder is a metal hydride powder or a hydride of a metal alloy or intermetallic.
- the invention provides a process as defined above, wherein metal hydride powder is recovered.
- the present invention provides a process for manufacturing metal hydride powder, comprising the steps of;
- the metal containing powder is a metal powder, a metal alloy or an intermetallic.
- the invention provides a process as defined above, further further comprising between steps (b) and (c):
- step (a) comprises mixing at least one metal oxide powder with Ca or Mg granules and/or calcium hydride or magnesium hydride in granule or powder form to form a mixture.
- Said at least one metal oxide is preferably chosen from oxides of:
- said at least one metal oxide is chosen from oxides of Sc, Ti, V, Cr, Mn, Y, Zr, Nb, Hf, Ta, rare earth metals, Th, U, and/or Si.
- oxides which may be used as starting material are oxides of Al, In, Sb, Sn, Ge, Bi, and/or Pb.
- oxides which may be used as starting material are oxides of Ti, Cr, Al, V, La, Nb and/or Ta.
- the temperature range in which to maintain the mixture under an H 2 atmosphere is preferably between 1000°C and 1500°C, more preferably 1020 °C and 1400 °C, more preferably 1020 °C and 1300 °C, more preferably 1020 °C and 1200 °C, still more preferably 1020 °C and 1 100 °C.
- the time for which the mixture is maintained under an H 2 atmosphere is preferably 1 - 10 hours, more preferably 1 -5 hours, more preferably 2-4 hours and most preferably around 3 hours.
- the invention provides a process for manufacturing metal hydride powder, comprising the steps of:
- the invention also provides a process for manufacturing metal powder, comprising steps a) and b) above, followed by;
- step d) involves maintaining the mixture under a temperature of from 1000°C to 1500°C, preferably 1020 °C to 1400 °C, more preferably 1020 °C to 1300 °C, yet more preferably 1020 °C to 1200 °C, and yet more preferably still 1020 °C to 1 100 °C.
- the temperature maintained in step d) is substantially the same as that used in step b).
- the mixture is maintained under an Ar atmosphere preferably for around 1 hour, but this may vary between 20 minutes and 5 hours, preferably 40 minutes to 3 hours, preferably 50 minutes to 2 hours, still more preferably 55 minutes to 80 minutes.
- the ratio between number of oxygen atoms in said metal oxide and the number of calcium atoms is in the range of 1 :1 .7-1 .1 or 1 :1 .5-1 :1 .1 or 1 :1 .5- 1 :1 .05, or 1 :1 .4-1 :2, or 1 :1 .2.
- said metal oxide powder is T1O2 powder and said powder mixture is maintained in step b) under an H 2 atmosphere, at a temperature between 1020 °C and 1 100°C for around 3 hours.
- the invention also includes the metal powder or metal hydride powder produced according to the above methods.
- the invention provides a metal powder or metal hydride powder wherein the metal is as defined herein subject to being other than Ti.
- the invention includes a metal powder or metal hydride powder so produced, wherein the metal is Ti, Cr, Nb, or Ta. In a particularly preferred aspect the metal is Cr.
- the invention includes a metal powder or metal hydride powder so produced, wherein the metal is substantially free from oxygen.
- the invention includes a metal powder or metal hydride powder so produced, having an amount of oxygen lower than 0.35% by weight.
- metal oxide may also include metal particles that contain substantial amounts of oxygen in the form of dissolved oxygen, oxide inclusions and/or oxide coatings, in such amounts that make them unfit for use in production using PM techniques.
- the Ca or Mg granules are preferably in the size range of 0.03-2mm.
- Ca hydride (CaH 2 ) and/or magnesium hydride granules in the same size range may also be used.
- the term "powder” is meant to describe a collection of particles having a size range of 50nm-1 mm.
- Particle size distribution X50 (sometimes denoted D50) is also known as the median diameter or the medium value of the particle size distribution, and is the value of the particle diameter at 50% in the cumulative distribution.
- the particle size distribution of the products produced by the present method typically has an X50 of less than 40 ⁇ , or less than 35 ⁇ , or less than 25 ⁇ , or less than 20 ⁇ .
- Particle size and size distribution may be determined by e.g. light scattering.
- the X50 distribution is discussed at pages 216-218 of "Metals Handbook", 9th Edition, Volume 7, Powder Metallurgy, American Society for Metals, Metals Park, Ohio 44073, ISBN 0-87170-013-1 .
- the amount of contaminants (e.g. oxygen or nitrogen) in the final product may be determined by combustion analysis and detection by way of IR absorption (to determine oxygen levels) or by thermic conductivity (to determine nitrogen levels).
- the starting materials may, in addition to only one metal oxide, also include one or more additional metal containing reagents, which could be one or more metals or metal oxides (preferably metal oxides).
- the final product may be a metal alloy or an intermetallic compound. Preferably it is a metal alloy.
- the term "metal powder" is therefore meant to include pure metals, metal alloys and also intermetallic compounds.
- elemental metal powders such as iron, aluminum, nickel, copper etc, may be added to the reaction mix to provide a source of additional elements (e.g. to provide alloying elements). Oxides of these elements may also be used, e.g. Fe3O 4 .
- the resulting end product is a metal alloy powder or intermetallic compound powder.
- the metal oxide powder is T1O2 powder.
- the product is a hydride
- the product of step b is recovered (without the subsequent possible steps of switching to an Ar atmosphere, cooling under Ar atmosphere, and then recovering metal powder).
- the starting materials may, in addition to only one metal oxide, also include one or more additional metal containing reagents, which could be one or more metals or metal oxides (preferably metal oxides).
- the final product may be a metal alloy hydride or an intermetallic hydride compound.
- elemental metal powders such as iron, aluminum, nickel, copper etc, may be added to the reaction mix to provide a source of additional elements (e.g. to provide alloying elements). Oxides of these elements may also be used, e.g. Fe3O 4 .
- the resulting end product is a hydride of a metal alloy or intermetallic compound (in powder form).
- Said one or more additional metal containing reagents are preferably included in the reaction mixture in powder or granular form, most preferably powder form.
- the hydrogen may be part of a substantially regular crystalline structure, but alternatively the hydrogen may be contained within the metal(s) in the form of a solid solution.
- percentages given in connection with the content of a given component in an alloy preferably indicate percentages by weight
- percentages given in connection with the content of a given component of an intermetallic compound preferably indicate percentages by mol. Unless indicated otherwise, percentage figures mentioned herein follow this general rule.
- the metal oxides may be present on the surface of metal particles or components, e.g. as a surrounding layer on a metal particle having been exposed to oxidizing conditions.
- the powder mixture in step b is preferably maintained under an H 2 atmosphere, at a temperature between 1020°C and 1 100°C, preferably for 3 hours.
- a strong exothermic reaction is interpreted as an un-controlled, thermal runaway reaction. It is believed that such an uncontrolled exothermic reaction (e.g. self-ignition combustion synthesis) leads to less pure material. These unwanted reactions can be avoided by e.g. using a specific ratio between oxygen and calcium, and optionally maintaining the reactants in non-compacted form.
- the reduction reaction should ideally take place under hydrogen atmosphere. In case a compacted form of reactants is to be used, this should ideally be in the form of thin plates, pellets, or granules.
- the resulting powders may be subjected to a drying step to remove water.
- the resulting metal powder typically has a particle size less than 25 ⁇ . Furthermore, the metal powder is of high purity, having an oxygen content lower than 0.35%, by weight.
- the equipment used to perform the experimental work was as follows: Any type of furnace suitable for working under temperatures for the reduction reaction, i.e. up to 1500°C may be used .
- the furnace should also be fitted with means for supplying various types of gases, or in some cases applying vacuum.
- a muffle open furnace was used to perform the heat treatment processes to achieve the reduction reaction of the oxides being used at different stages of work.
- a rectangular cross section crucible with a flat base was used.
- the crucible was made of high temperature resistant material such as e.g. chromium nickel steel (253 MA).
- the crucible was introduced to the furnace at each heat treatment process.
- the heat treatment was performed at different temperatures and time according to the examples below.
- the real temperature of the furnace was measured using a thermocouple to compare it with the set temperature.
- the difference in temperature between real temperature and set temperature was below 10°C.
- Containers filled with water were used for washing.
- the intermediate product after heat treatment was added to the water and washed.
- the containers were equipped with stirrers to stir the mixture of water and the intermediate material.
- Acetic acid was added to the slurry with continuous stirring.
- Calcium hydride may be prepared from its elements by direct combination of calcium and hydrogen at 300 to 400°C. Calcium granules were obtained from
- the amount of contaminants (e.g. oxygen or nitrogen) was determined by
- T1O2 100gram
- CaH 2 granules 145gram
- T1O2 in powder form Aldrich
- CaH 2 granules 0.4- ⁇ 2 mm
- the mixture was heated at 1 100°C during 2hrs under hydrogen gas in an open muffle furnace. After heating, the mixture was cooled for one hour under argon atmosphere.
- the resulting titanium powder particles had a particle size with X50 of 20.06 ⁇ , and did not form agglomerates.
- the oxygen content was 0.27%, nitrogen content
- the mixture was heated at 1 100°C during 2 hrs under hydrogen gas in an open muffle furnace. Both heating and cooling sessions were performed under hydrogen gas protection.
- the resulting chromium metal powder particles had a particle size with X50 of 5.93 ⁇ , and did not form agglomerates.
- the oxygen content was 0.08%, nitrogen content 0.003%, and hydrogen content 0.006%.
- XRD pattern showed that chromium was obtained without impurities.
- the calcium content was 0.004% as shown by ICP analysis.
- titanium hydride from TiO 2 and CaH 2 powder (metal hydride). 100 grams of ⁇ 2 in powder form(Aldrich) was mixed with 145 grams of calcium hydride powder at -325 mesh(Aldrich). The mixture was heated at 1 100°C during 2hrs under hydrogen gas in an open muffle furnace. Both heating and cooling sessions were maintained under hydrogen gas protection.
- the resulting titanium hydride powder particles had a particle size with X50 of ⁇ . ⁇ , and did not form agglomerates.
- the oxygen content was 0.12%, nitrogen content 0.72%, and hydrogen content 3.42% .
- XRD pattern showed that titanium hydride was obtained without impurities.
- the calcium content was 0.19% as shown by ICP analysis.
- the mixture was heated at 1 100°C during 2hrs under hydrogen gas, followed by argon gas, in an open muffle furnace.
- the resulting TM 9AI powder particles had a particle size with X50 of 16.4 ⁇ , and did not form agglomerates.
- the oxygen content was 0.28%, nitrogen content 0.03%, and hydrogen content 0.27%.
- XRD pattern showed that TM 9AI was obtained without impurities.
- the calcium content was 0.03% as shown by ICP analysis.
- the resulting ferrotitanium powder particles had a particle size with X50 of 10.69 ⁇ , and did not form agglomerates.
- the oxygen content was 0.13%, nitrogen content 0.06%, and hydrogen content 2.07%.
- XRD pattern showed that ferro titanium hydride powder was obtained without impurities.
- the calcium content was 0.026% as shown by ICP analysis
- T1O2 in powder form (Aldrich) was mixed with 7.1 grams of V 2 O 5 powder and 6gram of AI(Aldrich) powders were mixed with 245 grams of CaH 2 granules (Hoganas AB ) size of 0.4- ⁇ 2mm.
- the mixture was heated at 1 100°C during 3 hrs under hydrogen gas, then switched to argon gas environment, in an open muffle furnace.
- the switching of gases was performed in the open muffle furnace, with no need for transfer to another furnace for the dehydrogenation processing step.
- the resulting Ti6AI4V powder particles had a particle size with X50 of 9.73 ⁇ , and did not form agglomerates.
- the oxygen content was 0.24%, nitrogen content 0.05%, and hydrogen content 0.08%.
- XRD pattern showed that Ti6AI4V was obtained without impurities.
- the calcium content was 0.017% as shown by ICP analysis
- the mixture was heated at 1080°C for a period of 6 hrs under hydrogen gas protection, then switched to argon gas environment, in an open muffle furnace.
- the resulting LaNi 5 powder particles had a particle size with X50 of 9.57 ⁇ , and did not form agglomerates.
- the oxygen content was 0.17%, nitrogen content 0.08%, and hydrogen content 0.04%.
- XRD pattern showed that LaNi 5 was obtained without impurities.
- the calcium content was 0.06% as shown by ICP analysis Example 1 1
- Niobium metal powder was produced using heat treatment at 1050°C of the starting materials Nb 2 O 5 and CaH 2 granules (as 1 .2 of the stoichiometric ratio) for 2hrs under hydrogen followed by switching gases for the cooling session to be performed under argon gas protection.
- Tantalum metal powder from Ta 2 O 5 and CaH 2 granules (as 1 .2 of the stoichiometric ratio). Heat treatment was at 1050°C for 2hrs. Heating was under hydrogen gas protection followed by switching to argon gas environment ( in the same furnace without changing the furnace) for the dehydrogenation. SEM micrographs showed that the material is consisted of different sizes of agglomerates. These agglomerates were mostly consisted of very fine size particles but with few big sizes of the large agglomerates. In general the agglomerates were of very fine particles sizes as shown in Figure 12.
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Abstract
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CN201480041224.5A CN105392734A (zh) | 2013-05-21 | 2014-05-21 | 制造含金属的粉末的方法 |
US14/892,478 US20160089724A1 (en) | 2013-05-21 | 2014-05-21 | Process for manufacturing metal containing powder |
KR1020157036086A KR20160010874A (ko) | 2013-05-21 | 2014-05-21 | 금속 함유 분말을 제조하기 위한 공정 |
CA2912473A CA2912473A1 (fr) | 2013-05-21 | 2014-05-21 | Procede de fabrication d'une poudre contenant du metal |
JP2016514397A JP2016524040A (ja) | 2013-05-21 | 2014-05-21 | 金属含有粉末を製造する方法 |
BR112015028855A BR112015028855A2 (pt) | 2013-05-21 | 2014-05-21 | Processo para a fabricação de pó que contem metal |
EP14725204.3A EP2999661A1 (fr) | 2013-05-21 | 2014-05-21 | Procédé de fabrication d'une poudre contenant du métal |
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CN110802237B (zh) * | 2019-09-29 | 2021-06-15 | 中南大学 | 一种高纯锆金属粉的制备方法 |
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CN108602120B (zh) * | 2016-02-10 | 2021-03-09 | 犹他大学研究基金会 | 使固溶体中具有溶解于其中的氧的金属脱氧的方法 |
CN108602120A (zh) * | 2016-02-10 | 2018-09-28 | 犹他大学研究基金会 | 使固溶体中具有溶解于其中的氧的金属脱氧的方法 |
KR20180102691A (ko) * | 2016-02-10 | 2018-09-17 | 더 유니버시티 오브 유타 리서치 파운데이션 | 고용체 상태로 산소가 용해되어 있는 금속을 탈산소화시키는 방법 |
US11279996B2 (en) | 2016-03-22 | 2022-03-22 | Oerlikon Metco (Us) Inc. | Fully readable thermal spray coating |
US11939646B2 (en) | 2018-10-26 | 2024-03-26 | Oerlikon Metco (Us) Inc. | Corrosion and wear resistant nickel based alloys |
US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
Also Published As
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US20160089724A1 (en) | 2016-03-31 |
CA2912473A1 (fr) | 2014-11-27 |
TW201446364A (zh) | 2014-12-16 |
BR112015028855A2 (pt) | 2017-08-29 |
KR20160010874A (ko) | 2016-01-28 |
EP2999661A1 (fr) | 2016-03-30 |
GB201309173D0 (en) | 2013-07-03 |
CN105392734A (zh) | 2016-03-09 |
JP2016524040A (ja) | 2016-08-12 |
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