WO2022036938A1 - 高纯粉体材料的制备方法及其应用及一种双相粉体材料 - Google Patents
高纯粉体材料的制备方法及其应用及一种双相粉体材料 Download PDFInfo
- Publication number
- WO2022036938A1 WO2022036938A1 PCT/CN2020/134655 CN2020134655W WO2022036938A1 WO 2022036938 A1 WO2022036938 A1 WO 2022036938A1 CN 2020134655 W CN2020134655 W CN 2020134655W WO 2022036938 A1 WO2022036938 A1 WO 2022036938A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- phase
- powder
- particles
- matrix
- composition
- Prior art date
Links
- 239000000843 powder Substances 0.000 title claims abstract description 619
- 239000000463 material Substances 0.000 title claims abstract description 164
- 238000002360 preparation method Methods 0.000 title claims abstract description 84
- 230000002051 biphasic effect Effects 0.000 title abstract 2
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 533
- 239000000956 alloy Substances 0.000 claims abstract description 533
- 239000002245 particle Substances 0.000 claims abstract description 505
- 239000011159 matrix material Substances 0.000 claims abstract description 217
- 238000000889 atomisation Methods 0.000 claims abstract description 107
- 239000012535 impurity Substances 0.000 claims abstract description 104
- 238000000034 method Methods 0.000 claims abstract description 100
- 238000007711 solidification Methods 0.000 claims abstract description 94
- 230000008023 solidification Effects 0.000 claims abstract description 94
- 230000008569 process Effects 0.000 claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- -1 powder metallurgy Substances 0.000 claims abstract description 11
- 238000010146 3D printing Methods 0.000 claims abstract description 6
- 238000001746 injection moulding Methods 0.000 claims abstract description 6
- 238000004663 powder metallurgy Methods 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 230000001954 sterilising effect Effects 0.000 claims abstract description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 5
- 239000011358 absorbing material Substances 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 198
- 239000002994 raw material Substances 0.000 claims description 96
- 229910052760 oxygen Inorganic materials 0.000 claims description 59
- 229910052757 nitrogen Inorganic materials 0.000 claims description 54
- 229910052801 chlorine Inorganic materials 0.000 claims description 53
- 229910052731 fluorine Inorganic materials 0.000 claims description 53
- 229910052739 hydrogen Inorganic materials 0.000 claims description 53
- 229910052698 phosphorus Inorganic materials 0.000 claims description 53
- 229910052717 sulfur Inorganic materials 0.000 claims description 53
- 229910052740 iodine Inorganic materials 0.000 claims description 51
- 229910052794 bromium Inorganic materials 0.000 claims description 49
- 229910052720 vanadium Inorganic materials 0.000 claims description 46
- 238000005516 engineering process Methods 0.000 claims description 45
- 229910052746 lanthanum Inorganic materials 0.000 claims description 42
- 229910052804 chromium Inorganic materials 0.000 claims description 36
- 239000000470 constituent Substances 0.000 claims description 35
- 229910052742 iron Inorganic materials 0.000 claims description 33
- 239000002253 acid Substances 0.000 claims description 31
- 229910052802 copper Inorganic materials 0.000 claims description 31
- 229910052710 silicon Inorganic materials 0.000 claims description 31
- 229910052790 beryllium Inorganic materials 0.000 claims description 30
- 229910052759 nickel Inorganic materials 0.000 claims description 30
- 229910052684 Cerium Inorganic materials 0.000 claims description 29
- 229910052758 niobium Inorganic materials 0.000 claims description 29
- 229910052735 hafnium Inorganic materials 0.000 claims description 28
- 229910052750 molybdenum Inorganic materials 0.000 claims description 28
- 229910052715 tantalum Inorganic materials 0.000 claims description 28
- 229910052721 tungsten Inorganic materials 0.000 claims description 28
- 229910052726 zirconium Inorganic materials 0.000 claims description 28
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 27
- 229910052796 boron Inorganic materials 0.000 claims description 27
- 238000002844 melting Methods 0.000 claims description 27
- 229910052700 potassium Inorganic materials 0.000 claims description 27
- 229910052708 sodium Inorganic materials 0.000 claims description 27
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 26
- 229910052691 Erbium Inorganic materials 0.000 claims description 26
- 229910052693 Europium Inorganic materials 0.000 claims description 26
- 229910052689 Holmium Inorganic materials 0.000 claims description 26
- 229910052779 Neodymium Inorganic materials 0.000 claims description 26
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 26
- 229910052772 Samarium Inorganic materials 0.000 claims description 26
- 229910052771 Terbium Inorganic materials 0.000 claims description 26
- 229910052775 Thulium Inorganic materials 0.000 claims description 26
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 26
- 229910052749 magnesium Inorganic materials 0.000 claims description 26
- 230000008018 melting Effects 0.000 claims description 26
- 238000010298 pulverizing process Methods 0.000 claims description 26
- 229910052718 tin Inorganic materials 0.000 claims description 25
- 229910052782 aluminium Inorganic materials 0.000 claims description 24
- 229910052744 lithium Inorganic materials 0.000 claims description 24
- 229910052719 titanium Inorganic materials 0.000 claims description 24
- 229910052727 yttrium Inorganic materials 0.000 claims description 24
- 229910052738 indium Inorganic materials 0.000 claims description 23
- 229910052725 zinc Inorganic materials 0.000 claims description 23
- 229910052745 lead Inorganic materials 0.000 claims description 22
- 229910052789 astatine Inorganic materials 0.000 claims description 21
- 229910052732 germanium Inorganic materials 0.000 claims description 20
- 229910052733 gallium Inorganic materials 0.000 claims description 19
- 238000009689 gas atomisation Methods 0.000 claims description 19
- 229910052709 silver Inorganic materials 0.000 claims description 17
- 238000009692 water atomization Methods 0.000 claims description 16
- 229910052765 Lutetium Inorganic materials 0.000 claims description 14
- 239000011258 core-shell material Substances 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 13
- 229910052797 bismuth Inorganic materials 0.000 claims description 12
- 229910000765 intermetallic Inorganic materials 0.000 claims description 12
- 229910052791 calcium Inorganic materials 0.000 claims description 11
- 230000000717 retained effect Effects 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 238000009690 centrifugal atomisation Methods 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000004299 exfoliation Methods 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- 239000010936 titanium Substances 0.000 description 145
- 239000000243 solution Substances 0.000 description 49
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 24
- 230000000875 corresponding effect Effects 0.000 description 22
- 239000011734 sodium Substances 0.000 description 21
- 239000007771 core particle Substances 0.000 description 15
- 239000000155 melt Substances 0.000 description 15
- 229910052761 rare earth metal Inorganic materials 0.000 description 14
- 238000007780 powder milling Methods 0.000 description 13
- 150000002910 rare earth metals Chemical class 0.000 description 12
- 238000003723 Smelting Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 9
- 239000011858 nanopowder Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000001788 irregular Effects 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 210000001787 dendrite Anatomy 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910002555 FeNi Inorganic materials 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- 229910004356 Ti Raw Inorganic materials 0.000 description 2
- 229910010380 TiNi Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000009489 vacuum treatment Methods 0.000 description 2
- 229910016344 CuSi Inorganic materials 0.000 description 1
- 229910002062 Hf-Nb-Ta alloy Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910004688 Ti-V Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910011214 Ti—Mo Inorganic materials 0.000 description 1
- 229910010968 Ti—V Inorganic materials 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WJGAPUXHSQQWQF-UHFFFAOYSA-N acetic acid;hydrochloride Chemical compound Cl.CC(O)=O WJGAPUXHSQQWQF-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000048 melt cooling Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
-
- 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
- B22F1/054—Nanosized particles
-
- 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
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
-
- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
-
- 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
- C22C1/0425—Copper-based alloys
-
- 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
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- 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
- C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C11/00—Alloys based on lead
- C22C11/04—Alloys based on lead with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/10—Alloys based on copper with silicon as the next major constituent
-
- 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
- B22F1/17—Metallic particles coated with metal
-
- 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
- B22F2009/0824—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 with a specific atomising fluid
- B22F2009/0828—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 with a specific atomising fluid with water
-
- 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
- B22F2201/20—Use of vacuum
-
- 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
- B22F2301/10—Copper
-
- 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
- B22F2301/15—Nickel or cobalt
-
- 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
- B22F2301/35—Iron
-
- 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
- B22F2304/00—Physical aspects of the powder
- B22F2304/05—Submicron size particles
- B22F2304/054—Particle size between 1 and 100 nm
-
- 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
- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the invention relates to the technical field of micro-nano powder materials, in particular to a preparation method and application of a high-purity powder material and a dual-phase powder material.
- Atomization pulverizing method is a powder preparation method in which fast-moving fluid (atomizing medium) impacts or otherwise breaks metal or alloy liquids into fine droplets, followed by condensation into solid powders.
- Atomization pulverization methods mainly include: gas atomization, water atomization, water vapor-combined atomization, vacuum atomization, plasma atomization, centrifugal atomization, rotating disk atomization, rotating electrode atomization and ultrasonic atomization.
- the cost of obtaining a large number of ultrafine metal powders with a particle size of less than 10 ⁇ m by the atomization powder method is extremely high, and the submicron and nano powders with a size of less than 1 ⁇ m are even more difficult. It is directly obtained by the atomization pulverization method.
- the control of impurities in atomized pulverization is also a key problem that needs to be solved urgently.
- a preparation method of high-purity powder material characterized in that it comprises the following steps:
- Step 1 select the initial alloy raw material, and melt the initial alloy raw material according to the initial alloy composition ratio to obtain a uniform initial alloy melt;
- Step 2 Atomizing and solidifying the initial alloy melt through the atomization powder technology to obtain an intermediate alloy powder;
- the intermediate alloy powder is composed of a first phase and a second phase, the first phase is granular, and the second phase is granular.
- the phase is a matrix phase with a melting point lower than that of the first phase, and the particles of the first phase are coated in the matrix of the second phase;
- the impurity elements in the initial alloy melt are introduced into the process of atomization and solidification.
- the impurity elements are enriched in the second phase matrix, so that the first phase particles are purified;
- Step 3 The second phase matrix in the master alloy powder is removed and the first phase particles are retained, and the impurity elements enriched in the second phase matrix are removed accordingly, that is, high-purity particles composed of the first phase particles are obtained.
- Target metal powder material
- the impurity element in the initial alloy melt is T, and T includes at least one of O, H, N, P, S, F, Cl, I, and Br, and the total content of these impurity elements is is the content of the impurity element T;
- the source of the impurity element T in the initial alloy melt includes: impurities introduced from the initial alloy raw material, and impurities introduced from the atmosphere or the crucible during the smelting process.
- the impurities introduced into the atmosphere refer to impurities such as O, N, and H in the ambient atmosphere absorbed by the alloy melt.
- the raw material is each element or master alloy containing impurity elements, it can be melted according to the proportion to prepare the initial alloy melt. If the supplied raw material is directly the alloy raw material corresponding to the composition of the initial alloy melt, it can be remelted to obtain the initial alloy melt.
- the initial alloy raw material includes an M-T raw material containing an impurity element T.
- M is Ti and T contains O
- the M-T raw material includes Ti-O raw material containing O impurities.
- the average composition of the initial alloy melt includes any one of the following combinations (1)-(4):
- the average composition of the initial alloy melt is mainly A a (M x D y ) b T d , wherein A includes Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, At least one of Tb, Dy, Ho, Er, Tm, Yb, Lu, M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, D includes Fe, Co, At least one of Ni, wherein x, y; a, b, d represent the atomic percentage content of the corresponding constituent elements, and 0.5% ⁇ a ⁇ 99.5%, 0.5% ⁇ b ⁇ 99.5%, 0 ⁇ d ⁇ 10% ;
- A is composed of at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; preferably, M is composed of W, At least one of Cr, Mo, V, Ta, Nb, Zr, Hf, Ti is composed of; preferably, D is composed of at least one of Fe, Co, and Ni;
- the average composition of the initial alloy melt is mainly A a M b T d , wherein A includes Mg, Ca, Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm , at least one of Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti ; where a, b and d represent the atomic percentage content of the corresponding constituent elements, and 0.5% ⁇ a ⁇ 99.5%, 0.5% ⁇ b ⁇ 99.5%, 0 ⁇ d ⁇ 10%;
- A includes Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, One of Tb, Dy, Ho, Er, Tm, Yb, Lu;
- M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti
- A includes Cu
- A is composed of Mg, Ca, Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu
- M is composed of at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti;
- the average composition of the initial alloy melt is mainly A a M b T d , wherein A includes Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na , at least one of Li, M contains at least one of Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, and V, and the atomic percentage of Be, B, Si, and Ge in M
- the proportion of the total content in M is less than 50%; where a, b, d represent the atomic percentage content of the corresponding constituent elements, and 0.5% ⁇ a ⁇ 99.5%, 0.5% ⁇ b ⁇ 99.5%, 0 ⁇ d ⁇ 10% ;
- A contains at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li
- M contains Be, B, Bi, Fe, Ni, Cu, At least one of Ag, Si, Ge, Cr, and V, and when M includes Fe and Ni, M does not include Cr and V;
- A is composed of at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li;
- M is composed of Be, B, Bi, Fe, At least one composition of Ni, Cu, Ag, Si, Ge, Cr, and V, and when M includes Fe and Ni, M does not include Cr and V;
- M contains at least one of Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, and V, and the total atomic percentage content of Be, B, Si, and Ge in M is in M The proportion is less than 30%;
- A contains at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li
- M contains Be, Bi, Fe, Ni, Cu, Ag, At least one of Cr and V, wherein a, b and d represent the atomic percentage content of the corresponding constituent elements, and 0.5% ⁇ a ⁇ 99.5%, 0.5% ⁇ b ⁇ 99.5%, 0 ⁇ d ⁇ 10%;
- M contains B A contains at least one of Sn, Ge, Cu, and Zn; when M contains Bi, A contains at least one of Sn, Ga, and Al;
- M contains at least one of Fe, Ni, Cu, and Ag
- A contains at least one of La, In, Na, K, Li, Pb, and Mg
- M contains Fe, Ni
- M contains at least one of La, In, Na, K, Li, and Mg
- A contains at least one of Cu and Ag
- M contains at least one of Si and Ge
- A contains at least one of Zn, Sn, Pb, Ga, In, and Al;
- M contains at least one of Cr and V
- A contains Zn
- Combination (4) When the average composition of the initial alloy melt is mainly A a M b Al c T d , A contains Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy , at least one of Ho, Er, Tm, Yb, Lu; M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti; Al is aluminum; wherein a, b, c and d respectively represent the atomic percentage content of the corresponding constituent elements, and 0.5 ⁇ a ⁇ 99.4%, 0.5 ⁇ b ⁇ 99.4%, 0.1% ⁇ c ⁇ 25%, 0 ⁇ d ⁇ 10%;
- A is composed of at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; preferably, M is composed of W, At least one composition of Cr, Mo, V, Ta, Nb, Zr, Hf, Ti;
- the average composition of the initial alloy melt is any one of the above combinations (1)-(4);
- the combination of A and M in the average composition of the initial alloy melt in the first step is extremely important, and the selection principle is to ensure that no intermetallic compound is formed between A and M during the solidification of the alloy melt; Element (D) can form a high melting point intermetallic compound, but still no intermetallic compound is formed between A and M. In this way, the two-phase separation of the matrix phase dominated by A and the particle phase dominated by M(D) during the solidification of the initial alloy melt can be realized, which is beneficial to the subsequent preparation of powder materials dominated by M(D).
- the master alloy powder does not contain an intermetallic compound composed of A and M;
- the master alloy powder does not contain an intermetallic compound composed of A and D;
- the first phase particles and the composition of the master alloy powder are mainly (M x D y ) x1 T z1 and the main composition is A x2 T
- the second phase matrix of z2 wherein, 98% ⁇ x1 ⁇ 100%, 0 ⁇ z1 ⁇ 2%; 70% ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1 , z1, x2, and z2 respectively represent the atomic percentage content of the corresponding constituent elements;
- the first phase particles whose composition is mainly (M x D y ) x1 T z1 do not contain A element.
- the composition of the first phase particles is (M x D y ) x1 T z1 .
- the first phase particles formed in the master alloy powder are mainly composed of M x1 T z1 and the composition is mainly A x2 T
- the second phase matrix of z2 wherein, 98% ⁇ x1 ⁇ 100%, 0 ⁇ z1 ⁇ 2%; 70% ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1 , z1, x2, and z2 respectively represent the atomic percentage content of the corresponding constituent elements;
- the first phase particles whose composition is mainly M x1 T z1 do not contain A element.
- the composition of the first phase particles is M x1 T z1 .
- the master alloy powder forms the first phase particles with the main composition M x1 A y1 T z1 and the average composition mainly A x2 A y2 T
- the second phase matrix of z2 78% ⁇ x1 ⁇ 99.9%, 0.1% ⁇ y1 ⁇ 22%, 0 ⁇ z1 ⁇ 2%; 70% ⁇ x2 ⁇ 99.8%, 0.2% ⁇ y2 ⁇ 30%, 0 ⁇ z2 ⁇ 30%, z1 ⁇ d ⁇ z2, 2z1 ⁇ z2, y1 ⁇ y2, x1, y1, z1, x2, y2, z2 respectively represent the atomic percentage content of the corresponding constituent elements;
- the first phase particles whose composition is mainly M x1 Aly1 T z1 do not contain A element.
- the composition of the first phase particles is M x1 Aly1 T z1 .
- the impurity elements in the initial alloy melt are collected in the second phase matrix, so that the first phase particles are purified;
- z1 ⁇ d ⁇ z2, 3z1 ⁇ z2 preferably, z1 ⁇ d ⁇ z2, 3z1 ⁇ z2, and 0 ⁇ z1 ⁇ 1%;
- z1 ⁇ d ⁇ z2, 3z1 ⁇ z2 that is, the T impurity content in the first phase particles is lower than the T impurity content in the initial alloy melt, and the T impurity content in the first phase particles is less than 3 times is still lower than the T impurity content in the second phase matrix; preferably, z1 ⁇ d ⁇ z2, 3z1 ⁇ z2, and 0 ⁇ z1 ⁇ 1%.
- the atomic percentage content z1 of the T impurity element in the first phase particles is smaller than the atomic percentage content of the T impurity element in the M-T raw material.
- the present invention adopts the atomic percentage content to express the content of T impurity element.
- the composition of each element is characterized by the atomic percentage content of the element, and the increase or decrease of the element content, such as the increase or decrease of impurity elements, can be accurately expressed through the concept of material quantity. If the mass percentage content (or ppm concept) of elements is used to characterize the content of each element, it is easy to produce wrong conclusions due to the difference in atomic weight of each element. For example, an alloy whose atomic percent content is Ti 45 Gd 45 O 10 contains 100 atoms, and the atomic percent content of O is 10 at %.
- the 100 atoms are divided into two parts: Ti 45 O 4 (the atomic percentage composition is Ti 91.8 O 8.2 ) and Gd 45 O 6 (the atomic percentage composition is Gd 88.2 O 11.8 ), and the atomic percentage content of oxygen in Gd 45 O 6 is increased to 11.8at%, the atomic percentage of oxygen in Ti 45 O 4 is reduced to 8.2at%, which can accurately express that O is enriched in Gd.
- the mass percent content of O is used to measure, the mass percent content of O in Ti 45 Gd 45 O 10 is 1.70 wt %, and the mass percent content of O in Ti 45 O 4 and Gd 45 O 6 is 2.9 wt. % and 2.9 wt % respectively. 1.34wt.%, it would lead to the wrong conclusion that the O content in Ti 45 O 4 is significantly increased compared to that in Gd 45 O 6 .
- the atomization and pulverization technology includes gas atomization, water atomization, water vapor-combined atomization, vacuum atomization, plasma atomization, centrifugal atomization, rotating disk atomization, and rotary electrode atomization. at least one.
- the particle shape of the master alloy powder includes spherical shape, nearly spherical shape, water drop shape, dumbbell shape, and irregular rod shape.
- the initial alloy melt can obtain droplets with different particle sizes through the atomization process, and further solidify to obtain master alloy powders with different particle sizes.
- the energy of the atomizing medium is high enough, the master alloy powder with smaller particle size can be obtained, and the solidification rate of the master alloy powder is generally higher; when the energy of the atomizing medium is low, the master alloy powder with larger particle size can be obtained , and generally the solidification rate of the master alloy powder is low.
- the particle size range of the master alloy powder is 1 ⁇ m ⁇ 8mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 4mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 1mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 250 ⁇ m; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 100 ⁇ m; further, the particle size of the master alloy powder
- the diameter range is 1 ⁇ m ⁇ 50 ⁇ m; further, the particle diameter range of the master alloy powder is 1 ⁇ m ⁇ 20 ⁇ m;
- the particle size of the first phase particles in the master alloy powder is related to the atomization solidification rate of the initial alloy melt; generally, the particle size of the first phase particles in the master alloy powder is related to the initial alloy melt.
- the atomization solidification rate of the alloy is negatively correlated; that is, the higher the atomization solidification rate of the initial alloy melt, the smaller the particle size of the first phase particles in the master alloy powder.
- an intermediate alloy powder with a particle size of several hundreds of microns or millimeters can be obtained.
- the volume fraction of the first phase particles in the master alloy powder is determined by the contents of A and M in the master alloy powder; since the atomic percentage content of M in the master alloy powder is generally 0.5% ⁇ b ⁇ 99.5% Or 0.5% ⁇ b ⁇ 99.4%, the volume fraction of the first-phase particles dominated by M is also generally close to this ratio.
- volume percentage of the first phase particles in the master alloy powder ranges from 0.5% to 99.5%
- the specific value of the volume fraction of the first phase particles in the master alloy powder can be determined by the average composition of the master alloy powder, the composition of the first phase and the second phase, and the atomic weight and density of each element, and can be determined according to These parameters are obtained by calculation.
- the manner in which the first phase particles are coated in the second phase matrix includes: a mosaic structure in which a plurality of first phase particles are dispersed and distributed in the second phase matrix, or a single first phase particle is included in the second phase matrix.
- the particle size range of the first phase particles in the master alloy powder is 3 nm ⁇ 7.9 mm; further, the particle size range of the first phase particles in the master alloy powder is 3 nm ⁇ 3.9 mm; further , the particle size range of the first phase particles in the master alloy powder is 3nm ⁇ 0.95mm; further, the particle size range of the first phase particles in the master alloy powder is 3nm ⁇ 245 ⁇ m; further, the said The particle size range of the first phase particles in the master alloy powder is 3 nm to 96 ⁇ m; further, the particle size range of the first phase particles in the master alloy powder is 3 nm to 47 ⁇ m; further, in the master alloy powder The particle size of the first phase particles ranges from 3 nm to 18.5 ⁇ m;
- the b value content in the initial alloy takes a lower value, such as
- the first phase particles of the droplets in the process of atomization and solidification are mainly (M x D y ) x1 T z1 , A x1 T z1 , or A x1 Al y1 T z1 in the master alloy powder.
- the volume percentage of the ions is relatively low, and the first phase particles are easily precipitated in the form of a large number of dispersed particles and embedded in the second phase matrix.
- the first phase particles in the master alloy powder do not have enough time to grow up, and can mainly form nanoscale (such as 3nm to 100nm) or submicron.
- the first phase particles of the grade (such as 100nm ⁇ 1 ⁇ m);
- the first phase particles can grow up well, and can mainly form submicron (100nm ⁇ 1 ⁇ m) or micron (such as 1 ⁇ m to 100 ⁇ m) of the first phase particles.
- the atoms of the second phase matrix element in the master alloy powder involved in the present invention are generally larger than the atoms of the first phase particle element, so the second phase matrix can obtain a higher atomic ratio through a smaller atomic percentage. Volume percent content.
- the volume percentages in the master alloy powder are 51 vol.% and 49 vol.%, respectively.
- the main component is A a (M x D y ) b T d , A a M b T d , or A a M b Al c T d
- the b value content in the initial alloy takes a higher value, such as When 75% ⁇ b ⁇ 99.5% or 75% ⁇ b ⁇ 99.4%, the main components in the process of droplet atomization and solidification are (M x D y ) x1 T z1 , A x1 T z1 , or A x1 Al y1 T z1 .
- the volume percentage of the first phase particles in the master alloy powder is relatively high, and a large number of first phase particles precipitated during the solidification process will inevitably bridge-merge-grow; at this time, regardless of the cooling rate, the master alloy powder will After precipitation, the particles of the first phase are easily coated in the matrix of the second phase in the form of one particle or several particles after being combined.
- the first phase particles occupy the absolute dominance of the volume in the master alloy powder, and the first phase particles may only have one The form of particles is present in the master alloy powder, which forms a core-shell structure with the second phase matrix overlying the particles.
- the particle size of the individual first phase particles in the master alloy powder is only slightly smaller than the particle size of the corresponding master alloy powder.
- the particle size of the single first-phase particles inside it may be 96 ⁇ m.
- the method for removing the second phase matrix in the master alloy powder includes at least one of acid reaction removal, alkali reaction removal, and vacuum volatilization removal.
- composition and concentration of the acid solution and the alkali solution are not specifically limited, as long as the matrix phase can be removed and the first phase particle phase can be retained at the same time.
- the temperature and vacuum degree of the vacuum treatment are not specifically limited, as long as the matrix phase can be removed and the first phase particle phase can be retained at the same time.
- the method for removing the second phase matrix in the master alloy powder includes: natural oxidation-powdering and exfoliation removal of the second phase matrix.
- the second-phase matrix is an element that is easily oxidized naturally with oxygen, such as La and Ce
- the second-phase matrix can be separated from the first-phase particles through the natural oxidation-powdering process of the second-phase matrix;
- other technical means such as magnetic separation, it is possible to separate the first phase particles with magnetic properties from the natural oxides of the second phase matrix.
- the composition of the high-purity target powder material is mainly (M x D y ) x1 T z1 ;
- the high-purity target powder material whose composition is mainly (M x D y ) x1 T z1 does not contain A element.
- the composition of the high-purity target powder material is mainly (M x D y ) x1 T z1 ;
- the composition of the high-purity target powder material is mainly M x1 T z1 .
- the high-purity target powder material whose composition is mainly M x1 T z1 does not contain A element.
- the composition of the high-purity target powder material is M x1 T z1 .
- the composition of the high-purity target powder material is mainly M x1 Aly1 T z1 .
- the high-purity target powder material whose composition is mainly M x1 Aly1 T z1 does not contain A element.
- the composition of the high-purity target powder material is M x1 Aly1 T z1 .
- the particle size range of the high-purity target powder material is 3nm-7.9mm; further, the particle size range of the high-purity target powder material is 3nm-3.9mm; further, the high-purity target powder material has a particle size range of 3nm-3.9mm;
- the particle size range of the pure target powder material is 3nm-0.95mm; further, the particle size range of the high-purity target powder material is 3nm-245 ⁇ m; further, the particles of the high-purity target powder material
- the particle size range is 3nm-96 ⁇ m; further, the particle size range of the high-purity target powder material is 3nm-47 ⁇ m; further, the particle size range of the high-purity target powder material is 3nm-18.5 ⁇ m ;
- the shape of the high-purity target powder includes spherical, nearly spherical, dendritic, rod-shaped, and lath-shaped;
- the invention also relates to the application of the target powder material obtained by the above preparation method in catalytic materials, powder metallurgy, composite materials, wave absorbing materials, sterilization materials, metal injection molding, 3D printing additive manufacturing, and coatings.
- the present invention also relates to a dual-phase powder material, which is characterized in that the dual-phase powder material is in the form of powder, and a single particle of the dual-phase powder material further comprises an endogenous powder and a coating; the solidification of the dual-phase powder material
- the structure includes a matrix phase and a particle phase, the matrix phase is the coating body, and the granular phase is the endogenous powder in the dual-phase powder material; the melting point of the coating body is lower than the melting point of the endogenous powder, and the Endogenous powder is coated in the coated body;
- the chemical composition and structure of the dual-phase powder material include any one of the following four combinations:
- the composition of the endogenous powder in the dual-phase powder material is mainly (M x D y ) x1 T z1 , and the average composition of the coating is mainly A x2 T z2 ; and 98% ⁇ x1 ⁇ 100%,0 ⁇ z1 ⁇ 2%; 70% ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1, z1, x2, z2 respectively represent the atomic percentage content of the corresponding constituent elements; among them, A contains at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and M contains W, Cr, Mo, V, Ta , at least one of Nb, Zr, Hf, Ti, D includes at least one of Fe, Co, Ni; T includes at least one of O, H, N, P, S, F, Cl, I, Br species; x, y represent
- A is composed of at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; preferably, M is composed of W, At least one of Cr, Mo, V, Ta, Nb, Zr, Hf, Ti is composed of; preferably, D is composed of at least one of Fe, Co, and Ni;
- the endogenous powder does not contain A element
- the composition of the endogenous powder in the dual-phase powder material is (M x D y ) x1 T z1 , and the average composition of the coating is A x2 T z2 ;
- the composition of the endogenous powder in the dual-phase powder material is mainly M x1 T z1 , and the average composition of the coating is mainly A x2 T z2 ; and 98% ⁇ x1 ⁇ 100%, 0 ⁇ z1 ⁇ 2% ; 70% ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1, z1, x2, z2 represent the atomic percentage content of the corresponding constituent elements respectively; wherein, A contains Mg, Ca , at least one of Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, M includes W, At least one of Cr, Mo, V, Ta, Nb, Zr, Hf, Ti; T includes at least one of O, H, N, P, S, F, Cl, I, Br;
- A includes Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, One of Tb, Dy, Ho, Er, Tm, Yb, Lu;
- M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti
- A includes Cu
- A is composed of Mg, Ca, Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu
- M is composed of at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti;
- the internal raw powder of the dual-phase powder material whose composition is mainly M x1 T z1 does not contain A element;
- the composition of the endogenous powder in the dual-phase powder material is M x1 T z1 , and the average composition of the coating is A x2 T z2 ;
- the composition of the endogenous powder in the dual-phase powder material is mainly M x1 T z1 , and the average composition of the coating is mainly A x2 T z2 ; and 98% ⁇ x1 ⁇ 100%, 0 ⁇ z1 ⁇ 2% ; 70% ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1, z1, x2, z2 represent the atomic percentage content of the corresponding constituent elements respectively; wherein, A contains Zn, Mg , at least one of Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, Li, M includes Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, At least one of V, and the total atomic percentage of Be, B, Si, and Ge in M accounts for less than 50% in M; T includes O, H, N, P, S, F, Cl, I, at least one of Br;
- A contains at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li
- M contains Be, B, Bi, Fe, Ni, Cu, At least one of Ag, Si, Ge, Cr, and V, and when M includes Fe and Ni, M does not include Cr and V;
- A is composed of at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li;
- M is composed of Be, B, Bi, Fe, At least one composition of Ni, Cu, Ag, Si, Ge, Cr, and V, and when M includes Fe and Ni, M does not include Cr and V;
- M contains at least one of Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, and V, and the total atomic percentage content of Be, B, Si, and Ge in M is in M The proportion is less than 30%;
- A contains at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li
- M contains Be, Bi, Fe, Ni, Cu, Ag, At least one of Cr and V
- T includes at least one of O, H, N, P, S, F, Cl, I, and Br;
- M contains B A contains at least one of Sn, Ge, Cu, and Zn; when M contains Bi, A contains at least one of Sn, Ga, and Al;
- M contains at least one of Fe, Ni, Cu, and Ag
- A contains at least one of La, In, Na, K, Li, Pb, and Mg
- M contains Fe, Ni
- M contains at least one of La, In, Na, K, Li, and Mg
- A contains at least one of Cu and Ag
- M includes at least one of Si and Ge
- A includes at least one of Zn, Sn, Pb, Ga, In, and Al;
- M contains at least one of Cr and V
- A contains Zn
- the internal raw powder of the dual-phase powder material whose composition is mainly M x1 T z1 does not contain A element;
- the composition of the endogenous powder in the dual-phase powder material is M x1 T z1 , and the average composition of the coating is A x2 T z2 ;
- the composition of the endogenous powder in the dual-phase powder material is mainly M x1 Aly1 T z1
- the average composition of the clad is mainly A x2 A ly2 T z2
- 70% ⁇ x2 ⁇ 99.8%, 0.2% ⁇ y2 ⁇ 30%, 0 ⁇ z2 ⁇ 30%, z1 ⁇ d ⁇ z2, 2z1 ⁇ z2, y1 ⁇ y2, x1, y1, z1, x2, y2, z2 represent the atomic percentage content of the corresponding constituent elements, respectively; among them, A includes Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er , at least one of Tm, Yb, Lu; M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti; Al is aluminum; T includes
- A is composed of at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; preferably, M is composed of W, At least one composition of Cr, Mo, V, Ta, Nb, Zr, Hf, Ti;
- the endogenous powder does not contain A element
- the composition of the endogenous powder in the dual-phase powder material is M x1 A y1 T z1
- the average composition of the cladding body is A x2 A y2 T z2 ;
- the chemical composition and structure of the dual-phase powder material is any one of the four combinations described in 1)-4) above;
- the dual-phase powder material does not contain an intermetallic compound composed of A and M;
- the dual-phase powder material does not contain an intermetallic compound composed of A and D;
- the particle shape of the dual-phase powder material includes spherical, nearly spherical, drop-shaped, dumbbell-shaped, and irregular rod-shaped.
- the particle size range of the dual-phase powder material is 1 ⁇ m ⁇ 8 mm; preferably, the particle size range of the dual-phase powder material is 1 ⁇ m ⁇ 4 mm; Preferably, the particle size range of the dual-phase powder material is 1 ⁇ m-250 ⁇ m; preferably, the particle size range of the dual-phase powder material is 1 ⁇ m-100 ⁇ m; Preferably, the particle size of the dual-phase powder material ranges from 1 ⁇ m to 50 ⁇ m; preferably, the particle size of the dual-phase powder material ranges from 1 ⁇ m to 20 ⁇ m;
- the manner in which the endogenous powder is coated in the coating body in the dual-phase powder material includes: a mosaic structure in which a plurality of endogenous powders are dispersed and distributed in the coating body, or a single endogenous powder is included, The core-shell structure with the outer covering;
- the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 7.9 mm; preferably, the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 3.9 mm; Preferably, the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 0.95 mm; preferably, the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 245 ⁇ m; Preferably, the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 96 ⁇ m; preferably, the particle size of the endogenous powder in the dual-phase powder material ranges from 3 nm to 47 ⁇ m; The particle size range of the endogenous powder in the dual-phase powder material is 3 nm to 18.5 ⁇ m;
- the dual-phase powder material is prepared through steps 1 and 2 in the above-mentioned method for preparing a high-purity powder material
- volume percentage of the endogenous powder in the dual-phase powder material ranges from 0.5% to 99.5%
- the specific volume of the endogenous powder in the dual-phase powder material is 100%.
- the component content can be determined according to the average composition of the master alloy powder, combined with the composition of the endogenous powder and the cladding in the master alloy powder, as well as the atomic weight of each element and the density of each element, and can be calculated from these data.
- A, M, D or T in the solution of the present invention may also contain other elements or impurity elements other than those listed above. As long as the introduction of these elements or the changes in their contents do not cause a "qualitative change" in the solidification process and law of the initial alloy, it does not affect the realization of the above technical solutions of the present invention.
- the master alloy powder does not contain intermetallic compounds mainly composed of A and M, or A and D;
- the solidified structure in the master alloy powder includes a second phase matrix and first phase particles; the melting point of the second phase matrix is lower than that of the first phase particles, and the first phase particles are coated with the first phase particles; in the second phase matrix;
- the preparation of the target powder material is realized through two mechanisms: one is based on the basic principle of atomization powder making, and the alloy melt is broken into fine liquid by the impact of fast-moving fluid (atomizing medium)
- the second is to use the precipitation of the first phase particles of the master alloy powder in the second phase matrix during the solidification of the atomized droplets to further obtain a finer first phase. phase particles.
- the particle size of the first phase particles precipitated in the master alloy powder can reach nanoscale.
- the present invention solves the problem that it is difficult to obtain ultra-high-quality products mainly relying on the impact of the atomized medium by further utilizing the refinement principle that the first phase particles are precipitated in the second phase matrix.
- the technical difficulties of fine powder materials can greatly reduce the preparation cost of ultrafine powder materials.
- the common “dephasing method” The alloy strip is generally prepared by means such as a strip method, and then by removing the second matrix phase in the alloy strip, a powder material composed of the first phase particles detached from the alloy strip is obtained.
- the first-phase nanopowder particles are generally spherical, when the particle size of the first-phase particles is relatively large, such as micron-scale, the first-phase particles are mainly precipitated in the form of dendrite particles.
- micron-scale first-phase dendrite powder particles can be prepared by ordinary "dephasing method", and it is often difficult to prepare micron-scale spherical first-phase particles. If micron-scale spherical particles need to be obtained, the dendrite particles need to be spheroidized by means such as plasma spheroidization, which greatly increases the cost. For the "atomization powder milling + dephase method" of the present invention, this problem is well solved. When it is necessary to prepare micron spherical powder, the b value can be taken as a high value to greatly increase the volume percentage of the first phase particles in the master alloy powder, so as to obtain a single first phase particle covered by the second phase matrix.
- the spherical intermediate alloy powder with the core-shell structure and then by removing the coating of the base shell, a spherical powder material mainly composed of the first phase particles can be obtained.
- a spherical powder material mainly composed of the first phase particles can be obtained.
- the present invention skillfully combines the atomization pulverizing technology with the principle of "dephase method", and can adjust the working (impact) parameters of the atomizing medium, the cooling rate of the atomized droplets, and the b in the initial alloy (melt).
- the value can be used to control the size and morphology of the first phase particles in the master alloy powder, as well as its distribution characteristics (diffuse mosaic structure or core-shell structure) in the master alloy powder.
- nano-, sub-micron, micron, and even millimeter-scale spherical high-purity powder materials can be prepared respectively.
- phase separation occurs when the initial alloy melt solidifies, so that endogenous particles of a certain particle size target composition can be formed during the solidification process of the initial alloy melt and can be separated by subsequent processes.
- nano-metal powders can be easily prepared by bottom-up chemical methods, such as chemical reduction, but when the particle size increases to hundreds of nanometers or even micrometers, it is difficult to prepare.
- Metal particles of tens of microns or hundreds of microns can be easily prepared by top-down physical methods, such as atomization, ball milling, etc., but when the size of the particles is reduced to hundreds of nanometers to several microns, It is also difficult to prepare.
- the technical scheme of the present invention can easily prepare nano-, sub-micron, micron, and even millimeter-scale target powder materials according to the different cooling rates in the solidification process of the master alloy powder, combined with the powdering mechanism of the atomization method itself , which breaks through the above technical difficulties and has great advantages.
- high-purity target powder materials can be obtained from low-purity raw materials, and a new way is pointed out for the preparation of high-purity powder materials from low-purity raw materials, which greatly reduces the cost and is very creative.
- the improvement of the purity of the target powder material of the present invention is mainly achieved through the following mechanisms: 1) The "absorption" effect of the matrix main elements (such as RE rare earth elements) with high activity and low melting point on the impurity elements in the initial alloy melt. Since the matrix element is generally a highly active, low melting point element, it has a strong affinity with the impurity element T during the melting and solidification of the alloy melt, which can make the impurity element T in the initial alloy melt more It enters into the second phase matrix mainly composed of the main elements of the matrix phase, or forms slag with the main elements of the matrix in the melt state, and separates and removes it from the alloy melt; 2) The target powder material (the endogenous precipitation During the nucleation and growth of the first-phase particles), the impurity element T will be discharged into the remaining melt.
- the matrix main elements such as RE rare earth elements
- the impurities related to the crucible entering the melt due to the interaction between the crucible and the melt during the smelting process are generally concentrated in the second phase matrix, which makes the requirements for the crucible during the smelting process. Further reduction, greatly reducing the production cost.
- the gas impurity elements introduced through the atmosphere during the atomization and solidification process are also absorbed by the matrix phase, and it is difficult to enter the first phase particles, thereby further affecting the first phase particles.
- low-purity raw materials such as sponge Ti
- high-purity target metal powder materials such as high-purity Ti powder.
- the master alloy powder is composed of the second phase matrix covering the first phase particles.
- the first phase particles in the atomized droplets tend to be spherical. , nearly spherical, or dendrites grow out of the melt. Due to the coating of the second phase matrix, the first phase particles have a smoother outer surface than the master alloy powder.
- the value of b in the initial alloy A a (M x D y ) b T d , A a M b T d , or A a M b Al c T d takes a lower value, the first phase particles are uniform dispersed in the second phase matrix.
- the target powder material with high surface quality can be obtained by removing the matrix phase.
- the dual-phase powder material composed of the endogenous powder and the coating body creatively uses the in-situ-generated matrix phase coating body to wrap the endogenous powder, maintaining the high purity and high activity of the endogenous powder.
- metal or alloy powders prepared by traditional chemical methods or physical methods, especially nano-powders with extremely large specific surface areas, are easily oxidized naturally and face the problem of difficulty in powder preservation.
- the technical solution of the present invention does not rush to remove the coating, but directly uses the coating The body protects the endogenous metal powder from natural oxidation.
- This dual-phase powder material composed of endogenous powder and coating can be directly used as a raw material for downstream production, so it has the potential to become a special product.
- the downstream production needs to use high-purity powder to form a material, according to the characteristics of the next process, you can choose a suitable time and "release" the endogenous metal powder from the dual-phase powder material under a suitable environment, and then as far as possible In a short time, the released endogenous powder enters the next production process, so that the chance of endogenous meal being polluted by impurities such as oxygen is greatly reduced.
- the endogenous powder when the endogenous powder is nano-powder, the endogenous powder can be compounded with resin at the same time as the endogenous powder is released from the encapsulation body or immediately afterward, so as to prepare a resin-based composite material with high activity endogenous powder added.
- the first phase particles in the obtained master alloy powder are also composed of various elements, which makes the preparation of the target alloy powder material composed of the first phase particles more convenient and feasible, and greatly expands the target alloy powder.
- the composition range and application area of the material are also composed of various elements, which makes the preparation of the target alloy powder material composed of the first phase particles more convenient and feasible, and greatly expands the target alloy powder.
- the preparation method of the present invention adopts the combination method of "atomization powder milling + dephase method", which has the characteristics of simple process, easy operation and low cost, and can prepare nanoscale, submicron, micron, and even millimeter scales.
- atomization powder milling + dephase method which has the characteristics of simple process, easy operation and low cost, and can prepare nanoscale, submicron, micron, and even millimeter scales.
- high-purity powder materials which have good application prospects in the fields of catalytic materials, powder metallurgy, composite materials, wave absorbing materials, sterilization materials, metal injection molding, 3D printing additive manufacturing, coatings and other fields.
- the present invention also relates to a preparation method of a high-purity powder material, characterized in that it comprises the following steps:
- Step 1 select the initial alloy raw material, and melt the initial alloy raw material according to the initial alloy composition ratio to obtain a uniform initial alloy melt;
- Step 2 Atomizing and solidifying the initial alloy melt through the atomization powder technology to obtain an intermediate alloy powder;
- the intermediate alloy powder is composed of a first phase and a second phase, the first phase is granular, and the second phase is granular.
- the phase is a matrix phase with a melting point lower than that of the first phase, and the particles of the first phase are coated in the matrix of the second phase;
- the impurity elements in the initial alloy melt are introduced into the process of atomization and solidification.
- the impurity elements are enriched in the second phase matrix, so that the first phase particles are purified;
- Step 3 The second phase matrix in the master alloy powder is removed and the first phase particles are retained, and the impurity elements enriched in the second phase matrix are removed accordingly, that is, high-purity particles composed of the first phase particles are obtained.
- target powder material
- the impurity element in the initial alloy melt is T, and T includes at least one of O, H, N, P, S, F, Cl, I, and Br;
- the average composition of the initial alloy melt is mainly A a M b T d ,
- A includes at least one of Zn, Sn, Pb, Ga, In, Al, Ge, Cu;
- M includes Be, Si, Ge, B At least one of them, and the atomic percent content of Be, Si, Ge, and B in M is greater than or equal to 50%, where a, b, and d represent the atomic percent content of the corresponding constituent elements, and 0.5% ⁇ a ⁇ 99.5%, 0.5% ⁇ b ⁇ 99.5%, 0 ⁇ d ⁇ 10%;
- M contains at least one of Be, Si, Ge, and B, and the atomic percentage content of Be, Si, Ge, and B in M is greater than or equal to 70%;
- the average composition of the initial alloy melt is mainly A a M b T d , and when M includes at least one of Be, Si, and Ge, A includes Zn, Sn, Pb, Ga, In, Al At least one of; when M includes B, A includes at least one of Sn, Ge, Cu, and Zn;
- the master alloy powder includes first-phase particles mainly composed of M x1 T z1 and a second phase matrix mainly composed of A x2 T z2 ; wherein, 98% ⁇ x1 ⁇ 100%, 0 ⁇ z1 ⁇ 2%; 70 % ⁇ x2 ⁇ 100%, 0 ⁇ z2 ⁇ 30%; z1 ⁇ d ⁇ z2, 2z1 ⁇ z2; x1, z1, x2, z2 respectively represent the atomic percentage content of the corresponding constituent elements;
- first phase particles whose composition is mainly M x1 T z1 do not contain A element
- composition of the first phase particles is M x1 T z1 ;
- the impurity elements in the initial alloy melt are collected in the second phase matrix, so that the first phase particles are purified;
- the atomization and pulverization technology includes gas atomization, water atomization, water vapor-combined atomization, vacuum atomization, plasma atomization, centrifugal atomization, rotating disk atomization, and rotary electrode atomization. at least one.
- the particle shape of the master alloy powder includes spherical shape, nearly spherical shape, water drop shape, dumbbell shape, and irregular rod shape.
- the initial alloy melt can obtain droplets with different particle sizes through the atomization process, and further solidify to obtain master alloy powders with different particle sizes.
- the energy of the atomizing medium is high enough, the master alloy powder with smaller particle size can be obtained, and the solidification rate of the master alloy powder is generally higher; when the energy of the atomizing medium is low, the master alloy powder with larger particle size can be obtained , and generally the solidification rate of the master alloy powder is low.
- the particle size range of the master alloy powder is 1 ⁇ m ⁇ 8mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 4mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 1mm; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 250 ⁇ m; further, the particle size range of the master alloy powder is 1 ⁇ m ⁇ 100 ⁇ m; further, the particle size of the master alloy powder
- the diameter range is 1 ⁇ m ⁇ 50 ⁇ m; further, the particle diameter range of the master alloy powder is 1 ⁇ m ⁇ 20 ⁇ m;
- the particle size of the first phase particles in the master alloy powder is related to the atomization solidification rate of the initial alloy melt; generally, the particle size of the first phase particles in the master alloy powder is related to the initial alloy melt.
- the atomization solidification rate of the alloy is negatively correlated; that is, the higher the atomization solidification rate of the initial alloy melt, the smaller the particle size of the first phase particles in the master alloy powder.
- an intermediate alloy powder with a particle size of several hundreds of microns or millimeters can be obtained.
- the volume fraction of the first phase particles in the master alloy powder is determined by the contents of A and M in the master alloy powder; since the atomic percentage content of M in the master alloy powder is generally 0.5% ⁇ b ⁇ 99.5% Or 0.5% ⁇ b ⁇ 99.4%, the volume fraction of the first phase particles dominated by M is also generally close to this ratio, and the specific value can be obtained by calculating the atomic weight and density of each element.
- volume percentage of the first phase particles in the master alloy powder ranges from 0.5% to 99.5%
- the specific value of the volume fraction of the first phase particles in the master alloy powder can be determined by the average composition of the master alloy powder, the composition of the first phase and the second phase, and the atomic weight and density of each element, and can be determined according to These parameters are obtained by calculation.
- the manner in which the first phase particles are coated in the second phase matrix includes: a mosaic structure in which a plurality of first phase particles are dispersed and distributed in the second phase matrix, or a single first phase particle is included in the second phase matrix.
- the particle size range of the first phase particles in the master alloy powder is 3 nm ⁇ 7.9 mm; further, the particle size range of the first phase particles in the master alloy powder is 3 nm ⁇ 3.9 mm; further , the particle size range of the first phase particles in the master alloy powder is 3nm ⁇ 0.95mm; further, the particle size range of the first phase particles in the master alloy powder is 3nm ⁇ 245 ⁇ m; further, the said The particle size range of the first phase particles in the master alloy powder is 3 nm to 96 ⁇ m; further, the particle size range of the first phase particles in the master alloy powder is 3 nm to 47 ⁇ m; further, in the master alloy powder The particle size of the first phase particles ranges from 3 nm to 18.5 ⁇ m;
- the method for removing the second phase matrix in the master alloy powder includes at least one of acid reaction removal, alkali reaction removal, and vacuum volatilization removal.
- composition and concentration of the acid solution and the alkali solution are not specifically limited, as long as the matrix phase can be removed and the first phase particle phase can be retained at the same time.
- the temperature and vacuum degree of the vacuum treatment are not specifically limited, as long as the matrix phase can be removed and the first phase particle phase can be retained at the same time.
- the high-purity target powder material whose composition is mainly M x1 T z1 does not contain A element.
- the composition of the high-purity target powder material is M x1 T z1 .
- the particle size range of the high-purity target powder material is 3nm-7.9mm; further, the particle size range of the high-purity target powder material is 3nm-3.9mm; further, the high-purity target powder material has a particle size range of 3nm-3.9mm;
- the particle size range of the pure target powder material is 3nm-0.95mm; further, the particle size range of the high-purity target powder material is 3nm-245 ⁇ m; further, the particles of the high-purity target powder material
- the particle size range is 3nm-96 ⁇ m; further, the particle size range of the high-purity target powder material is 3nm-47 ⁇ m; further, the particle size range of the high-purity target powder material is 3nm-18.5 ⁇ m ;
- the shape of the high-purity target powder includes spherical, nearly spherical, dendritic, rod-shaped, and lath-shaped;
- the present invention also provides a method for preparing a high-purity metal powder material, which is characterized by:
- Step 1 Select the initial alloy raw material, and melt the initial alloy raw material according to the initial alloy composition ratio to obtain a uniform initial alloy melt;
- Step 2 Atomizing and solidifying the initial alloy melt by the atomization powder technology to obtain a master alloy powder;
- the master alloy powder is composed of a first phase and a second phase, the first phase is granular, and the second phase is granular.
- the phase is a matrix phase with a melting point lower than that of the first phase, and the particles of the first phase are coated in the matrix of the second phase;
- the impurity elements in the initial alloy melt are introduced into the process of atomization and solidification.
- the impurity elements are enriched in the second phase matrix, so that the first phase particles are purified;
- Step 3 The second phase matrix in the master alloy powder is removed and the first phase particles are retained, and the impurity elements enriched in the second phase matrix are removed accordingly, that is, high-purity particles composed of the first phase particles are obtained.
- Target metal powder material
- the preparation of ultrafine metal powder with low impurity content can be achieved by the above-mentioned "atomization powder milling + dephase method".
- preliminary refinement can be carried out through the preparation of master alloy powder; at the same time, through the formation of first phase particles in master alloy powder, a plurality of finer first phases can be further obtained particles, including nanoscale first phase particles.
- ultra-fine target metal powder By further removing the second phase matrix, ultra-fine target metal powder can be obtained, which greatly reduces the preparation cost of the ultra-fine metal powder material.
- the impurity elements are enriched in the second phase matrix in the process of alloy smelting and atomization, so that the first phase particles can be purified and protected, which further reduces the high Production cost of pure target metal powder.
- the initial alloy raw material is selected according to the initial alloy composition ratio, and the initial alloy raw material can be a simple metal or an intermediate alloy.
- the initial alloy raw material ensures that the melt is completely homogenized during the melting process, so as to facilitate the smooth progress of subsequent atomization and powdering.
- A is selected from Mg, Ca, Li, Na, K, Zn, In, Sn, Pb, Ga, Cu, Y, La, Ce, Pr, Nd , at least one of Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu
- A is selected from Mg, Ca, Li, Na, K, Zn, Pb, Sn, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, At least one of Yb, Lu, M is selected from at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, Fe, Co, Ni, Cu, Ag, Si, Ge; as Preferably, 40% ⁇ b ⁇ 98%; as a further preference, 45% ⁇ b ⁇ 98%.
- A is selected from Mg, Ca, Li, Na, K, Zn, In, Sn, Pb, Ga, Y, La, Ce, Pr, Nd , at least one of Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Al is aluminum
- A is selected from at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and M is selected from W, Cr, At least one of Mo, V, Ta, Nb, Zr, Hf, Ti, Fe, Co, and Ni; preferably, 35% ⁇ b ⁇ 98%; more preferably, 40% ⁇ b ⁇ 98%.
- the atomization pulverizing technology includes gas atomization, water atomization, water vapor-combined atomization, vacuum atomization, plasma atomization, centrifugal atomization, rotating disk atomization, rotating electrode atomization and ultrasonic atomization at least one of them.
- the particle size of the master alloy powder ranges from 1 ⁇ m to 8 mm; the particle shapes of the master alloy powder include spherical, nearly spherical, drop-shaped, dumbbell-shaped, and irregular rod-shaped.
- volume fraction of the first phase particles in the master alloy powder ranges from 0.5% to 98%.
- the manner in which the first phase particles are coated in the second phase matrix includes: a core-shell structure with a single first phase particle inside and the second phase matrix outside; or a dispersed distribution of a plurality of first phase particles The mosaic structure in the second phase matrix.
- the impurity elements in the initial alloy melt and the impurity elements introduced in the process of atomization and solidification include at least one of H, O, N, S, P, F, Cl, I, and Br.
- the impurity elements in the initial alloy melt come from the initial alloy raw materials, or are introduced into the crucible or atmosphere in contact with the melt during the alloy melting process; the impurities introduced during the atomization and solidification process are mainly introduced through the atomizing atmosphere and the atomizing medium.
- the method for removing the second phase matrix in the master alloy powder includes at least one of acid reaction removal, alkali reaction removal, and vacuum volatilization removal.
- the method for removing the second phase matrix in the master alloy powder includes: natural oxidation-powdering and exfoliation removal of the second phase matrix.
- the particle size range of the high-purity target metal powder material composed of the first phase particles is 3 nm to 300 ⁇ m; the shape of the high-purity target metal powder includes spherical, nearly spherical, dendrite, and rod. Shaped, slatted.
- the target metal powder material is classified and sieved according to different particle sizes, so as to obtain a target metal powder material with a narrower particle size range.
- the total content of H, O, N, S, P, F, Cl, I, and Br in the high-purity target metal powder material is lower than 2000 ppm.
- step 2 of the present invention fine first-phase particles are obtained through two mechanisms: one is based on the basic principle of atomization powder milling, and the alloy melt is broken into The fine droplets are then condensed into a certain particle size of the master alloy powder; the second is to use the precipitation of the first phase particles in the second phase matrix during the solidification of the atomized droplets to further obtain a finer first phase. particles. Therefore, on the basis of the impact of the atomized medium on the melt, the present invention solves the problem that it is difficult to obtain ultra-high-quality products mainly relying on the impact of the atomized medium by further utilizing the refinement principle that the first phase particles are precipitated in the second phase matrix.
- the technical difficulties of fine powder materials can greatly reduce the preparation cost of ultrafine metal powder materials.
- the content of b value in the initial alloy A a M b or A a M b Al c takes a lower value, such as 0.5% ⁇ b ⁇ 50%
- the composition of the atomized droplets during solidification is mainly composed of A Or the content of the second phase matrix composed of A x2 A y2 is higher. Since the solidification process of atomized droplets generally corresponds to a high melt cooling rate, when the second phase content is high, the first phase particles are easily precipitated in the form of a large number of dispersed particles and embedded in the second phase matrix.
- the first phase particles do not have time to grow sufficiently, and can mainly form nano-scale (such as 3 nm to 3 nm to 100 ⁇ m). 100nm) or submicron (such as 100nm ⁇ 1 ⁇ m) first phase particles; when the cooling rate of the atomized droplets is lower than 10 3 K/s and the particle size range of the corresponding master alloy powder is 100 ⁇ m ⁇ 8mm, the first phase particles are The phase particles can grow up well, and can mainly form the first phase particles of submicron scale (100 nm ⁇ 1 ⁇ m) or micron scale.
- the composition of the atomized droplet during solidification is mainly composed of M or M x1 Al
- the content of the first phase particles composed of y1 is relatively high. Since a large number of first-phase particles precipitated during the solidification process will inevitably bridge-merge-grow, no matter what the cooling rate is, the first-phase particles in the master alloy powder are likely to be separated by one particle or several particles after precipitation. is encapsulated in the second phase matrix.
- the first phase particles are absolutely dominant in the master alloy powder, and the first phase particles can exist in the master alloy powder in the form of only one particle , which forms a core-shell structure with the second phase matrix that coats the particles.
- the master alloy powder with a particle size range of 1 ⁇ m to 300 ⁇ m can be prepared by the existing atomization powder milling technology
- the present invention can also use the atomization powder milling technology to prepare a particle size range equivalent to that. Master alloy powder in which the first phase particles are only slightly smaller than the master alloy powder.
- the present invention can control the size of the first phase particles in the master alloy powder and the size of the first phase particles in the master alloy powder by adjusting the working (impact) parameters of the atomizing medium, the cooling rate of the atomized droplets, and the b value in the initial alloy formulation. distribution characteristics (mosaic structure or core-shell structure).
- nanoscale, submicron, and micron-scale metal powders can be prepared respectively.
- the master alloy powder is composed of the second phase matrix covering the first phase particles.
- the first phase particles in the atomized droplets tend to be spherical, Near-spherical, or dendrite-like precipitation grows from the matrix phase that has not yet fully solidified. Due to the coating of the second phase matrix, the first phase particles have a smoother outer surface than the master alloy powder.
- the content of b value in the initial alloy A a M b or A a M b Al c takes a lower value, such as 0.5% ⁇ b ⁇ 50%, a large number of first-phase particles are dispersed and distributed with the second-phase matrix middle. In this case, even if the shape of the prepared master alloy powder is extremely irregular and the surface smoothness is extremely poor, it will not affect the first phase particles dispersed and precipitated therein to obtain higher sphericity and surface smoothness.
- the second phase matrix in the master alloy powder is generally composed of elements with low melting point and high activity. Therefore, in the process of atomization and solidification, the impurity elements in the melt are easily combined with the second phase matrix to be enriched in the second phase matrix, thereby purifying and protecting the first phase particles.
- the impurities related to the crucible entering the melt due to the interaction between the crucible and the melt during the smelting process are generally concentrated in the second phase matrix, which makes the requirements for the crucible during the smelting process. Further reduction, greatly reducing the production cost.
- the gas impurity elements introduced through the atmosphere during the atomization and solidification process are also absorbed by the matrix phase, and it is difficult to enter the first phase particles, which further plays a role in preventing the first phase particles.
- Protective effects due to the protective effect of the second phase matrix, in the preparation process of the master alloy powder, even if non-high-purity raw materials and ordinary crucibles are used, or other impurity elements enter the melt during the smelting process and the atomizing powder spraying process, the The first phase particles with low impurity content can be obtained, which greatly reduces the production cost of the target high-purity metal powder material.
- the first phase particles in the obtained master alloy powder are also composed of multiple elements, which makes The preparation of the target alloy powder material composed of the first phase particles becomes more convenient and feasible, which greatly expands the composition range and application field of the target alloy powder material.
- the second phase matrix in the master alloy powder is a low melting point and high activity component
- the second phase matrix can be removed by at least one of the following three methods, and the second phase matrix can be retained.
- First-phase particles 1) The second-phase matrix is removed by etching with an acid solution or an alkaline solution, while retaining the first-phase particles; 2) The low-melting-point second-phase matrix is volatilized and removed by vacuum volatilization, while retaining the first-phase matrix 3)
- the second-phase matrix that is easily oxidized, such as the second-phase matrix whose main component is rare earth elements
- the second-phase matrix can also be turned into powder by natural oxidation-powdering of the matrix elements.
- the pulverized oxide powder is then further separated from the first phase particles and the matrix pulverized product to obtain the target metal powder material.
- the preparation method of the alternative invention adopts the combination method of "atomization powder milling + dephasing method", which has the characteristics of simple process, easy operation and low cost, and can prepare nano-, sub-micron and micron-scale multi-materials. It is a high-purity metal powder material with good application prospects in catalysis, powder metallurgy, composite materials, sterilization, metal injection molding, 3D printing, and other additive manufacturing fields.
- the present embodiment provides a preparation method of nano-CrV powder, and the preparation method comprises the following steps:
- the solidification structure of the master alloy powder is composed of a second phase matrix with a composition of Zn and a large number of first-phase high-melting-point particles with a composition of Cr 50 V 50 scattered and embedded on the Zn matrix, wherein the shape of the Cr 50 V 50 particles is close to Spherical, with particle size ranging from 3nm to 300nm.
- the volume content of Cr 50 V 50 particles in the master alloy powder is about 38%; impurities are enriched in the Zn matrix during solidification.
- the Zn in the master alloy powder is volatilized and removed by the method of vacuum heat treatment, so that the Cr 50 V 50 particles that are difficult to volatilize in the master alloy powder are detached, and the nano-Cr 50 V 50 powder is obtained, and the particle size range is 3nm ⁇ 300nm, And the total content of H, O, N, S, P, F, Cl, I, and Br in the nano-Cr 50 V 50 powder is less than 1500 ppm.
- the present embodiment provides a preparation method of nano-CrV powder, and the preparation method comprises the following steps:
- the solidification structure of the master alloy powder is composed of a second phase matrix with a composition of Zn and a large number of first-phase high-melting-point particles with a composition of Cr 50 V 50 scattered and embedded on the Zn matrix, wherein the shape of the Cr 50 V 50 particles is close to Spherical, with particle size ranging from 3nm to 200nm.
- the volume content of Cr 50 V 50 particles in the master alloy powder is about 17.5%; the impurities are enriched in the Zn matrix during solidification.
- the Zn in the master alloy powder is reacted and removed by the sodium hydroxide solution, so that the Cr 50 V 50 particles in the master alloy powder that do not react with alkali are separated out, that is, the nano-Cr 50 V 50 powder is obtained, and its particle size ranges from 3 nm to 3 nm. 200nm, and the total content of H, O, N, S, P, F, Cl, I, and Br in the nano-Cr 50 V 50 powder is less than 1600 ppm.
- the present embodiment provides a preparation method of submicron-micron Nb powder, and the preparation method includes the following steps:
- the alloy whose atomic ratio formula is Cu 54 Nb 46 is selected, and the raw materials are weighed according to the formula. After the initial alloy raw material is melted uniformly, the alloy melt is atomized and solidified by the gas atomization powder technology, and the particle size range is obtained.
- the solidification structure of the master alloy powder is composed of a second phase matrix with a composition of Cu and a large amount of first phase high melting point particles with a composition of Nb and dispersed on the Cu matrix, wherein the shape of the Nb particles is nearly spherical, and the particle size ranges It is 50nm ⁇ 5 ⁇ m.
- the volume content of Nb particles in the master alloy powder is about 46%; impurities are enriched in the Cu matrix during solidification.
- the Cu in the master alloy powder is removed by the hydrochloric acid solution, so that the Nb particles that are difficult to react with the hydrochloric acid solution in the master alloy powder are separated, and the Nb powder is obtained, the particle size of which ranges from 50 nm to 5 ⁇ m, and the H,
- the total content of O, N, S, P, F, Cl, I and Br is less than 1400ppm.
- the present embodiment provides a preparation method of micron FeNi powder, and the preparation method comprises the following steps:
- the alloy whose atomic ratio formula is Li 10 (Fe 50 Ni 50 ) 90 is selected, the raw materials are weighed according to the formula, and after the initial alloy raw material is melted uniformly, the alloy melt is atomized and solidified by vacuum air atomization pulverizing technology. , to obtain nearly spherical master alloy powder with a particle size range of 3 ⁇ m to 120 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix shell with Li composition and a first phase high melting point core particle with Fe 50 Ni 50 composition.
- the shape of Fe 50 Ni 50 particles is nearly spherical, and the particle size ranges from 2 ⁇ m to 110 ⁇ m.
- the volume content of FeNi particles in the master alloy powder is about 82%; impurities are enriched in the Li matrix shell during solidification.
- the Fe 50 Ni 50 particles are separated from the oxides after lithium pulverization through the natural oxidation-powdering process of Li in the air and the magnetic properties of the Fe 50 Ni 50 particles to obtain the micron Fe 50 Ni 50 particles with the particle size of the Fe 50 Ni 50 particles.
- the range is 2 ⁇ m ⁇ 110 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I, Br in the micron Fe 50 Ni 50 powder is less than 1800ppm.
- This embodiment provides a preparation method of micron Fe-Cr-V-Ti-Mo powder, and the preparation method includes the following steps:
- the Fe 20 Cr 20 V 20 Ti 20 Mo 20 particles are nearly spherical in shape, and the particle size ranges from 2 ⁇ m to 144 ⁇ m.
- the volume content of Fe 20 Cr 20 V 20 Ti 20 Mo 20 particles in the master alloy powder is about 78%; impurities are enriched in the La matrix shell during solidification.
- the La matrix in the master alloy powder is removed by the dilute hydrochloric acid solution, so that the Fe 20 Cr 20 V 20 Ti 20 Mo 20 particles in the master alloy powder that are difficult to react with the dilute hydrochloric acid solution are separated out, that is, the micron Fe 20 Cr 20 V 20 is obtained.
- Ti 20 Mo 20 particles have a particle size range of 2 ⁇ m to 144 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I and Br in Fe 20 Cr 20 V 20 Ti 20 Mo 20 powder is low at 1800ppm.
- the present embodiment provides a preparation method of micron Ti powder, and the preparation method comprises the following steps:
- the alloy whose atomic ratio formula is Ce 25 Ti 75 is selected, and the raw materials are weighed according to the formula. After the initial alloy raw material is melted uniformly, the alloy melt is atomized and solidified by gas atomization powder making technology, and the particle size range is obtained.
- the solidified structure of the master alloy powder is composed of a second phase matrix whose composition is Ce and a plurality of first phase high melting point dispersed particles whose composition is Ti.
- the shape of the Ti particles is nearly spherical or dendritic, and the particle size ranges from 2 ⁇ m to 50 ⁇ m.
- the volume content of Ti particles in the master alloy powder is about 61%; the titanium raw material, impurities introduced in the smelting process and impurities introduced by the atomizing atmosphere are enriched in the Ce matrix.
- the Ce matrix in the master alloy powder is removed by the dilute acid solution, so that the Ti particles in the master alloy powder that are difficult to react with the dilute acid solution are detached, that is, the micron Ti powder finer than the master alloy powder is obtained. 2 ⁇ m ⁇ 50 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I and Br in the micron Ti powder is less than 1500ppm.
- This embodiment provides a preparation method of micron-scale Ti-Zr-Hf-Nb-Ta high-entropy powder, and the preparation method includes the following steps:
- the alloy whose atomic ratio formula is Ce 10 (Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 ) 90 weigh the raw materials according to the formula, and after the initial alloy raw material is melted uniformly, the alloy melt is atomized by water atomization pulverizing technology. It is made to solidify, and a near spherical master alloy powder with a particle size ranging from 3 ⁇ m to 150 ⁇ m is obtained.
- the solidification structure of the master alloy powder is composed of a matrix shell with a composition of Ce and a high-melting core particle with a composition of Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 .
- the shape of the Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 particles is nearly spherical, and the particle size ranges from 2 ⁇ m to 142 ⁇ m.
- the volume content of Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 particles in the master alloy powder is 84%; impurities are enriched in the Ce matrix shell during solidification.
- the Ce in the master alloy powder is removed by the dilute acid solution, so that the Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 particles in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, the micron Ti 20 Zr 20 Hf 20 Nb 20 is obtained.
- Ta 20 powder its particle size range is 2 ⁇ m ⁇ 142 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I, Br in the micron Ti 20 Zr 20 Hf 20 Nb 20 Ta 20 powder is less than 1500ppm.
- This embodiment provides a preparation method of micron-scale TiNi powder, and the preparation method comprises the following steps:
- the solidified structure of the master alloy powder is composed of a matrix phase whose composition is Gd and a plurality of high-melting-point dispersed particles whose composition is Ti 50 Ni 50 .
- the shape of the Ti 50 Ni 50 particles is nearly spherical or dendritic, and the particle size ranges from 2 ⁇ m to 50 ⁇ m.
- the volume content of Ti 50 Ni 50 particles in the master alloy powder is 56%; impurities are enriched in the Gd matrix during solidification.
- the Gd in the master alloy powder is removed by the dilute acid solution, so that the Ti 50 Ni 50 particles in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, the micron Ti 50 Ni 50 powder finer than the master alloy powder is obtained.
- the composition is Ti 50 Ni 50 , the particle size ranges from 2 ⁇ m to 50 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I and Br in the micron Ti 50 Ni 50 powder is less than 1400 ppm.
- This embodiment provides a preparation method of micron Fe-Cr-Ti powder, and the preparation method includes the following steps:
- the solidification structure of the master alloy powder is composed of the second phase matrix shell with the composition La and the first phase high melting point inner core particles with the composition Fe 79 Cr 20 Ti 1 .
- the shape of Fe 79 Cr 20 Ti 1 particles is nearly spherical, and the particle size ranges from 2.9 ⁇ m to 147 ⁇ m.
- the volume content of Fe 79 Cr 20 Ti 1 particles in the master alloy powder is about 94%; impurities are enriched in the La matrix shell during solidification.
- the La matrix in the master alloy powder is reacted and removed by the dilute hydrochloric acid solution, so that the Fe 79 Cr 20 Ti 1 particles in the master alloy powder that are difficult to react with the dilute hydrochloric acid solution are detached, that is, the micron Fe 79 Cr 20 Ti 1 particles are obtained.
- the diameter ranges from 2.9 ⁇ m to 147 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I and Br in the micron Fe 79 Cr 20 Ti 1 powder is less than 1800 ppm.
- This embodiment provides a preparation method of micron-scale Ti-Al-V powder, and the preparation method includes the following steps:
- the solidified structure of the master alloy powder is composed of a second phase matrix with an average composition of Ce 85 Al 15 and a plurality of first phase high melting point dispersed particles with a composition of (Ti 96 V 4 ) 90 Al 10 .
- the shape of the (Ti 96 V 4 ) 90 Al 10 particles is nearly spherical or dendritic, and the particle size ranges from 1 ⁇ m to 50 ⁇ m.
- the volume content of (Ti 96 V 4 ) 90 Al 10 particles in the master alloy powder is about 52%; impurities are enriched in the Ce 85 Al 15 matrix during solidification.
- the Ce 85 Al 15 matrix phase in the master alloy powder is removed by the dilute hydrochloric acid solution, so that the (Ti 96 V 4 ) 90 Al 10 particles in the master alloy powder that are difficult to react with the dilute hydrochloric acid solution are detached, that is, a higher ratio of the master alloy powder is obtained.
- the finer (Ti 96 V 4 ) 90 Al 10 powder has a particle size range of 1 ⁇ m to 50 ⁇ m, and the H, O, N, S, P, F, The total content of Cl, I and Br is less than 1400ppm.
- This embodiment provides a preparation method of micron-scale Fe-Cr-Nb-Mo-Ti-V powder, and the preparation method includes the following steps:
- An alloy whose atomic ratio formula is La 25 (Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 ) 75 is selected, and the raw materials are weighed according to the formula.
- the bulk is atomized and solidified to obtain nearly spherical master alloy powder with a particle size ranging from 2 ⁇ m to 150 ⁇ m.
- the solidified structure of the master alloy powder is composed of a second phase matrix with a composition of La and a plurality of first-phase high melting point dispersed particles with a composition of Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 .
- the shape of Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 particles is nearly spherical or dendritic, and the particle size ranges from 1 ⁇ m to 50 ⁇ m.
- the volume content of Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 particles in the master alloy powder is about 50%; impurities are enriched in La matrix during solidification.
- the La in the master alloy powder is removed by the dilute hydrochloric acid solution, so that the Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 particles with high Cr content in the master alloy powder that are difficult to react with the dilute hydrochloric acid solution are separated out, that is to say, the result is that the Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 particles in the master alloy powder are more Fine Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 powder with particle size ranging from 1 ⁇ m to 50 ⁇ m, and H, O, N, S in the micron Fe 76 Cr 16 Nb 2 Mo 2 Ti 2 V 2 powder , P, F, Cl, I, Br total content less than 1400ppm.
- This embodiment provides a preparation method of micron-scale Fe-Cr-Mo-Ti powder, and the preparation method includes the following steps:
- Fe 76 Cr 20 Mo 2 Ti 2 particles with high Cr content in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, the micron finer than the master alloy powder is obtained.
- Fe 76 Cr 20 Mo 2 Ti 2 powder has a particle size range of 2 ⁇ m to 50 ⁇ m, and H, O, N, S, P, F, Cl, I, Br in the micron Fe 76 Cr 20 Mo 2 Ti 2 powder The total content is less than 1800ppm.
- This embodiment provides a preparation method of micron-scale Fe-Cr-C powder, and the preparation method includes the following steps:
- An alloy with an atomic ratio formula of La 2.5 (Fe 84.9 Cr 15 C 0.1 ) 97.5 is selected, the raw materials are weighed according to the formula, and the initial alloy raw materials are melted uniformly, and the alloy melt is atomized and made by water atomization powder technology. After solidification, a near-spherical master alloy powder with a particle size range of 3 ⁇ m to 150 ⁇ m is obtained.
- the solidification structure of the master alloy powder is composed of the second phase matrix shell with the composition La and the first phase high melting point core particles with the composition Fe 84.9 Cr 15 C 0.1 .
- the Fe 84.9 Cr 15 C 0.1 particles are nearly spherical in shape, and the particle size ranges from 2.9 ⁇ m to 146 ⁇ m.
- the volume content of Fe 84.9 Cr 15 C 0.1 particles in the master alloy powder is 92%; impurities are enriched in the La matrix shell during solidification.
- the Fe 84.9 Cr 15 C 0.1 particles are separated from the oxides after La pulverization through the natural oxidation-powdering process of La in the air and the magnetic properties of the Fe 84.9 Cr 15 C 0.1 particles to obtain the micron Fe 84.9 Cr 15 C 0.1
- the particle size ranges from 2 ⁇ m to 50 ⁇ m, and the total content of H, O, N, S, P, F, Cl, I and Br in the micron Fe 84.9 Cr 15 C 0.1 powder is less than 1600 ppm.
- the present embodiment provides a preparation method of nano Fe powder, and the preparation method comprises the following steps:
- the alloy whose atomic ratio formula is La 59 Fe 41 is selected, the raw materials are weighed according to the formula, and after the initial alloy raw material is melted uniformly, the alloy melt is atomized and solidified by the water atomization powder technology, and the particle size range is obtained.
- the solidification structure of the master alloy powder is composed of a second phase matrix shell with a composition of La and a large amount of first-phase high-melting-point particles with a composition of Fe and dispersed and embedded on the La matrix.
- the shape of the Fe particles is nearly spherical, and the particle size ranges from 3 nm to 300 nm.
- the volume content of Fe particles in the master alloy powder is 18%; impurities are enriched in the La matrix shell during solidification.
- the Fe particles and the oxides after pulverization of La are separated to obtain nano-Fe particles, whose particle size ranges from 2 ⁇ m to 50 ⁇ m.
- the total content of H, O, N, S, P, F, Cl, I and Br in the powder is less than 1900ppm.
- the present embodiment provides a preparation method of submicron-micron Fe powder, and the preparation method comprises the following steps:
- the alloy whose atomic ratio formula is La 40 Fe 60 is selected, the raw materials are weighed according to the formula, and after the initial alloy raw material is melted uniformly, the alloy melt is atomized and solidified by the water atomization powder technology, and the particle size range is obtained.
- the solidification structure of the master alloy powder is composed of a second phase matrix shell with a composition of La and a large amount of first-phase high-melting-point particles with a composition of Fe and dispersed and embedded on the La matrix.
- the shape of the Fe particles is nearly spherical or dendritic, and the particle size ranges from 100 nm to 10 ⁇ m.
- the volume content of Fe particles in the master alloy powder is 32%; impurities are enriched in the La matrix shell during solidification.
- Fe particles are separated from La pulverized oxides to obtain Fe particles, whose particle size ranges from 100 nm to 10 ⁇ m.
- the total content of H, O, N, S, P, F, Cl, I and Br is less than 1600ppm.
- the obtained Fe powder is further classified to obtain submicron Fe powder with a particle size range of 100 nm-1 ⁇ m, and ultra-fine micron-level Fe powder with a particle size range of 1 ⁇ m to 10 ⁇ m.
- the present embodiment provides a preparation method and application of nano-Ti powder, and the preparation method comprises the following steps:
- the initial alloy melt is atomized and solidified by the water atomization powder technology to obtain nearly spherical master alloy powder with a particle size range of 5 ⁇ m to 80 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage composition is mainly Ce 96.3 T 3.7 and a large amount of first phase dispersed particles whose composition is mainly Ti 99.7 T 0.3 .
- the first phase Ti 99.7 T 0.3 particles are nearly spherical in shape, and their particle size ranges from 5 nm to 150 nm.
- the volume percentage of the first phase Ti 99.7 T 0.3 particles in the master alloy powder is about 19.5%;
- the Ce 96.3 T 3.7 matrix in the master alloy powder is removed by the dilute acid solution, so that the Ti 99.7 T 0.3 particles in the master alloy powder that are difficult to react with the dilute acid solution are detached, that is, the nanometer Ti 99.7 T finer than the master alloy powder is obtained.
- the nanometer powder whose main component is Ti 99.7 T 0.3 is mixed with epoxy resin and other coating components under a protective atmosphere, thereby preparing a nanometer Ti modified polymer anti-corrosion coating.
- This embodiment provides a preparation method of submicron Ti-Nb powder, and the preparation method includes the following steps:
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 150 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage composition is mainly Gd 96.4 T 3.6 and a large amount of first phase dispersed particles whose composition is mainly Ti 49.88 Nb 49.88 T 0.24 .
- the first phase Ti 49.88 Nb 49.88 T 0.24 particles are nearly spherical in shape, and their particle size ranges from 50 nm to 500 nm.
- the volume percentage of the first phase Ti 49.88 Nb 49.88 T 0.24 particles in the master alloy powder is about 26%;
- the Gd 96.4 T 3.6 matrix in the master alloy powder is removed by the dilute acid solution, so that the Ti 49.88 Nb 49.88 T 0.24 particles in the master alloy powder that are difficult to react with the dilute acid solution are detached, that is, the main components are finer than the master alloy powder.
- It is a submicron powder of Ti 49.88 Nb 49.88 T 0.24 with a particle size range of 50nm to 500nm, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.24at. %.
- the present embodiment provides a preparation method of micron Ti powder, and the preparation method comprises the following steps:
- Ti raw materials and rare earth Ce raw materials whose atomic percentage contents of T (including O, H, N, P, S, F, Cl, Br, and I) impurity elements are respectively 1 at.% and 2.5 at.% are selected. According to the molar ratio of Ce to Ti about 5:95, the sponge Ti and the rare earth Ce are fully melted to obtain a uniform initial alloy melt whose atomic percentage is mainly Ce 4.9 Ti 94 T 1.1 .
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second-phase matrix outer shell mainly composed of Ce 86 T 14 in atomic percentage and a single first-phase inner core particle mainly composed of Ti 99.7 T 0.3 .
- the particle size of the inner core particles of the first phase ranges from 14.5 ⁇ m to 97 ⁇ m.
- the volume percentage of the first phase Ti 99.7 T 0.3 particles in the master alloy powder is about 91%;
- the outer shell of Ce 86 T 14 in the master alloy powder is removed by the dilute acid solution, so that the Ti 99.7 T 0.3 core particles in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, the main component of Ti 99.7 T 0.3 is obtained.
- the powder has a particle size range of 14.5 ⁇ m to 97 ⁇ m, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in the powder is 0.3 at.%.
- the present embodiment provides a preparation method of nano-submicron Fe powder, and the preparation method comprises the following steps:
- La raw materials with the atomic percentage content of T including O, H, N, P, S, F, Cl, Br, and I
- impurity elements are respectively 1 at.% and 2.5 at.% are selected.
- the molar ratio of La:Fe of about 3:2 each alloy raw material is melted to obtain a uniform initial alloy melt whose atomic percentage composition is mainly La 58.5 Fe 39.6 T 1.9 .
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 150 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage composition is mainly La 97 T 3 and a large amount of first phase dispersed particles whose composition is mainly Fe 99.75 T 0.25 .
- the shape of the first phase Fe 99.75 T 0.25 particles is nearly spherical or dendritic, and the particle size ranges from 50 nm to 600 nm.
- the volume percentage of the first phase Fe 99.75 T 0.25 particles in the master alloy powder is about 18%;
- the Fe 99.75 T 0.25 particles are separated from the pulverized oxides of La 97 T 3 by the method of magnetic separation, that is, the main component is Fe 99.75
- the nano-submicron powder with T 0.25 has a particle size range of 50 nm to 600 nm, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.25 at.%.
- This embodiment provides a preparation method of micron spherical TiNi powder, and the preparation method includes the following steps:
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of the second phase matrix shell with the main atomic percentage composition of Gd 87.5 T 12.5 and the single first phase core particle with the main composition of Ti 49.9 Ni 49.9 T 0.2 .
- the particle size of the inner core particles of the first phase ranges from 14.5 ⁇ m to 97 ⁇ m.
- the volume percentage of the first phase Ti 49.9 Ni 49.9 T 0.2 particles in the master alloy powder is about 89%;
- the Gd 87.5 T 12.5 matrix shell in the master alloy powder is removed by the dilute acid solution, so that the Ti 49.9 Ni 49.9 T 0.2 core particles in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, the main component is Ti 49.9 Ni 49.9
- the nearly spherical micron powder with T 0.2 has a particle size range of 14.5 ⁇ m to 97 ⁇ m, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.2 at.%%.
- This embodiment provides a preparation method of nano-Ti-V-Al alloy powder, and the preparation method includes the following steps:
- the atomic percentages of T (including O, H, N, P, S, F, Cl) impurity elements are selected as sponge Ti, V block, 3at.%, 1at.%, 2.5at.%, 0.2at. Rare earth Ce, and Al raw materials.
- the initial alloy raw materials are fully melted according to a certain proportion to obtain an initial alloy melt whose atomic percentage composition is mainly Ce 70.5 Al 10 (Ti 96 V 4 ) 17 T 2.5 .
- the initial alloy melt is atomized and solidified by the water atomization pulverizing technology to obtain nearly spherical master alloy powder with a particle size ranging from 5 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose average composition is mainly Ce 86.5 Al 10.5 T 3 and a first phase dispersed particle whose composition is mainly (Ti 96 V 4 ) 92.25 Al 7.5 T 0.25 ; the first phase is dispersed
- the particle size is 10nm-200nm, the shape is nearly spherical, and the volume percentage of the first phase (Ti 96 V 4 ) 92.25 Al 7.5 T 0.25 particles in the master alloy powder is about 12%;
- the Ce 86.5 Al 10.5 T 3 second phase matrix in the master alloy powder is removed by the dilute acid solution, so that the (Ti 96 V 4 ) 92.25 Al 7.5 T 0.25 particles in the master alloy powder that are difficult to react with the dilute acid solution are separated out, that is, The obtained (Ti 96 V 4 ) 92.25 Al 7.5 T 0.25 nano-powder is finer than the master alloy powder, and its particle size is in the range of 50 nm to 200 nm, and it contains O, H, N, P, S, F, Cl, The total content of Br and I was 0.25 at.%.
- the nanometer powder whose main component is (Ti 96 V 4 ) 92.25 Al 7.5 T 0.25 is mixed with epoxy resin and other coating components under a protective atmosphere to prepare a nano-Ti alloy modified polymer anti-corrosion coating.
- This embodiment provides a preparation method of micron Ti-V-Al alloy powder, and the preparation method includes the following steps:
- the atomic percentage content of T (including O, H, N, P, S, F, Cl) impurity elements is 1at.%, 1at.%, 1at.%, 1at.% sponge Ti, V block, rare earth Ce , and Al raw materials.
- the initial alloy raw materials are fully melted according to a certain proportion to obtain an initial alloy melt whose atomic percentage composition is mainly Ce 4.5 Al 0.5 (Ti 96 V 4 ) 94 T 1 .
- the initial alloy melt is atomized and solidified by gas atomization powder milling technology to obtain nearly spherical master alloy powder with particle size ranging from 5 ⁇ m to 80 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose average composition is mainly Ce 82 Al 1.8 T 16.2 and a first phase particle whose composition is mainly (Ti 96 V 4 ) 99.5 Al 0.4 T 0.1 ; The size is about 4.85 ⁇ m ⁇ 78 ⁇ m, and the shape is nearly spherical.
- the structure of the master alloy powder is a core-shell structure, a single first phase particle is coated in the second phase matrix shell, and the volume percentage of (Ti 96 V 4 ) 99.5 Al 0.4 T 0.1 particles in the master alloy powder about 90%;
- the Ce 82 Al 1.8 T 16.2 second phase matrix in the master alloy powder is removed by the dilute acid solution, so that the (Ti 96 V 4 ) 99.5 Al 0.4 T 0.1 particles in the master alloy powder that are difficult to react with the dilute acid solution are detached, that is, The (Ti 96 V 4 ) 99.5 Al 0.4 T 0.1 spherical powder with shape and size close to the master alloy powder was obtained, and the particle size ranged from 4.85 ⁇ m to 78 ⁇ m, and it contained O, H, N, P, S, F, The total content of Cl, Br, and I was 0.1 at.%.
- the obtained spherical (Ti 96 V 4 ) 99.5 Al 0.4 T 0.1 alloy powder can be used in the fields of powder metallurgy, injection molding, or metal 3D printing.
- the present embodiment provides a preparation method of micron Nb powder, and the preparation method comprises the following steps:
- Nb raw materials and Cu raw materials whose atomic percentage contents of T (including O, H, N, P, S, F, Cl, Br, and I) impurity elements are 0.5 at.% and 0.5 at.% respectively.
- T including O, H, N, P, S, F, Cl, Br, and I
- the Nb raw material and the Cu raw material are fully melted to obtain a uniform initial alloy melt whose atomic percentage composition is mainly Cu 11.9 Nb 87.6 T 0.5 .
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix outer shell whose atomic percentage composition is mainly Cu 97.7 T 2.3 and a single first phase inner core particle whose composition is mainly Nb 99.8 T 0.2 .
- the particle size of the inner core particles of the first phase ranges from about 14.5 ⁇ m to 97 ⁇ m, and the shape is nearly spherical.
- the volume percentage of the first phase Nb 99.8 T 0.2 particles in the master alloy powder is about 92%;
- the Cu 97.7 T 2.3 matrix shell in the master alloy powder is removed by the concentrated hydrochloric acid solution, so that the Nb 99.8 T 0.2 core particles in the master alloy powder that are difficult to react with the concentrated hydrochloric acid solution are separated out, that is, the micron with the main component of Nb 99.8 T 0.2 is obtained.
- the powder has a particle size range of about 14.5 ⁇ m to 97 ⁇ m, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.2 at.%.
- the present embodiment provides a preparation method of submicron Si powder, and the preparation method comprises the following steps:
- Si raw materials and Zn raw materials whose atomic percentage contents of T (including O, H, N, P, S, F, Cl, Br, and I) impurity elements are 0.5 at.% and 0.5 at.% respectively are selected. According to the molar ratio of Si to Zn about 30:70, the Si raw material and the Zn raw material are fully melted to obtain a uniform initial alloy melt with the main atomic percentage composition of Si 29.85 Zn 69.65 T 0.5 .
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage is mainly Zn 99.35 T 0.65 and dispersed particles whose atomic percentage is mainly Si 97.83 T 0.17 .
- the particle size range of the dispersed particles is about 100 nm to 2 ⁇ m, and the shape is nearly spherical.
- the volume percentage of the first phase Si 97.83 T 0.17 dispersed particles in the master alloy powder is about 36%;
- the Zn 99.35 T 0.65 matrix in the master alloy powder is removed by the hydrochloric acid solution, so that the Si 97.83 T 0.17 particles in the master alloy powder that are difficult to react with the hydrochloric acid solution are separated out, that is, the submicron powder whose main component is Si 97.83 T 0.17 is obtained.
- the particle size ranges from about 100 nm to 2 ⁇ m, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.17 at.%.
- the present embodiment provides a preparation method of micron Si powder, and the preparation method comprises the following steps:
- Si raw materials and Zn raw materials whose atomic percentage contents of T (including O, H, N, P, S, F, Cl, Br, and I) impurity elements are 0.5 at.% and 0.5 at.% respectively are selected. According to the molar ratio of Si to Zn about 90:10, the Si raw material and the Zn raw material are fully melted to obtain a uniform initial alloy melt with the main atomic percentage composition of Si 89.55 Zn 9.95 T 0.5 .
- the initial alloy melt is atomized and solidified by the gas atomization powder technology to obtain nearly spherical master alloy powder with a particle size ranging from 15 ⁇ m to 100 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage is mainly Zn 96.1 T 3.9 and a first phase particle whose atomic percentage is mainly Si 99.1 T 0.1 .
- the master alloy powder has a core-shell structure, with a single first phase particle inside and a second phase matrix outside and covering the first phase particle.
- the particle size range of the first phase particles is about 14.5 ⁇ m to 97 ⁇ m, the shape is nearly spherical, and the volume percentage of the first phase Si 99.1 T 0.1 particles in the master alloy powder is about 92%;
- the Zn 96.1 T 3.9 matrix shell in the master alloy powder is removed by the hydrochloric acid solution, so that the Si 97.83 T 0.17 particles in the master alloy powder that are difficult to react with the hydrochloric acid solution are separated out, that is, the micron powder whose main component is Si 99.1 T 0.1 is obtained.
- the particle size ranges from about 14.5 ⁇ m to 97 ⁇ m, and the total content of O, H, N, P, S, F, Cl, Br, and I contained in it is 0.1 at.%.
- the present embodiment provides a preparation method of nano CuSi powder, and the preparation method comprises the following steps:
- the initial alloy melt is atomized and solidified by the water atomization powder technology to obtain nearly spherical master alloy powder with a particle size range of 5 ⁇ m to 80 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix mainly composed of Pb 99.4 T 0.6 in atomic percentage and a large amount of first phase dispersed particles mainly composed of (Cu 90 Si 10 ) 99.8 T 0.2 .
- the shape of the first phase (Cu 90 Si 10 ) 99.8 T 0.2 particles is nearly spherical, and the particle size ranges from 5 nm to 150 nm.
- the volume percentage of the first phase (Cu 90 Si 10 ) 99.8 T 0.2 particles in the master alloy powder is about 12%;
- the Pb 99.4 T 0.6 matrix in the master alloy powder is removed by the dilute hydrochloric acid-acetic acid mixed acid solution, so that the (Cu 90 Si 10 ) 99.8 T 0.2 particles in the master alloy powder that are difficult to react with the mixed acid solution are separated out, that is, the main component is obtained.
- the present embodiment provides a preparation method and application of nano-Ti powder, and the preparation method comprises the following steps:
- the raw materials of sponge Ti and rare earth Ce with the atomic percentage content of T (including O, H, N, P, S, F, Cl, Br, and I) impurity elements are respectively 3 at.% and 2.5 at.% are selected.
- Sponge Ti also contains 0.5at.% Mn; rare earth Ce also contains 0.7at.% Mg.
- the sponge Ti and the rare earth Ce are fully melted to obtain a uniform initial alloy melt whose atomic percentage composition is mainly (Ce 99.3 Mg 0.7 ) 64.9 (Ti 99.5 Mn 0.5 ) 32.5 T 2.6 .
- the initial alloy melt is atomized and solidified by the water atomization powder technology to obtain nearly spherical master alloy powder with a particle size range of 5 ⁇ m to 80 ⁇ m.
- the solidification structure of the master alloy powder is composed of a second phase matrix whose atomic percentage composition is mainly (Ce 99.3 Mg 0.7 ) 96.3 T 3.7 and a large amount of first phase dispersed particles whose composition is mainly (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 .
- the first phase (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 particles are nearly spherical in shape, and their particle size ranges from 5 nm to 150 nm.
- the volume percentage of the first phase (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 particles in the master alloy powder is about 19.5%;
- the (Ce 99.3 Mg 0.7 ) 96.3 T 3.7 matrix in the master alloy powder is removed by the dilute acid solution, so that the (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 particles in the master alloy powder that are difficult to react with the dilute acid solution are detached, that is, the ratio of The finer nanometer (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 powder of the master alloy powder has a particle size range of 5 nm to 150 nm, and contains O, H, N, P, S, F, Cl, Br, I of The total content is 0.3 at.%.
- the nanometer powder whose main component is (Ti 99.5 Mn 0.5 ) 99.7 T 0.3 is mixed with epoxy resin and other coating components under a protective atmosphere, thereby preparing nanometer Ti-modified polymer anti-corrosion coating.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Claims (13)
- 一种高纯粉体材料的制备方法,其特征在于,其包括以下步骤:步骤一:选择初始合金原料,按照初始合金成分配比将初始合金原料熔化,得到均匀的初始合金熔体;步骤二:通过雾化制粉技术将初始合金熔体雾化并使之凝固,得到中间合金粉末;所述中间合金粉末由第一相和第二相构成,第一相为颗粒状,第二相为熔点低于第一相的基体相,第一相颗粒被包覆于第二相基体中;所述雾化制粉过程中,初始合金熔体中的杂质元素与雾化凝固过程中引入的杂质元素富集于所述第二相基体中,从而使所述第一相颗粒得到纯化;步骤三:将所述中间合金粉末中的第二相基体去除并保留第一相颗粒,富集于第二相基体中的杂质元素随之被去除,即得到由第一相颗粒组成的高纯目标金属粉体材料。
- 根据权利要求1所述的高纯粉体材料的制备方法,其特征在于,所述初始合金熔体中的杂质元素为T,且T包含O、H、N、P、S、F、Cl、I、Br中的至少一种。
- 根据权利要求2所述的高纯粉体材料的制备方法,其特征在于,根据初始合金原料配比的不同,所述初始合金熔体的平均成分包括如下组合(1)-(4)中的任意一种:组合(1):所述初始合金熔体的平均成分主要为A a(M xD y) bT d,其中,A包含Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种,D包含Fe、Co、Ni中的至少一种,其中,x、y;a、b、d代表对应组成元素的原子百分比含量,且0.5%≤a≤99.5%,0.5%≤b≤99.5%,0≤d≤10%;5%≤x≤55%,45%≤y≤95%;组合(2):所述初始合金熔体的平均成分主要为A aM bT d,其中,A包含Mg、Ca、Li、Na、K、Cu、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种;其中a、b、d代表对应组成元素的原子百分比含量,且0.5%≤a≤99.5%,0.5%≤b≤99.5%,0≤d≤10%;组合(3):所述初始合金熔体的平均成分主要为A aM bT d,其中,A包含Zn、Mg、Sn、Pb、Ga、In、Al、La、Ge、Cu、K、Na、Li中的至少一种,M包含Be、B、Bi、Fe、Ni、Cu、Ag、Si、Ge、Cr、V中的至少一种,且M中Be、B、Si、Ge的原子百分比总含量在M中的占比小于50%,其中a、b、d代表对应组成元素的原子百分比含量,且0.5%≤a≤99.5%,0.5%≤b≤99.5%,0≤d≤10%;组合(4):当所述初始合金熔体的平均成分主要为A aM bAl cT d时,A包含Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种;M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种;Al为铝;其中a、b、c、d分别代表对应组成元素的原子百分比含量,且0.5≤a≤99.4%,0.5≤b≤99.4%,0.1%≤c≤25%,0≤d≤10%;
- 根据权利要求3所述的高纯粉体材料的制备方法,其特征在于:当初始合金熔体的平均成分为步骤一组合(1)所述时,所述中间合金粉末包含成分主要为(M xD y) x1T z1的第一相颗粒与成分主要为A x2T z2的第二相基体;其中,98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量;当初始合金熔体的平均成分为步骤一组合(2)或组合(3)所述时,所述中间合金粉末包含成分主要为M x1T z1的第一相颗粒与成分主要为A x2T z2的第二相基体;其中,98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量;当初始合金熔体的平均成分为步骤一组合(4)所述时,所述中间合金粉末包含成分主要为M x1Al y1T z1的第一相颗粒与平均成分主要为A x2Al y2T z2的第二相基体;且78%≤x1≤99.9%,0.1%≤y1≤22%,0≤z1≤2%;70%≤x2≤99.8%,0.2%≤y2≤30%,0≤z2≤30%,z1≤d≤z2,2z1≤z2,x1、y1、z1、x2、y2、z2分别代表对应组成元素的原子百分比含量;
- 根据权利要求1所述的高纯粉体材料的制备方法,其特征在于,所述雾化制粉技术包括气雾化、水雾化、水汽-联合雾化、真空雾化、等离子体雾化、离心雾化、旋转盘雾化、以及旋转电极雾化中的至少一种。
- 根据权利要求1所述的高纯粉体材料的制备方法,其特征在于,所述第一相颗粒被包覆于第二相基体中的方式包括:多个第一相颗粒弥散分布于第二相基体中的镶嵌结构,或者单个第一相颗粒在内、第二相基体在外的核壳结构。
- 根据权利要求1所述的高纯粉体材料的制备方法,其特征在于,所述将中间合金粉末中的第二相基体去除方法包括:酸反应去除、碱反应去除、真空挥发去除,以及第二相基体自然氧化-粉化剥落去除中的至少一种。
- 根据权利要求1所述的高纯粉体材料的制备方法,其特征在于,所述高纯目标粉体材料的颗粒粒径范围为3nm~7.9mm。
- 根据权利要求1-8任一项所述的高纯粉体材料在催化材料、粉末冶金、复合材料、吸波材料、杀菌材料、金属注射成型、3D打印增材制造、涂料中的应用。
- 一种双相粉体材料,其特征在于,所述双相粉体材料为粉体状,其单一颗粒进一步包含内生粉与包覆体;所述双相粉体材料的凝固组织包括基体相和颗粒相,基体相即为所述包覆体,颗粒相即为双相粉体材料中的内生粉;所述包覆体的熔点低于所述内生粉的熔点,所述内生粉被包覆于所述包覆体中;所述双相粉体材料中内生粉被包覆于包覆体中的方式包括:多个内生粉弥散分布于包覆体中的镶嵌结构,或者单个内生粉在内、包覆体在外的核壳结构;所述双相粉体材料的化学组成与结构包含以下四种组合中的任意一种:1)所述双相粉体材料中内生粉的成分主要为(M xD y) x1T z1,包覆体的平均成分主要为A x2T z2;且98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量;其中,A包含Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种,D包含Fe、Co、Ni中的至少一种;T包含O、H、N、P、S、F、Cl、I、Br中的至少一种;x、y代表对应组成元素的原子百分比含量,5%≤x≤55%,45%≤y≤95%;2)所述双相粉体材料中内生粉的成分主要为M x1T z1,包覆体的平均成分主要为A x2T z2;且98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量;其中,A包含Mg、Ca、Li、Na、K、Cu、Y、La、 Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种;T包含O、H、N、P、S、F、Cl、I、Br中的至少一种;3)所述双相粉体材料中内生粉的成分主要为M x1T z1,包覆体的平均成分主要为A x2T z2;且98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量;其中,A包含Zn、Mg、Sn、Pb、Ga、In、Al、La、Ge、Cu、K、Na、Li中的至少一种,M包含Be、B、Bi、Fe、Ni、Cu、Ag、Si、Ge、Cr、V中的至少一种,且M中Be、B、Si、Ge的原子百分比总含量在M中的占比小于50%;T包含O、H、N、P、S、F、Cl、I、Br中的至少一种;4)所述双相粉体材料中内生粉的成分主要为M x1Al y1T z1,包覆体的平均成分主要为A x2Al y2T z2;且78%≤x1≤99.9%,0.1%≤y1≤22%,0≤z1≤2%;70%≤x2≤99.8%,0.2%≤y2≤30%,0≤z2≤30%,z1≤d≤z2,2z1≤z2,x1、y1、z1、x2、y2、z2分别代表对应组成元素的原子百分比含量;其中,A包含Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种;M包含W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti中的至少一种;Al为铝;T包含O、H、N、P、S、F、Cl、I、Br中的至少一种。
- 一种高纯粉体材料的制备方法,其特征在于,其包括以下步骤:步骤一:选择初始合金原料,按照初始合金成分配比将初始合金原料熔化,得到均匀的初始合金熔体;步骤二:通过雾化制粉技术将初始合金熔体雾化并使之凝固,得到中间合金粉末;所述中间合金粉末由第一相和第二相构成,第一相为颗粒状,第二相为熔点低于第一相的基体相,第一相颗粒被包覆于第二相基体中;所述雾化制粉过程中,初始合金熔体中的杂质元素与雾化凝固过程中引入的杂质元素富集于所述第二相基体中,从而使所述第一相颗粒得到纯化;步骤三:将所述中间合金粉末中的第二相基体去除并保留第一相颗粒,富集于第二相基体中的杂质元素随之被去除,即得到由第一相颗粒组成的高纯目标粉体材料;其中,所述初始合金熔体中的杂质元素为T,且T包含O、H、N、P、S、F、Cl、I、Br中的至少一种;所述初始合金熔体的平均成分主要为A aM bT d,A包含Zn、Sn、Pb、Ga、In、Al、Ge、Cu中的至少一种;M包含Be、Si、Ge、B中的至少一种,且Be、Si、Ge、B的原子百分比含量在M中的占比大于等于50%,其中a、b、d代表对应组成元素的原子百分比含量,且0.5%≤a≤99.5%,0.5%≤b≤99.5%,0≤d≤10%;所述中间合金粉末包含成分主要为M x1T z1的第一相颗粒与成分主要为A x2T z2的第二相基体;其中,98%≤x1≤100%,0≤z1≤2%;70%≤x2≤100%,0≤z2≤30%;z1≤d≤z2,2z1≤z2;x1、z1、x2、z2分别代表对应组成元素的原子百分比含量。
- 一种高纯金属粉体材料的制备方法,其特征在于:步骤1:选择初始合金原料,按照初始合金成分配比将初始合金原料熔化,得到均匀的初始合金熔体;步骤2:通过雾化制粉技术将初始合金熔体雾化并使之凝固,得到中间合金粉末;所述中间合金粉末由第一相和第二相构成,第一相为颗粒状,第二相为熔点低于第一相的基体相,第一相颗粒被包覆于第二相基体中;所述雾化制粉过程中,初始合金熔体中的杂质元素与雾化凝固过程中引入的杂质元素富集于所述第二相基体中,从而使所述第一相颗粒得到纯化;步骤3:将所述中间合金粉末中的第二相基体去除并保留第一相颗粒,富集于第二相基体中的杂质元素随之被去除,即得到由第一相颗粒组成的高纯目标金属粉体材料。
- 根据权利要求12所述的高纯金属粉体材料的制备方法,其特征在于,当所述初始合金的成分配比为A aM b时,A选自Mg、Ca、Li、Na、K、Zn、In、Sn、Pb、Ga、Cu、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,M选自W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti、Fe、Co、Ni、Mn、Cu、Ag、Si、Ge、B、Be、C中的至少一种;其中a、b代表对应组成元素的原子百分含量,0.5%≤b≤98%,a+b=100%;且所述A aM b合金熔体雾化凝固时不形成由A与M构成的金属间化合物,而是形成成分为M的第一相颗粒与成分为A的第二相基体。当所述初始合金的成分配比为A aM bAl c时,A选自Mg、Ca、Li、Na、K、Zn、In、Sn、Pb、Ga、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的至少一种,Al为铝,M选自W、Cr、Mo、V、Ta、Nb、Zr、Hf、Ti、Fe、Co、Ni、Mn、Cu、Ag、Si、Ge、B、Be、C中的至少一种;其中a、b、c分别代表对应组成元素的原子百分比含量,0.5%≤b≤98%,0.1%≤c≤30%,a+b+c=100%;且所述A aM bAl c合金熔体雾化凝固时不形成由A与M构成的金属间化合物,而是形成成分为M x1Al y1的第一相颗粒与成分为A x2Al y2的第二相基体,其中x1、y1、x2、y2分别代表对应组成元素的原子百分比含量,且0.1%≤y1≤25%,0.1%≤y2≤35%,x1+y1=100%,x2+y2=100%。
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020237009455A KR20230051702A (ko) | 2020-08-19 | 2020-12-08 | 고순도 분말체 재료의 제조방법, 응용 및 2상 분말체 재료 |
CA3190201A CA3190201A1 (en) | 2020-08-19 | 2020-12-08 | Method for preparing high-purity powder material, application thereof, and double-phase powder material |
CN202080066665.6A CN114555264B (zh) | 2020-08-19 | 2020-12-08 | 高纯粉体材料的制备方法及其应用及一种双相粉体材料 |
US18/022,246 US20240033822A1 (en) | 2020-08-19 | 2020-12-08 | Method for preparing high-purity powder material, application thereof, and double-phase powder material |
AU2020464490A AU2020464490A1 (en) | 2020-08-19 | 2020-12-08 | Preparation method for and use of high-purity powder material and biphasic powder material |
JP2023511880A JP2023539090A (ja) | 2020-08-19 | 2020-12-08 | 高純度粉体材料の作製方法と応用及びある種類二相粉体材料 |
EP20950141.0A EP4201553A4 (en) | 2020-08-19 | 2020-12-08 | PREPARATION METHOD AND USE OF HIGH PURITY POWDERED MATERIAL AND BIPHASIC POWDERED MATERIAL |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010838571 | 2020-08-19 | ||
CN202010838571.8 | 2020-08-19 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2022036938A1 true WO2022036938A1 (zh) | 2022-02-24 |
Family
ID=74775585
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CN2020/134655 WO2022036938A1 (zh) | 2020-08-19 | 2020-12-08 | 高纯粉体材料的制备方法及其应用及一种双相粉体材料 |
Country Status (8)
Country | Link |
---|---|
US (1) | US20240033822A1 (zh) |
EP (1) | EP4201553A4 (zh) |
JP (1) | JP2023539090A (zh) |
KR (1) | KR20230051702A (zh) |
CN (2) | CN112404445A (zh) |
AU (1) | AU2020464490A1 (zh) |
CA (1) | CA3190201A1 (zh) |
WO (1) | WO2022036938A1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115319114A (zh) * | 2022-08-18 | 2022-11-11 | 福州大学 | 一种使用选区激光熔化工艺制备SnBi-xFe低熔点复合材料的方法 |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022100656A1 (zh) * | 2019-11-28 | 2022-05-19 | 赵远云 | 一种含铝合金粉体的制备方法及其应用及一种合金条带 |
AU2020464490A1 (en) * | 2020-08-19 | 2023-05-04 | Yuanyun ZHAO | Preparation method for and use of high-purity powder material and biphasic powder material |
AU2021354564A1 (en) * | 2020-09-30 | 2023-06-08 | Yuanyun ZHAO | Alloy powder, preparation method therefor, and use thereof |
CN112919908B (zh) * | 2021-03-04 | 2023-03-21 | 内蒙古工业大学 | 一种新型钙钛矿结构高熵陶瓷及其制备方法 |
CN114290012A (zh) * | 2021-12-31 | 2022-04-08 | 南通华严磨片有限公司 | 一种具有铣削和磨削功能的多孔圆刀的制备方法 |
WO2023142563A1 (zh) * | 2022-01-25 | 2023-08-03 | 赵远云 | 一种球形铁合金粉体材料及其制备方法与用途 |
CN116251963A (zh) * | 2023-01-13 | 2023-06-13 | 吉林大学 | 一种具有室温磁相变性能的镍锰锡钴合金及其高效增材制造方法和应用 |
CN116727656B (zh) * | 2023-06-07 | 2024-01-02 | 连云港倍特超微粉有限公司 | 一种熔融烧结复合合金微粉及其制备方法和应用 |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06299208A (ja) * | 1993-04-14 | 1994-10-25 | Daido Steel Co Ltd | タンディッシュからの溶湯滴下方法及びそのための装置 |
CN102161099A (zh) * | 2011-03-22 | 2011-08-24 | 唐山威豪镁粉有限公司 | 纳米晶高纯球形镁合金粉末生产方法及装置 |
CN103317141A (zh) * | 2013-06-17 | 2013-09-25 | 中国科学院宁波材料技术与工程研究所 | 一种金属纳米颗粒的制备方法 |
CN106811750A (zh) * | 2015-11-30 | 2017-06-09 | 中国科学院宁波材料技术与工程研究所 | 一种纳米多孔金属颗粒及其制备方法 |
CN106916988A (zh) * | 2015-12-28 | 2017-07-04 | 中国科学院宁波材料技术与工程研究所 | 一种纳米多孔金属薄膜的制备方法 |
CN107406251A (zh) * | 2015-03-18 | 2017-11-28 | 斐源有限公司 | 金属氧化物粒子以及其制造方法 |
CN111334682A (zh) * | 2020-03-12 | 2020-06-26 | 东莞理工学院 | 一种纳米多孔金属粉末及其制备方法 |
CN111590084A (zh) * | 2019-02-21 | 2020-08-28 | 刘丽 | 一种金属粉体材料的制备方法 |
CN111945000A (zh) * | 2019-05-15 | 2020-11-17 | 刘丽 | 一种金属提纯方法 |
CN111940750A (zh) * | 2019-05-15 | 2020-11-17 | 刘丽 | 一种合金粉体材料的制备方法 |
CN112404445A (zh) * | 2020-08-19 | 2021-02-26 | 赵远云 | 高纯粉体材料的制备方法及其应用及一种双相粉体材料 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101195160A (zh) * | 2006-12-07 | 2008-06-11 | 比亚迪股份有限公司 | 一种非晶合金粉末及其制备方法 |
DE102010029078A1 (de) * | 2010-05-18 | 2011-11-24 | Matthias Fockele | Verfahren zur Herstellung eines Gegenstandes durch schichtweises Aufbauen aus pulverförmigem Werkstoff |
CN105149603B (zh) * | 2015-08-26 | 2017-12-01 | 上海材料研究所 | 高球形度Inconel625合金粉末及其制备方法与应用 |
-
2020
- 2020-12-08 AU AU2020464490A patent/AU2020464490A1/en active Pending
- 2020-12-08 CN CN202011445898.5A patent/CN112404445A/zh not_active Withdrawn
- 2020-12-08 KR KR1020237009455A patent/KR20230051702A/ko unknown
- 2020-12-08 US US18/022,246 patent/US20240033822A1/en active Pending
- 2020-12-08 JP JP2023511880A patent/JP2023539090A/ja active Pending
- 2020-12-08 EP EP20950141.0A patent/EP4201553A4/en active Pending
- 2020-12-08 WO PCT/CN2020/134655 patent/WO2022036938A1/zh active Application Filing
- 2020-12-08 CN CN202080066665.6A patent/CN114555264B/zh active Active
- 2020-12-08 CA CA3190201A patent/CA3190201A1/en active Pending
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06299208A (ja) * | 1993-04-14 | 1994-10-25 | Daido Steel Co Ltd | タンディッシュからの溶湯滴下方法及びそのための装置 |
CN102161099A (zh) * | 2011-03-22 | 2011-08-24 | 唐山威豪镁粉有限公司 | 纳米晶高纯球形镁合金粉末生产方法及装置 |
CN103317141A (zh) * | 2013-06-17 | 2013-09-25 | 中国科学院宁波材料技术与工程研究所 | 一种金属纳米颗粒的制备方法 |
CN107406251A (zh) * | 2015-03-18 | 2017-11-28 | 斐源有限公司 | 金属氧化物粒子以及其制造方法 |
CN106811750A (zh) * | 2015-11-30 | 2017-06-09 | 中国科学院宁波材料技术与工程研究所 | 一种纳米多孔金属颗粒及其制备方法 |
CN106916988A (zh) * | 2015-12-28 | 2017-07-04 | 中国科学院宁波材料技术与工程研究所 | 一种纳米多孔金属薄膜的制备方法 |
CN111590084A (zh) * | 2019-02-21 | 2020-08-28 | 刘丽 | 一种金属粉体材料的制备方法 |
CN111945000A (zh) * | 2019-05-15 | 2020-11-17 | 刘丽 | 一种金属提纯方法 |
CN111940750A (zh) * | 2019-05-15 | 2020-11-17 | 刘丽 | 一种合金粉体材料的制备方法 |
CN111334682A (zh) * | 2020-03-12 | 2020-06-26 | 东莞理工学院 | 一种纳米多孔金属粉末及其制备方法 |
CN112404445A (zh) * | 2020-08-19 | 2021-02-26 | 赵远云 | 高纯粉体材料的制备方法及其应用及一种双相粉体材料 |
Non-Patent Citations (1)
Title |
---|
See also references of EP4201553A4 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115319114A (zh) * | 2022-08-18 | 2022-11-11 | 福州大学 | 一种使用选区激光熔化工艺制备SnBi-xFe低熔点复合材料的方法 |
CN115319114B (zh) * | 2022-08-18 | 2023-12-19 | 福州大学 | 一种使用选区激光熔化工艺制备SnBi-xFe低熔点复合材料的方法 |
Also Published As
Publication number | Publication date |
---|---|
CN114555264A (zh) | 2022-05-27 |
AU2020464490A1 (en) | 2023-05-04 |
EP4201553A4 (en) | 2024-02-14 |
JP2023539090A (ja) | 2023-09-13 |
KR20230051702A (ko) | 2023-04-18 |
CN112404445A (zh) | 2021-02-26 |
EP4201553A1 (en) | 2023-06-28 |
US20240033822A1 (en) | 2024-02-01 |
CN114555264B (zh) | 2023-04-28 |
CA3190201A1 (en) | 2022-02-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2022036938A1 (zh) | 高纯粉体材料的制备方法及其应用及一种双相粉体材料 | |
CN112207285B (zh) | 粉体材料的制备方法及其应用 | |
KR102539775B1 (ko) | 알루미늄 합금 함유 분말체의 제조 방법 및 이의 응용과 합금 스트립 | |
WO2022068710A1 (zh) | 一类合金粉及其制备方法与用途 | |
WO2022036906A1 (zh) | 一种高纯粉体材料的制备方法及其应用及一种合金条带 | |
CN111940750B (zh) | 一种合金粉体材料的制备方法 | |
CN116056819A (zh) | 一种包含贵金属元素的粉体材料的制备方法及其应用 | |
JP4264873B2 (ja) | ガスアトマイズ法による微細金属粉末の製造方法 | |
WO2022100656A1 (zh) | 一种含铝合金粉体的制备方法及其应用及一种合金条带 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 20950141 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 2023511880 Country of ref document: JP Kind code of ref document: A |
|
ENP | Entry into the national phase |
Ref document number: 3190201 Country of ref document: CA |
|
WWE | Wipo information: entry into national phase |
Ref document number: 18022246 Country of ref document: US |
|
WWE | Wipo information: entry into national phase |
Ref document number: AU2020464490 Country of ref document: AU |
|
ENP | Entry into the national phase |
Ref document number: 20237009455 Country of ref document: KR Kind code of ref document: A |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 2020950141 Country of ref document: EP Effective date: 20230320 |
|
ENP | Entry into the national phase |
Ref document number: 2020464490 Country of ref document: AU Date of ref document: 20201208 Kind code of ref document: A |