CN113897528A - A kind of preparation method of uniformly dispersed Fe-Ni/Al2O3 magnetic composite material - Google Patents
A kind of preparation method of uniformly dispersed Fe-Ni/Al2O3 magnetic composite material Download PDFInfo
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- CN113897528A CN113897528A CN202111087984.8A CN202111087984A CN113897528A CN 113897528 A CN113897528 A CN 113897528A CN 202111087984 A CN202111087984 A CN 202111087984A CN 113897528 A CN113897528 A CN 113897528A
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- Prior art keywords
- nickel
- iron
- composite material
- alumina
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims description 24
- 229910052593 corundum Inorganic materials 0.000 title 1
- 229910001845 yogo sapphire Inorganic materials 0.000 title 1
- 239000000843 powder Substances 0.000 claims abstract description 50
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims abstract description 42
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 16
- 239000000446 fuel Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000004471 Glycine Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 3
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 claims description 2
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 2
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- -1 nonahydrate ferric nitrate Chemical class 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims 1
- 238000002490 spark plasma sintering Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 15
- 239000000956 alloy Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 5
- 229910001374 Invar Inorganic materials 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910000889 permalloy Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229940032296 ferric chloride Drugs 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- VXWSFRMTBJZULV-UHFFFAOYSA-H iron(3+) sulfate hydrate Chemical compound O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VXWSFRMTBJZULV-UHFFFAOYSA-H 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
- C22C33/00—Making ferrous alloys
- C22C33/006—Making ferrous alloys compositions used for making ferrous alloys
-
- 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
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Electromagnetism (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
A production method of iron-nickel magnetic nano composite material doped with alumina particles belongs to the technical field of composite material preparation. The process comprises the following steps: (1) preparing an iron source, a nickel source, a fuel and an aluminum source into a solution according to a proportion; (2) heating and stirring, volatilizing the solution, concentrating and decomposing to obtain precursor powder; (3) and reacting the precursor powder for 1-3 hours at the temperature of 300-600 ℃ in a protective atmosphere to obtain the alloy powder. (4) Pressing and molding the alloy powder, and calcining and densifying at 800-1300 ℃; and (3) directly sintering the powder by using discharge plasma at 600-750 ℃ or carrying out hot isostatic pressing at the sintering temperature of 700-900 ℃ to obtain the iron-nickel/alumina composite material. The method has the advantages of cheap and easily-obtained raw materials, simple and quick manufacturing process, low process energy consumption and low cost, and the obtained iron-nickel/alumina composite material has fine and dispersed oxide particles and uniform distribution, can effectively improve the mechanical property of the iron-nickel magnetic composite material and has good magnetic property.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a production method of an iron-nickel magnetic composite material doped with alumina particles.
Background
The iron-nickel alloy has many excellent properties, for example, the iron-nickel alloy with the nickel content of 30% -90% has good soft magnetic characteristics in a weak magnetic field and a medium magnetic field, has high magnetic permeability and low coercive force, is called permalloy, and the permalloy containing 78% of nickel has the highest initial magnetic permeability which is tens of times that of the traditional silicon steel material. The iron core material, the magnetic shielding material, the rectangular magnetic alloy and the thermomagnetic alloy permalloy are widely applied. When the mass fraction of nickel is 36%, the invar effect is produced, the expansion rate of the alloy is almost zero at room temperature, and the alloy shows good dimensional stability, so that the prepared iron-nickel soft magnetic material has the characteristics of low cost, high compressibility, high saturation magnetization and the like, can be used for manufacturing precise instruments, standard measuring tools, resonant cavities, wave guide tubes, variable capacitance blades, hard disk drives, shadow masks of kinescopes, thermosensitive transverse splicing bimetallic strips, laser elements and the like, and is widely applied to the fields of electronic industry, aerospace, precise instruments and the like.
For functional materials, only a single characteristic of the functional material in a certain aspect is concerned in the past, the requirement of scientific and technological development on the material cannot be met, the functional material is required to have certain mechanical bearing capacity in certain scenes, and for example, a nickel core ferromagnetic ring commonly used in the communication industry needs to have certain mechanical properties to maintain the shape and size of the nickel core ferromagnetic ring and support surrounding parts besides the functions of magnetic storage, signal transmission and the like. And if the addition of other elements is strictly controlled by the invar alloy, the internal structure of the alloy is a single austenite structure, so that the strength of the invar alloy is generally low, about 500MPa, the invar alloy is used as a material of some non-bearing parts for a long time, and the development of the structure-function integrated application potential of the invar alloy is limited by the low strength.
Although the traditional methods for reinforcing materials, such as solid solution strengthening, work hardening and the like, can improve the strength of the materials to a certain extent, the traditional methods are all based on cold and hot working processes with complex processes, the iron-nickel alloy is extremely sensitive to various macroscopic and microscopic stresses generated in the working process, and the traditional mechanical processing method is used for generating irreversible damage to the magnetic properties of the iron-nickel alloy, so that the magnetic induction strength and the magnetic permeability of the iron-nickel alloy are reduced, and the balance among the options of functions/structures is difficult.
Therefore, the invention tries to introduce the alumina particles into the iron-nickel alloy in a liquid phase mixing mode, and aims to improve the mechanical property of the iron-nickel alloy and widen the application of the iron-nickel alloy in the aspects of stressed structural members with certain requirements on material functions and the like by introducing the second phase which is dispersed and distributed. Alumina is a high temperature structural ceramic with high hardness, high wear resistance, high chemical stability, low cost, and wide application in industry. The aluminum oxide particles are distributed in the iron-nickel alloy, so that on one hand, the movement of dislocation in the alloy can be hindered, dislocation winding, plugging and the like are generated at the particles, the strength of the alloy is improved, and the aluminum oxide particles with fine and uniformly distributed particles can also play a role in dispersion strengthening; on the other hand, the alumina particles among the crystal grains can block the transmission of dislocation among different crystal grains, the mutual fusion and growth of alloy crystal grains are limited, the alloy crystal grains are enabled to be finer and more dispersed, and particularly the stable physical and chemical properties of the alumina at high temperature also enable the alloy to keep good dimensional stability at high temperature. The yield strength, tensile strength and plastic toughness of the iron-nickel alloy are improved while the unique magnetic properties of the iron-nickel alloy are maintained.
The method for preparing the iron-nickel magnetic composite material mainly comprises the following steps: mechanical alloying method, spray pyrolysis method, chemical method, etc. In publication No. CN108568529A, leichenolong et al mixes iron, nickel metal salt and precipitant in a solution at a certain ratio, precipitates, filters, dries, mechanically mixes with sodium chloride and alumina, and anneals and cools at a certain temperature and time to obtain iron-nickel alloy powder. In publication No. CN108726581B, Naciocong et al use spray pyrolysis method to make iron-nickel alloy melt obtained by electric furnace reduction smelting of nickel iron ore, refining desulfurization, blowing and impurity removal in converter, and then make it undergo the processes of ball-milling, screening and fluid-state oxidation roasting so as to obtain iron-nickel oxide. In publication No. CN110813296A, Hexuan et al uniformly mixed the precursors of zinc, nickel and iron and alkali in solution at a certain ratio, carried out hydrothermal reaction in a hydrothermal kettle, filtered, washed, dried, and reduced in a tube furnace to obtain the nano-porous iron-nickel alloy powder. The method is simple and feasible, but is not easy to realize industrial mass production.
Disclosure of Invention
The invention provides a method for producing an iron-nickel magnetic composite material doped with alumina particles, aiming at breaking through the damage of the traditional machining process to the magnetic performance of iron-nickel alloy.
The method for producing the magnetic composite material is characterized by comprising the following steps of:
a. dissolving an iron source, a nickel source, a fuel and an aluminum source in deionized water according to a certain proportion, wherein the mass fraction of nickel in the iron-nickel alloy of the target product is 30-90%, the proportion of the fuel to the total amount of the iron source and the nickel source is (1-4): 1, the aluminum source is doped into the composite material in the form of ions existing in the solution, and the addition amount is calculated by calculating the mass ratio of the alumina to the whole composite material and is about 1-5%;
b. b, stirring the mixed solution formed in the step a to fully and uniformly mix the mixed solution, standing for a period of time without precipitation, and heating the solution to volatilize, concentrate and decompose the solution to obtain precursor powder;
c. b, reacting the precursor powder obtained in the step b for 1-3 hours at the temperature of 400-600 ℃ in a certain protective atmosphere to obtain iron-nickel/alumina composite powder;
d. c, pressing and forming the iron-nickel/alumina powder obtained in the step c to obtain an iron-nickel/alumina green body;
e. and d, calcining the green body obtained in the step d at the temperature of 800-1300 ℃ under a certain condition to obtain the iron-nickel/alumina composite material.
f. The iron-nickel/aluminum oxide composite powder obtained in the step c can be directly sintered by spark plasma to directly obtain a composite material, wherein the sintering temperature is 600-750 ℃, the sintering pressure is 30-50 MPa, and the sintering time is 3-5 minutes; or hot isostatic pressing for direct forming, wherein the sintering pressure is 100-150MPa, the sintering temperature is 700-900 ℃, and the sintering time is 0.5-1.5 hours, so as to obtain the iron-nickel/alumina composite material.
Further, the iron source added in the step a is soluble iron salt such as ferric nitrate nonahydrate, ferric sulfate hydrate, ferric chloride hexahydrate and the like; wherein the nickel source is soluble nickel salts such as nickel nitrate hexahydrate, nickel acetate tetrahydrate, nickel dichloride hexahydrate and the like; when the iron source is ferric nitrate nonahydrate, the fuel is oxidant such as glycine, urea, glucose, citric acid and the like, and the molar ratio of the fuel to the total amount of the iron source and the nickel source is (1-4): 1; wherein the aluminum source is soluble aluminum salt such as aluminum nitrate nonahydrate, hydrated aluminum sulfate and the like.
Further, the predetermined atmosphere in step c is a reducing atmosphere such as hydrogen or carbon monoxide. The optimal reaction temperature is 400-500 ℃; the optimal reaction time is 1.5 to 2.5 hours.
Further, the pressing molding in the step d is die pressing and cold isostatic pressing, and the pressure range is 150-300 MPa.
Further, the sintering conditions in step e are protective atmosphere such as vacuum, hydrogen, nitrogen, argon, etc. The sintering time is 1-3 hours.
Based on the dispersion strengthening principle, by a solution combustion synthesis method, alumina particles are introduced into the iron-nickel alloy as a second phase in a liquid-liquid mixing mode and are uniformly mixed with the matrix at an atomic level to prepare precursor powder with alumina uniformly dispersed and distributed on the iron-nickel oxide matrix, and the obtained powder is loose, porous and good in dispersibility. And reducing the precursor powder, removing oxygen in iron and nickel, and obtaining the aluminum oxide/iron-nickel composite powder.
The key points of the technology of the invention are as follows:
1. alumina particles are introduced into the iron-nickel alloy to obtain alumina/iron-nickel composite powder. The porous structure of the powder provides large specific surface area and high sintering activity, and the densification of the material is carried out under certain protective gas by a powder metallurgy atmosphere sintering method to obtain the aluminum oxide dispersion strengthened iron-nickel alloy. On the premise of maintaining the excellent magnetic property of the iron-nickel alloy, the mechanical property is greatly improved. The application of the iron-nickel-based composite material in the aspects of strengthening iron-nickel alloy, iron-nickel soft magnetic materials and the like by using particle oxides is greatly improved. The method has the characteristics of low cost, high efficiency and excellent product performance.
2. The method comprises the steps of preparing precursor powder by controlling the proportion of an iron source, a nickel source, a fuel and an aluminum source through a solution combustion synthesis method, reacting for 1-3 hours at the temperature of 400-600 ℃ in a protective atmosphere to obtain iron-nickel/alumina composite powder, pressing and calcining to obtain the alumina/iron-nickel composite powder.
The method has the following advantages: (1) the reaction is carried out in a liquid phase, so that the uniform mixing of the atomic levels of all components can be realized, and the particles can be uniformly dispersed and distributed in a matrix; (2) the heat released by the reaction can make the reaction self-maintained, and the energy consumption is low; (3) gas generated in the reaction process can play a role in dispersing products, and can effectively prevent agglomeration of powder particles; (4) the prepared precursor has high reaction activity, and can reduce the subsequent reaction temperature and improve the reaction speed. (5) The prepared powder has fine particles, large specific surface area and high sintering activity, and can effectively reduce the densification temperature; (6) the raw materials are cheap and easy to obtain, the manufacturing process is simple, convenient and quick, the process energy consumption is low, the cost is low, and the large-scale production can be realized;
Detailed Description
The present invention is further illustrated below with reference to examples, which are intended to illustrate the invention and not to limit the scope of the invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings herein, and such equivalents may fall within the scope of the invention as defined in the appended claims.
Example 1:
weighing 0.1mol of ferric nitrate, 0.095mol of nickel nitrate, 0.2 mol of glycine and 0.01 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 2 hours at the temperature of 400 ℃ in a hydrogen atmosphere to obtain the iron-nickel/alumina composite powder. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 300 MPa. And (3) putting the green body into a tubular furnace, introducing hydrogen, and sintering at 800 ℃ for 3h to obtain the iron-nickel/alumina composite material.
Example 2:
weighing 0.07 mol of ferric chloride, 0.1mol of nickel chloride, 0.35 mol of glycine and 0.03 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 1.5 hours at the temperature of 500 ℃ in the atmosphere of carbon monoxide to obtain the iron-nickel/alumina composite powder. And (3) carrying out cold isostatic pressing on the composite powder at the pressure of 200MPa to obtain a green body. And (3) putting the green body into a hot-pressing sintering furnace, sintering for 2h at 900 ℃ in a vacuum atmosphere, and densifying to obtain the iron-nickel/aluminum oxide composite material.
Example 3:
weighing 0.1mol of ferric chloride, 0.095mol of nickel sulfate, 0.4 mol of glucose and 0.015 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 1 hour at 500 ℃ in a hydrogen atmosphere to obtain the iron-nickel/alumina composite powder. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 300 MPa. And (3) putting the green body into a tube furnace, introducing argon, and sintering at 1100 ℃ for 1.5h to obtain the iron-nickel/alumina composite material.
Example 4:
weighing 0.07 mol of ferric sulfate, 0.1mol of nickel nitrate, 0.25 mol of urea and 0.025 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 1 hour at the temperature of 600 ℃ in the atmosphere of carbon monoxide to obtain the iron-nickel/alumina composite powder. And (3) sheathing the composite powder, sintering the composite powder by hot isostatic pressing, sintering the composite powder at the sintering pressure of 150MPa for 1.5h at 800 ℃ for densification to obtain the iron-nickel/alumina composite material.
Example 5:
weighing 0.1mol of ferric nitrate, 0.095mol of nickel acetate, 0.35 mol of glycine and 0.03 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 2.5 hours at 350 ℃ in hydrogen atmosphere to obtain the iron-nickel/alumina composite powder. And (3) filling the composite powder into a mold, performing discharge plasma sintering, and sintering at 700 ℃ for 3 minutes under the sintering pressure of 50MPa to obtain the iron-nickel/alumina composite material.
Claims (5)
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