JPH06163231A - Magnetic powder for bonded magnet and manufacture thereof - Google Patents
Magnetic powder for bonded magnet and manufacture thereofInfo
- Publication number
- JPH06163231A JPH06163231A JP4341284A JP34128492A JPH06163231A JP H06163231 A JPH06163231 A JP H06163231A JP 4341284 A JP4341284 A JP 4341284A JP 34128492 A JP34128492 A JP 34128492A JP H06163231 A JPH06163231 A JP H06163231A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- type
- magnetic powder
- fine particles
- particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 64
- 239000010419 fine particle Substances 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
- 239000002184 metal Substances 0.000 claims abstract description 32
- 150000003839 salts Chemical class 0.000 claims abstract description 28
- 230000001603 reducing effect Effects 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 239000008139 complexing agent Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052755 nonmetal Chemical class 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 230000005415 magnetization Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910015371 AuCu Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000011164 primary particle Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910016629 MnBi Inorganic materials 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 34
- 239000000843 powder Substances 0.000 description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 230000009467 reduction Effects 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000011651 chromium Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910002546 FeCo Inorganic materials 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910001047 Hard ferrite Inorganic materials 0.000 description 2
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 229910000828 alnico Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- -1 Boron bromide compound Chemical class 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910016551 CuPt Inorganic materials 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 125000003289 ascorbyl group Chemical class [H]O[C@@]([H])(C([H])([H])O*)[C@@]1([H])OC(=O)C(O*)=C1O* 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- VDTVZBCTOQDZSH-UHFFFAOYSA-N borane N-ethylethanamine Chemical compound B.CCNCC VDTVZBCTOQDZSH-UHFFFAOYSA-N 0.000 description 1
- GKFJEDWZQZKYHV-UHFFFAOYSA-N borane;2-methylpropan-2-amine Chemical compound B.CC(C)(C)N GKFJEDWZQZKYHV-UHFFFAOYSA-N 0.000 description 1
- WVMHLYQJPRXKLC-UHFFFAOYSA-N borane;n,n-dimethylmethanamine Chemical compound B.CN(C)C WVMHLYQJPRXKLC-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- NNTOJPXOCKCMKR-UHFFFAOYSA-N boron;pyridine Chemical compound [B].C1=CC=NC=C1 NNTOJPXOCKCMKR-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- GBHRVZIGDIUCJB-UHFFFAOYSA-N hydrogenphosphite Chemical compound OP([O-])[O-] GBHRVZIGDIUCJB-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、磁気特性に優れ、且つ
コストパフォーマンスにも優れたボンド磁石用磁粉およ
びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a magnetic powder for bonded magnets having excellent magnetic properties and cost performance, and a method for producing the same.
【０００２】[0002]
【従来の技術】近年、電子機器、電子部品の発展に伴っ
て、これらに使用される永久磁石材料も多様なものが用
いられている。これらの永久磁石材料の態様としては、
大別して粉末冶金法もしくは鋳造法に代表されるバルク
磁石と、永久磁石粉を結合剤によって成形せしめたボン
ド磁石がある。かかるボンド磁石は形状の自由度、寸法
精度の良さ、軽量、等の長所を生かして増加の一途にあ
る。2. Description of the Related Art In recent years, with the development of electronic devices and electronic parts, various permanent magnet materials have been used. Examples of these permanent magnet materials include:
Broadly classified, there are a bulk magnet represented by a powder metallurgy method or a casting method, and a bonded magnet obtained by molding a permanent magnet powder with a binder. The number of such bonded magnets is increasing owing to their advantages such as freedom of shape, good dimensional accuracy, and light weight.
【０００３】かかるボンド磁石に使用される永久磁石材
料粉としては、ハードフェライト系、アルニコ系及び希
土類−遷移金属系が使用されており、例えば希土類−遷
移金属系としては、Ｓｍ−Ｃｏ系の１−５型、２−１７
型、Ｎｄ−Ｆｅ−Ｂ系、さらには最近発見され、現在研
究が進んでいるＳｍ−Ｆｅ−Ｎ系などが実用化、または
開発されつつある。これらの内で高磁気特性を要求され
る場合は、希土類−遷移金属系磁石粉を用いている。As the permanent magnet material powder used for such a bonded magnet, hard ferrite type, alnico type and rare earth-transition metal type are used. For example, rare earth-transition metal type is Sm-Co type. -5 type, 2-17
Type, Nd-Fe-B system, and more recently, Sm-Fe-N system, which has been recently discovered and is currently being researched, are being put to practical use or being developed. When high magnetic properties are required among these, rare earth-transition metal magnet powder is used.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、従来の
永久磁石粉は、ハードフェライトは安価であるが磁気特
性が低く、アルニコ系は比較的安価であるが磁気特性の
うち保磁力が低く、また希土類−遷移金属系は磁気特性
は高いもののかなり高価であるという問題がある。ま
た、従来のボンド磁石用磁粉は、いずれも冶金的手法に
よって製造されており、理論的に保有するｉＨｃよりか
なり低いレベルのｉＨｃしか実現されていない。この原
因は、冶金的手法の場合、合金もしくは酸化物を所望の
結晶系にするために、かなり高温での熱処理が必要であ
るため、内部に構造的な欠陥や、歪が残るためであると
考えられる。且つ、粉状とするためには、作製した合金
塊またはリボンを１ｍｍ以下の磁粉に粉砕する必要があ
るが、この場合はほとんどが機械的粉砕法によって磁粉
にしているのが現状である。このような機械的粉砕によ
っても磁粉内部に構造的な欠陥や歪が残るために、磁粉
のｉＨｃは理論的な値より相当下回ったものしか実現さ
れていない。However, in the conventional permanent magnet powder, hard ferrite is inexpensive but has low magnetic properties, and alnico series is relatively inexpensive, but coercive force is low among magnetic properties, and rare earth elements are also rare. -Transition metal systems have the problem that they are quite expensive although they have high magnetic properties. In addition, all the conventional magnetic powders for bonded magnets are manufactured by a metallurgical method, and only iHc at a level considerably lower than theoretically held iHc is realized. This is because the metallurgical method requires heat treatment at a considerably high temperature in order to make the alloy or oxide into a desired crystal system, so that structural defects and strain remain inside. Conceivable. Moreover, in order to make powder, it is necessary to crush the produced alloy lump or ribbon into magnetic powder of 1 mm or less, but in this case, most of them are magnetic powder by the mechanical pulverization method at present. Due to structural defects and strains remaining inside the magnetic powder even by such mechanical pulverization, only iHc of the magnetic powder is significantly lower than the theoretical value.
【０００５】[0005]
【課題を解決するための手段】本発明は、上記の様な従
来技術が有する問題を解決し、高い磁気特性を有し、コ
ストパフォーマンスに優れたボンド磁石用磁粉およびそ
の製造方法を提供することを目的とする。The present invention solves the problems of the prior art as described above, and provides a magnetic powder for bonded magnets having high magnetic properties and excellent cost performance, and a method for producing the same. With the goal.
【０００６】具体的には、本発明は、以下に述べる方法
により前述の従来技術の課題を解決するものである。 （１） 溶液中に溶解させた１種または２種以上の金属
塩と溶液中に溶解または分散させた沈殿剤とを混合し、
溶液中に前駆体として沈殿微粒子を生成させた後に、前
記微粒子を還元する方法で生成せしめた０．００１〜
１．０μｍの平均粒子径を有する合金微粒子の集合体で
あり、前記集合粒子の平均粒子径が１．０〜５００μｍ
であるボンド磁石用磁粉。 （２） 溶液中に溶解させた１種または２種以上の金属
塩または前記金属塩と非金属塩及び／または錯化剤を溶
液中に溶解または分散させた溶液と、還元剤を溶液中に
溶解または分散させた溶液を混合し反応せしめる方法で
生成せしめた０．００１〜１．０μｍの平均粒子径を有
する合金微粒子の集合体であり、前記集合粒子の平均粒
子径が１．０〜５００μｍであるボンド磁石用磁粉。 （３） 前記合金微粒子の集合体の容易磁化方向が一方
向に整列されている前記（１）または（２）記載のボン
ド磁石用磁粉。 （４） 前記合金微粒子がＦｅ、Ｃｏ、Ｎｉ、Ｍｎの少
なくとも１種以上を主成分とし、Ｂ、Ｃ、Ｎ、Ｐ、Ｓ
ｉ、Ａｌ、Ｔｉ、Ｖ、Ｍｏ、Ｐｔ、Ｐｄ、Ｇｅ、Ｇａ、
Ｓｎ、Ｚｒ、Ｎｂ、Ａｓ、Ｔａ、Ｈｆ、ＢｉまたはＣｒ
の内から選択される１種以上の元素を含有する前記
（１）、（２）または（３）記載のボンド磁石用磁粉。 （５） 前記合金微粒子の結晶構造が、ＡｕＣｕＩ型、
ＡｕＣｕ3 Ｉ型、ＭｎＢｉ型、Ｗ2 Ｃ型、ＣｕＰｔ型、
Ｎｉ2 Ｃｒ型、Ｃｒ2 Ａｌ型、ＣｕＡｕII型、Ｆｅ2 Ｐ
型、ＺｎＳ型、ＰｂＯ型、ＴｉＯ2 型、ＦｅＳ2 型、β
−Ｕ型、Ａｇ3 Ｍｇ型、Ｎｉ3 Ｖ型、Ｎｉ2 Ｉｎ型、Ｆ
ｅ3 Ｃ型のいずれか１種または複数の組合せである前記
（１）、（２）、（３）または（４）記載のボンド磁石
用磁粉。 （６） 溶液中に溶解させた１種または２種以上の金属
塩と溶液中に溶解または分散させた沈殿剤とを混合し、
溶液中に前駆体として沈殿微粒子を生成させた後に、前
記微粒子を還元する方法で０．００１〜１．０μｍの平
均粒子径を有する合金微粒子を生成せしめ、前記合金微
粒子を一次粒子として１．０〜５００μｍの平均粒子径
を有する集合体粒子としたボンド磁石用磁粉の製造方
法。 （７） 溶液中に溶解させた１種または２種以上の金属
塩または前記金属塩と非金属塩及び／または錯化剤を溶
液中に溶解または分散させた溶液と、還元剤を溶液中に
溶解または分散させた溶液を混合し反応せしめる方法で
０．００１〜１．０μｍの平均粒子径を有する合金微粒
子を生成せしめ、前記合金微粒子を一次粒子として１．
０〜５００μｍの平均粒子径を有する集合体粒子とした
ボンド磁石用磁粉の製造方法。 （８） 前記集合体粒子を形成する方法が、還元性もし
くは不活性雰囲気中での熱処理である前記（６）または
（７）記載のボンド磁石用磁粉の製造方法。Specifically, the present invention solves the above-mentioned problems of the prior art by the method described below. (1) Mixing one or more kinds of metal salts dissolved in a solution with a precipitant dissolved or dispersed in the solution,
After the precipitated fine particles were formed as a precursor in the solution, 0.001 produced by the method of reducing the fine particles
It is an aggregate of alloy fine particles having an average particle diameter of 1.0 μm, and the average particle diameter of the aggregate particles is 1.0 to 500 μm.
Is a magnetic powder for bonded magnets. (2) A solution in which one or more kinds of metal salts dissolved in a solution or the metal salt and a non-metal salt and / or a complexing agent are dissolved or dispersed in the solution, and a reducing agent in the solution. It is an aggregate of alloy fine particles having an average particle diameter of 0.001 to 1.0 μm produced by a method of mixing and reacting a dissolved or dispersed solution, and the average particle diameter of the aggregate particles is 1.0 to 500 μm. Is a magnetic powder for bonded magnets. (3) The magnetic powder for bonded magnets according to the above (1) or (2), wherein the easy magnetization direction of the alloy fine particle aggregate is aligned in one direction. (4) The alloy fine particles contain at least one of Fe, Co, Ni, and Mn as main components, and contain B, C, N, P, and S.
i, Al, Ti, V, Mo, Pt, Pd, Ge, Ga,
Sn, Zr, Nb, As, Ta, Hf, Bi or Cr
The magnetic powder for a bonded magnet according to the above (1), (2) or (3), which contains one or more elements selected from the above. (5) The crystal structure of the alloy fine particles is AuCuI type,
AuCu 3 I type, MnBi type, W 2 C type, CuPt type,
Ni 2 Cr type, Cr 2 Al type, CuAuII type, Fe 2 P
Type, ZnS type, PbO type, TiO 2 type, FeS 2 type, β
-U type, Ag 3 Mg type, Ni 3 V type, Ni 2 an In type, F
e 3 C type wherein is any one or more combinations of (1), (2), (3) or (4) magnetic powder for bonded magnets according. (6) Mixing one or more metal salts dissolved in a solution with a precipitant dissolved or dispersed in the solution,
After generating fine particles of a precipitate as a precursor in a solution, alloy fine particles having an average particle diameter of 0.001 to 1.0 μm are generated by a method of reducing the fine particles, and the fine alloy particles are used as primary particles to obtain 1.0. A method for producing magnetic powder for a bonded magnet, which is an aggregate particle having an average particle diameter of ˜500 μm. (7) One or more metal salts dissolved in a solution or a solution in which the metal salt and a non-metal salt and / or a complexing agent are dissolved or dispersed in a solution, and a reducing agent in the solution. 1. The alloy fine particles having an average particle diameter of 0.001 to 1.0 μm are produced by the method of mixing and reacting the dissolved or dispersed solutions, and the alloy fine particles are used as primary particles.
A method for producing magnetic powder for a bonded magnet, which comprises aggregate particles having an average particle diameter of 0 to 500 μm. (8) The method for producing a magnetic powder for a bonded magnet according to the above (6) or (7), wherein the method of forming the aggregate particles is a heat treatment in a reducing or inert atmosphere.
【０００７】[0007]
【作用】本発明のような構成とすることによって、粉砕
工程を必要としないため、高い磁気特性と高いコストパ
フォーマンスを兼ね備えたボンド磁石用磁粉およびその
製造方法を提供することが出来る。With the structure of the present invention, since no crushing step is required, it is possible to provide a magnetic powder for a bonded magnet having both high magnetic properties and high cost performance, and a method for producing the same.
【０００８】[0008]
【実施例】以下、本発明を実施例により説明するが、本
発明はこれらにより何ら制限されるものではない。EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited thereto.
【０００９】本発明における合金微粒子の合成方法は以
下の内容である。すなわち、本発明における合成方法の
１実施態様は溶液中で化学反応によって金属を含んだ沈
殿物を生成させるため、反応温度は通常は常温である。
使用する沈殿剤によっては、反応熱を伴うか、溶液の温
度を上昇させて行うものもあるが、この場合でも反応時
の温度は２００℃を超えることはない。さらに、沈殿微
粒子を還元気体中で合金微粒子とする場合も、熱処理温
度は８００℃までであり、粉末冶金法による合金化の温
度と比較するとかなり低温度で合金化出来る。更に他の
実施態様は、溶液中で金属塩及びまたは非金属塩を還元
剤を加えることによって直接合金化するものであり、こ
の場合も微粉生成過程において、過剰の熱や粉砕歪が入
ることはない。以上述べた本発明のように、複数の金属
イオンを化学反応によって沈殿させた場合、金属が分子
レベルで均一に混合された沈殿物が得られるため、低温
で容易に合金化、もしくは金属間化合物を作製すること
が可能となる。さらに、本発明のように溶液中で微粒子
を生成させることで、粉末冶金法のように粉砕をする必
要がなく、粉砕による歪、欠陥を残すこともない。この
ように、低温で目的とする単一金属または複数の金属か
らなる合金または金属間化合物を作製し、かつ粉砕工程
を経ないで金属微粒子を作製できる事より、従来技術の
欠点である磁粉内部の歪や欠陥を極力除去することが可
能となり、磁粉の磁気特性を向上させることが容易に達
成可能となる。The method for synthesizing the alloy fine particles in the present invention is as follows. That is, since one embodiment of the synthesis method of the present invention produces a precipitate containing a metal by a chemical reaction in a solution, the reaction temperature is usually room temperature.
Depending on the precipitating agent used, there are some which are accompanied by heat of reaction or by raising the temperature of the solution, but even in this case, the temperature during the reaction does not exceed 200 ° C. Further, even when the precipitated fine particles are made into alloy fine particles in a reducing gas, the heat treatment temperature is up to 800 ° C., and alloying can be performed at a considerably low temperature as compared with the alloying temperature by the powder metallurgy method. Still another embodiment is to directly alloy a metal salt and / or a non-metal salt in a solution by adding a reducing agent, and in this case too, excessive heat and crushing strain are not generated in the fine powder generation process. Absent. When a plurality of metal ions are precipitated by a chemical reaction as in the present invention described above, a precipitate in which the metals are uniformly mixed at the molecular level is obtained, which facilitates alloying at low temperatures or intermetallic compounds. Can be manufactured. Furthermore, by generating fine particles in a solution as in the present invention, it is not necessary to pulverize as in the powder metallurgy method, and distortion and defects due to pulverization are not left. In this way, it is possible to produce an alloy or intermetallic compound composed of a target single metal or a plurality of metals at a low temperature, and to produce fine metal particles without going through a crushing step. It is possible to remove the distortion and the defect as much as possible, and it is possible to easily improve the magnetic characteristics of the magnetic powder.
【００１０】さらに、本発明のボンド磁石用磁粉は上記
の製造方法によって合成された合金微粒子の平均粒子径
が０．００１〜１．０μｍである微粉を集合体としたも
のである。この合金微粒子の平均粒子径は上記の範囲で
実用上全く問題ないが、より高い磁気特性を得るために
は単磁区粒子径以下であることが好ましい。ボンド磁石
用の磁粉として必要な性状はその粒子径が１．０〜５０
０μｍであることが重要であり、前記の合成した微粉で
は粒子径が小さすぎる。よって、前記微粒子を集合体と
し、集合粒子の大きさを１．０〜５００μｍとすること
が本発明の重要な構成要素である。集合粒子が１．０μ
ｍ以下であるとボンド磁石とした場合、工程上の取扱い
がむずかしくなり、高い密度のボンド磁石が得られにく
く、５００μｍ以上になると、集合粒子そのものに空孔
を多く含むことになり好ましくない。Further, the magnetic powder for bonded magnets of the present invention is an aggregate of fine powders having the average particle diameter of the alloy fine particles synthesized by the above manufacturing method of 0.001 to 1.0 μm. The average particle size of the alloy fine particles is practically no problem within the above range, but it is preferably not more than the single domain particle size in order to obtain higher magnetic properties. The property required as magnetic powder for a bonded magnet is that the particle size is 1.0 to 50.
It is important that the particle size is 0 μm, and the particle size of the above-mentioned synthesized fine powder is too small. Therefore, it is an important component of the present invention that the fine particles are aggregated and the aggregated particles have a size of 1.0 to 500 μm. Aggregate particle is 1.0μ
If it is m or less, it becomes difficult to handle the bonded magnet in the process, and it is difficult to obtain a high-density bonded magnet. If it is 500 μm or more, the aggregated particles themselves include many voids, which is not preferable.
【００１１】本発明の微粒子の集合体において、磁気特
性の面から好ましくは、集合体を構成する微粒子の磁化
容易方向が一方向に整列していることである。このこと
によって、集合体粒子は異方性を有することになり、異
方性ボンド磁石が製造可能となる。In the aggregate of fine particles of the present invention, from the viewpoint of magnetic characteristics, it is preferable that the easy magnetization directions of the fine particles forming the aggregate are aligned in one direction. As a result, the aggregate particles have anisotropy, and the anisotropic bonded magnet can be manufactured.
【００１２】合金微粒子の集合体を作製する方法は、前
記合金微粉の溶液中での析出過程において凝集粒子とな
ることを利用することによって容易に達成できる。すな
わち、前駆体微粒子を生成させた後に還元する方法で
は、還元工程で熱処理を施す際に、微粒子の粒成長を起
こさない範囲で微粒子集合体粒子の形成と粒子径の制御
が可能である。また、溶液中で直接還元する方法におい
ては、反応後の凝集粒子を不活性ガス中で熱処理するこ
とによって、同様に集合体粒子を形成させることができ
る。前記の方法で作製した微粒子の集合体の粒子径をさ
らに制御するためには、集合体形成後に解砕を施して粒
度調整することが好ましい。The method of producing an aggregate of alloy fine particles can be easily achieved by utilizing the fact that the alloy fine powder becomes aggregated particles in the precipitation process in the solution. That is, in the method in which precursor particles are generated and then reduced, when heat treatment is performed in the reduction step, it is possible to form particle aggregate particles and control the particle diameter within a range that does not cause particle growth of the particles. Further, in the method of directly reducing in solution, aggregate particles can be similarly formed by heat-treating the aggregated particles after the reaction in an inert gas. In order to further control the particle size of the aggregate of fine particles produced by the above method, it is preferable to crush the aggregate after forming the aggregate to adjust the particle size.
【００１３】本発明における合金微粒子の組成として好
ましい態様は、Ｆｅ（鉄）、Ｃｏ（コバルト）、Ｎｉ
（ニッケル）、Ｍｎ（マンガン）の内１種以上を主成分
とし、Ｂ（ホウ素）、Ｃ（炭素）、Ｐ（リン）、Ｓｉ
（ケイ素）、Ａｌ（アルミニウム）、Ｔｉ（チタニウ
ム）、Ｇｅ（ゲルマニウム）、Ｇａ（ガリウム）、Ｖ
（バナジウム）、Ｍｏ（モリブデン）、Ｐｔ（白金）、
Ｐｄ（パラジウム）、Ｓｎ（すず）、Ｚｒ（ジルコニウ
ム）、Ｎｂ（ニオブ）、Ａｓ（ヒ素）、Ｔａ（タンタ
ル）、Ｈｆ（ハフニウム）、Ｂｉ（ビスマス）およびＣ
ｒ（クロム）から選択される１種以上の元素を含有する
ことが磁気特性の面から好ましい。添加元素の含有量は
５０原子％以下、特に３５原子％以下であることが好ま
しい。添加元素の含有量が前記範囲を超えると、飽和磁
化の大幅な低下を招き好ましくない。また、Ｆｅの一部
をＣｏまたはＮｉで置換することがより好ましい態様で
ある。A preferred embodiment of the composition of the alloy fine particles in the present invention is Fe (iron), Co (cobalt), Ni.
One or more of (nickel) and Mn (manganese) are the main components, and B (boron), C (carbon), P (phosphorus), Si
(Silicon), Al (aluminum), Ti (titanium), Ge (germanium), Ga (gallium), V
(Vanadium), Mo (molybdenum), Pt (platinum),
Pd (palladium), Sn (tin), Zr (zirconium), Nb (niobium), As (arsenic), Ta (tantalum), Hf (hafnium), Bi (bismuth) and C
From the viewpoint of magnetic properties, it is preferable to contain at least one element selected from r (chromium). The content of the additional element is preferably 50 atomic% or less, and particularly preferably 35 atomic% or less. When the content of the additional element exceeds the above range, the saturation magnetization is significantly reduced, which is not preferable. Further, it is a more preferable embodiment that a part of Fe is replaced with Co or Ni.
【００１４】本発明で合成される合金微粉は０．５ｋＯ
ｅ以上の保磁力を有することが必要である。高い保磁力
を得るためにはその結晶磁気異方性定数が高いことが好
ましく、そのためには結晶構造の対称性が低いことが重
要である。この観点からは、結晶系が六方晶、正方晶、
斜方晶であることが好ましく、さらには結晶構造がＡｕ
ＣｕＩ型、ＡｕＣｕ3 Ｉ型、ＭｎＢｉ型、Ｗ2 Ｃ型、Ｃ
ｕＰｔ型、Ｎｉ2 Ｃｒ型、Ｃｒ2 Ａｌ型、ＣｕＡｕII
型、Ｆｅ2 Ｐ型、ＺｎＳ型、ＰｂＯ型、ＴｉＯ2型、Ｆ
ｅＳ2 型、β−Ｕ型、Ａｇ3 Ｍｇ型、Ｎｉ3 Ｖ型、Ｎｉ
2 Ｉｎ型、Ｆｅ3Ｃ型のいずれか１種または複数の組合
せであることが好ましい。The fine alloy powder synthesized in the present invention is 0.5 kO.
It is necessary to have a coercive force of e or more. In order to obtain a high coercive force, it is preferable that the magnetocrystalline anisotropy constant is high, and for that purpose, it is important that the symmetry of the crystal structure is low. From this viewpoint, the crystal system is hexagonal, tetragonal,
It is preferably orthorhombic, and moreover, the crystal structure is Au.
CuI type, AuCu 3 I type, MnBi type, W 2 C type, C
uPt type, Ni 2 Cr type, Cr 2 Al type, CuAuII
Type, Fe 2 P type, ZnS type, PbO type, TiO 2 type, F
eS 2 type, β-U type, Ag 3 Mg type, Ni 3 V type, Ni
Any one of 2 In type and Fe 3 C type or a combination of a plurality of them is preferable.
【００１５】本発明における金属塩の塩とは、コスト面
と安定性の面から硫酸塩、硝酸塩、リン酸塩、塩化物を
用いることが好ましい。これらの塩を用いた場合は、反
応に供する溶液は通常は、水を用いるが、反応によって
は非水溶媒を用いることもできる。非水溶媒としては、
メタノール、エタノール、等のアルコール類、アセト
ン、メチルエチルケトン、等のケトン類、またはエーテ
ル類、等が例示できる。そして、沈殿剤とは、シュウ
酸、水酸化ナトリウム、水酸化カリウム、アンモニア
水、炭酸、硫化水素、等の金属元素と反応して溶液に難
溶性の沈殿物を生成するものである。As the metal salt of the present invention, it is preferable to use a sulfate, a nitrate, a phosphate or a chloride from the viewpoint of cost and stability. When these salts are used, water is usually used as the solution to be subjected to the reaction, but a non-aqueous solvent can be used depending on the reaction. As a non-aqueous solvent,
Examples thereof include alcohols such as methanol and ethanol, ketones such as acetone and methyl ethyl ketone, and ethers. The precipitating agent is one that reacts with metal elements such as oxalic acid, sodium hydroxide, potassium hydroxide, aqueous ammonia, carbonic acid and hydrogen sulfide to form a hardly soluble precipitate in the solution.
【００１６】さらに、本発明の他の金属塩の塩として
は、沈殿粒子の組成の均一性が良いことから金属アルコ
キシド、金属アセチルアセトナートなどの溶液中で水を
加えることによって容易に加水分解し、沈殿物を生成す
るものが好ましい態様である。これらの塩を用いた場合
の沈殿剤は水であり、溶媒は非水溶媒とする必要があ
る。加水分解を促進するために、溶液のｐＨ値を高くす
ることも可能である。特に、金属アセチルアセトナート
を用いた場合はアルカリ雰囲気にすることが好ましい。Further, as salts of other metal salts of the present invention, since the composition of the precipitated particles is good in uniformity, they can be easily hydrolyzed by adding water in a solution of metal alkoxide, metal acetylacetonate or the like. The one that produces a precipitate is a preferred embodiment. When these salts are used, the precipitant is water and the solvent needs to be a non-aqueous solvent. It is also possible to increase the pH value of the solution in order to accelerate the hydrolysis. In particular, when metal acetylacetonate is used, it is preferable to use an alkaline atmosphere.
【００１７】本発明における非金属塩とは、合金微粉中
に含有せしめる非金属元素を含有する化合物であり、ホ
ウ酸、リン酸などが例示出来る。The non-metal salt in the present invention is a compound containing a non-metal element contained in the alloy fine powder, and boric acid, phosphoric acid and the like can be exemplified.
【００１８】本発明における沈殿微粒子を還元する方法
は、一般的な還元性を有する気体を流通させながら熱処
理する方法、金属Ｃａまたは金属Ｍｇと混合し熱処理す
る方法、等を用いることができるが、還元性を有する気
体を流通させながら熱処理する方法が好ましい。ここ
で、還元性を有する気体とは、水素、一酸化炭素、アン
モニアガス、一酸化窒素、一酸化硫黄または、これらの
気体の混合気体である。コスト、安全性の面から好まし
くは水素もしくは一酸化炭素を用いることが良い。ま
た、還元時の熱処理温度は、目的とする金属の種類によ
んで適宜選択できるが、好ましくは７００℃以下であ
る。熱処理温度を高温にしすぎると金属微粒子の焼結現
象が起こり、粒子径の成長を伴うため保磁力の低下を招
く。As the method of reducing the precipitated fine particles in the present invention, a general method of heat treatment while passing a gas having a reducing property, a method of heat treatment by mixing with metal Ca or metal Mg, etc. can be used. A method of performing heat treatment while circulating a reducing gas is preferable. Here, the reducing gas is hydrogen, carbon monoxide, ammonia gas, nitric oxide, sulfur monoxide, or a mixed gas of these gases. From the viewpoint of cost and safety, hydrogen or carbon monoxide is preferably used. The heat treatment temperature at the time of reduction can be appropriately selected depending on the kind of the target metal, but is preferably 700 ° C. or lower. If the heat treatment temperature is too high, the sintering phenomenon of the metal fine particles occurs, and the coercive force is lowered because the particle diameter grows.
【００１９】本発明において溶液中で直接還元する場合
に用いられる還元剤とは還元作用を呈する物質であり、
次亜りん酸Ｎａなどの次亜りん酸塩、亜りん酸塩、亜り
ん酸水素塩、水素化ほう素Ｎａ、水素化ほう素Ｋ、水素
化ほう素ヒドラジン、水素化ほう素ピリジンなどの水素
化ほう素化合物、ジメチルアミンボラン、ジエチルアミ
ンボラン、トリメチルアミンボラン、第３ブチルアミン
ボラン、ピリジンボラン、ホルムアルデヒド、ヒドラジ
ン、塩酸ヒドラジン、硫酸ヒドラジン、グリオキシル
酸、ヒドロキシメチルスルフィン酸Ｎａ、ビピリジン、
アスコルビン酸Ｎａなどのアスコルビン酸塩、ヒドロキ
シルアミン塩酸塩、ぎ酸、酢酸、ベンジルアルコール、
メチルアルコールなどアルコール類などが例示できる。
尚、Ｌｉ、Ｋ、Ｂａ、Ｃａ、Ｎａ、Ｍｇ、Ａｌ、Ｔｉ、
Ｖ、Ｍｎなどの卑金属も本発明の還元剤の範ちゅうであ
る。還元剤は価格、反応性、溶解度、分散性などを考慮
し適宜選択しなければならない。In the present invention, the reducing agent used when directly reducing in a solution is a substance exhibiting a reducing action,
Hydrogen such as hypophosphite such as sodium hypophosphite, phosphite, hydrogen phosphite, sodium borohydride, boron hydride K, borohydride hydrazine, borohydride pyridine, etc. Boron bromide compound, dimethylamine borane, diethylamine borane, trimethylamine borane, tert-butylamine borane, pyridine borane, formaldehyde, hydrazine, hydrazine hydrochloride, hydrazine sulfate, glyoxylic acid, sodium hydroxymethylsulfinate, bipyridine,
Ascorbic acid salts such as sodium ascorbate, hydroxylamine hydrochloride, formic acid, acetic acid, benzyl alcohol,
Examples thereof include alcohols such as methyl alcohol.
In addition, Li, K, Ba, Ca, Na, Mg, Al, Ti,
Base metals such as V and Mn are also included in the reducing agent of the present invention. The reducing agent must be appropriately selected in consideration of price, reactivity, solubility, dispersibility and the like.
【００２０】しかしながら、還元剤はその酸化還元電位
が還元しようとする金属イオンの酸化還元電位よりも低
い場合にのみ金属イオンを還元でき、その結果、析出物
を得ることができるものであり、還元剤と金属塩の組合
せによっては必ずしも還元できるとは限らない。そこ
で、金属イオンの酸化還元電位を低下させる目的で錯化
剤を使用することは有効である。本発明に用いられる錯
化剤には−ＯＨ、−ＣＯＯＨ、＞Ｃ＝Ｏ、−Ｏ−、−Ｃ
ＯＯＲ、−ＣＯＮＨ2 、−ＮＯ、−ＮＯ2 、−ＳＯ
3 Ｈ、−ＰＨＯ（ＯＨ）、−Ｐ（ＯＨ）2 、−ＮＨ2 、
＞ＮＨ、＞Ｎ−、−Ｎ＝Ｎ−、＞Ｃ＝Ｎ−、−ＣＯＮＨ
2 、＞Ｃ＝Ｎ−ＯＨ、＞Ｃ＝ＮＨ、−ＳＨ、−Ｓ−、＞
Ｃ＝Ｓ、−ＣＯＳＨ、＞Ｐ−、などの配位基を有する化
合物であり、使用する金属塩類によって適宜選択するこ
とができ、１種または２種以上を使用することができ
る。また、これら錯化剤を金属イオンの溶媒中に於ける
安定化の目的で使用することもできる。However, the reducing agent can reduce the metal ion only when its redox potential is lower than the redox potential of the metal ion to be reduced, and as a result, a precipitate can be obtained. It is not always possible to reduce depending on the combination of the agent and the metal salt. Therefore, it is effective to use a complexing agent for the purpose of lowering the redox potential of metal ions. The complexing agent used in the present invention includes -OH, -COOH,> C = O, -O-, -C.
OOR, -CONH 2, -NO, -NO 2, -SO
3 H, -PHO (OH), - P (OH) 2, -NH 2,
>NH,> N-, -N = N-,> C = N-, -CONH
2 ,> C = N-OH,> C = NH, -SH, -S-,>
It is a compound having a coordinating group such as C = S, -COSH,> P-, and can be appropriately selected depending on the metal salt used, and one kind or two or more kinds can be used. Further, these complexing agents can be used for the purpose of stabilizing metal ions in a solvent.
【００２１】また、溶液中で直接還元して合金微粉を得
た場合は、その全部または一部が非晶質である場合があ
る。これは析出粉末中に多くの非金属元素を含有する場
合に多い傾向である。しかし、非晶質構造は磁気特性
上、特に保磁力に悪影響を及ぼすためこれらを結晶化さ
せることが好ましい。本発明に用いられる結晶化熱処理
とは、不活性雰囲気あるいは還元性雰囲気などの非酸化
性雰囲気中で加熱することであり、その雰囲気の選択、
加熱条件の設定は合金微粉の物性などを考慮し、行う必
要がある。When alloy fine powder is obtained by direct reduction in a solution, the whole or a part thereof may be amorphous. This tends to be the case when many non-metallic elements are contained in the precipitated powder. However, since the amorphous structure adversely affects the coercive force in terms of magnetic characteristics, it is preferable to crystallize them. The crystallization heat treatment used in the present invention is heating in a non-oxidizing atmosphere such as an inert atmosphere or a reducing atmosphere, and the selection of the atmosphere,
It is necessary to set the heating conditions in consideration of the physical properties of the fine alloy powder.
【００２２】次に、本発明の製造方法を、従来技術との
比較においてその効果を示すために、具体的な実験手順
とともに述べる。Next, the manufacturing method of the present invention will be described together with specific experimental procedures in order to show its effect in comparison with the prior art.
【００２３】（実施例１）出発原料としてＦｅＣｌ2 ・
７Ｈ2 Ｏ：１９．５ｇとＣｏＣｌ2 ・６Ｈ2 Ｏ：７．１
ｇを１００ｍｌイオン交換水に溶解させ、さらにＮａＯ
Ｈ：２０ｇをイオン交換水に溶解させた。ＦｅとＣｏ金
属塩が溶解している溶液にＮａＯＨ水溶液を室温でゆっ
くりと攪はんしながら添加した。この時すぐに沈殿物が
生成した。この状態で１０分間攪はんを行なった後に、
過剰のイオン交換水を加えて、溶液ｐＨ値が７になるま
で沈殿物の洗浄を行った。得られた沈殿物を１００℃の
温度で乾燥し、還元処理前の前駆体微粉を得た。次い
で、水素気流中（３００ｍｌ／分）で４００℃×４ｈｒ
の熱処理を行った。還元処理後の磁粉はトルエンに浸漬
して取り出し、空気中でトルエンを蒸発させることで徐
々に表面を酸化させた。(Example 1) FeCl 2 · as a starting material
7H 2 O: 19.5 g and CoCl 2 · 6H 2 O: 7.1
g was dissolved in 100 ml of ion-exchanged water, and NaO was added.
H: 20 g was dissolved in ion-exchanged water. An aqueous solution of NaOH was added to the solution in which the Fe and Co metal salts were dissolved at room temperature with slow stirring. A precipitate formed immediately at this time. After stirring for 10 minutes in this state,
Excess ion-exchanged water was added, and the precipitate was washed until the solution pH value became 7. The obtained precipitate was dried at a temperature of 100 ° C. to obtain precursor fine powder before reduction treatment. Next, in a hydrogen stream (300 ml / min), 400 ° C x 4 hr
Was heat treated. The magnetic powder after the reduction treatment was immersed in toluene and taken out, and the surface was gradually oxidized by evaporating toluene in the air.
【００２４】還元されたＦｅＣｏ粒子の形態観察を電子
顕微鏡で実施したところ、合金微粒子の平均粒子径は
０．１μｍであり、その集合体の平均粒子径は５μｍで
あった。また、ＶＳＭ（試料振動型磁力計）により前記
磁粉の磁気特性を測定した結果、σ＝１７５ｅｍｕ／
ｇ、ｉＨｃ＝１．２ｋＯｅであった。When the morphology of the reduced FeCo particles was observed with an electron microscope, the average particle diameter of the alloy fine particles was 0.1 μm, and the average particle diameter of the aggregate was 5 μm. In addition, as a result of measuring the magnetic characteristics of the magnetic powder with a VSM (sample vibrating magnetometer), σ = 175 emu /
g, iHc = 1.2 kOe.
【００２５】（実施例２）出発原料としてＦｅ（Ｏ−ｎ
−Ｃ3 Ｈ7 ）3 ：２ｇ、Ｃｏ（Ｏ−ｎ−Ｃ3 Ｈ7）3 ：
１．５２ｇ、を乾燥したｎ−Ｃ3 Ｈ7 ＯＨ中に溶解し、
均一溶液を調製した。次ぎに、調製した溶液を８０℃に
保持しながら、蒸留水：１．５５ｇとｎ−Ｃ3 Ｈ7 Ｏ
Ｈ：１５．５ｍｌとを混合した溶液を加え、沈殿物を生
成させた。生成した沈殿物を遠心分離して取り出した
後、得られた沈殿物を１００℃の温度で乾燥し、還元処
理前の前駆体微粉を得た。次いで、水素気流中（３００
ｍｌ／分）で４００℃×４ｈｒの熱処理を行った。還元
処理後の磁粉はトルエンに浸漬して取り出し、空気中で
トルエンを蒸発させることで徐々に表面を酸化させた。Example 2 Fe (O-n) was used as a starting material.
-C 3 H 7) 3: 2g , Co (O-n-C 3 H 7) 3:
1.52 g, was dissolved in n-C 3 in H 7 OH drying the,
A homogeneous solution was prepared. Next, while maintaining the prepared solution at 80 ° C., distilled water: 1.55 g and n-C 3 H 7 O were added.
A solution in which H: 15.5 ml was mixed was added to generate a precipitate. The produced precipitate was centrifuged and taken out, and then the obtained precipitate was dried at a temperature of 100 ° C. to obtain a precursor fine powder before the reduction treatment. Then, in a hydrogen stream (300
Heat treatment was performed at 400 ° C. for 4 hours at (ml / min). The magnetic powder after the reduction treatment was immersed in toluene and taken out, and the surface was gradually oxidized by evaporating toluene in the air.
【００２６】還元されたＦｅＣｏ粒子の形態観察を電子
顕微鏡で実施したところ、平均粒子径は０．１μｍであ
り、その集合体の平均粒子径は１０μｍであった。ま
た、ＶＳＭにより前記磁粉の磁気特性を測定した結果、
σ＝１８３ｅｍｕ／ｇ、ｉＨｃ＝１．５ｋＯｅであっ
た。When the morphology of the reduced FeCo particles was observed with an electron microscope, the average particle diameter was 0.1 μm, and the average particle diameter of the aggregate was 10 μm. In addition, as a result of measuring the magnetic characteristics of the magnetic powder by VSM,
σ = 183 emu / g, iHc = 1.5 kOe.
【００２７】（実施例３）イオン交換水１００ｍｌにＦ
ｅＳＯ4 ・７Ｈ2 Ｏを１９．４６ｇ、ＣｏＣｌ2・６Ｈ
2 Ｏを３．９０ｇ加え攪はん溶解し、塩溶液を得た。ま
た、イオン交換水１００ｍｌに水素化ほう素カリウムを
５３．３４ｇを加え攪はん混合し、還元剤溶液を得た。
これら塩溶液と還元剤溶液を混合攪はんし、反応せしめ
て析出粉末を得、ろ過、洗浄を行った後、アルゴンガス
雰囲気中で１５０℃、２時間の結晶化熱処理を行った。
作製した磁石粉末の形態観察を電子顕微鏡で実施したと
ころ、合金微粒子の平均粒子径は０．０５μｍであり、
その集合体の平均粒子径は３μｍであった。また、作製
した磁石粉末の磁気特性をＶＳＭを用いて測定したとこ
ろ、σ＝１５６ｅｍｕ／ｇ、ｉＨｃ＝１．０２ｋＯｅで
あった。(Example 3) F was added to 100 ml of deionized water.
eSO 4 · 7H 2 O and 19.46g, CoCl 2 · 6H
2.90 g of 2 O was added and dissolved with stirring to obtain a salt solution. Further, 53.34 g of potassium borohydride was added to 100 ml of ion-exchanged water and mixed by stirring to obtain a reducing agent solution.
These salt solution and reducing agent solution were mixed and stirred to react with each other to obtain a precipitated powder, which was filtered and washed, and then heat-treated for crystallization at 150 ° C. for 2 hours in an argon gas atmosphere.
When the morphology of the produced magnet powder was observed with an electron microscope, the average particle diameter of the alloy fine particles was 0.05 μm,
The average particle size of the aggregate was 3 μm. Moreover, when the magnetic characteristics of the produced magnet powder were measured using VSM, σ = 156 emu / g and iHc = 1.02 kOe.
【００２８】（比較例１）出発原料として、Ｆｅ金属塊
とＣｏ金属塊をＦｅ70Ｃｏ30（原子％）の組成となるよ
うにアーク溶解によって合金化した。得られた合金塊を
スタンプミルによって粗粉砕を行い、次いで遊星型ボー
ルミルによって、有機溶媒中で２００ｒｐｍ×１０時間
の条件で微粉砕を行なった。(Comparative Example 1) As starting materials, Fe metal lumps and Co metal lumps were alloyed by arc melting so as to have a composition of Fe 70 Co 30 (atomic%). The obtained alloy lump was roughly pulverized by a stamp mill, and then finely pulverized by a planetary ball mill in an organic solvent under the conditions of 200 rpm × 10 hours.
【００２９】得られたＦｅＣｏ粒子の形態観察を電子顕
微鏡で実施したところ、平均粒子径は１．０μｍであっ
た。また、ＶＳＭにより前記磁粉の磁気特性を測定した
結果、σ＝１８５ｅｍｕ／ｇ、ｉＨｃ＝０．１ｋＯｅで
あった。When the morphology of the obtained FeCo particles was observed with an electron microscope, the average particle size was 1.0 μm. Moreover, as a result of measuring the magnetic characteristics of the magnetic powder by VSM, σ = 185 emu / g and iHc = 0.1 kOe.
【００３０】以上の本発明による実施例１〜３と従来技
術である比較例１との比較より明かなように、本発明に
よれば高いσ（飽和磁化）を維持したまま、保磁力を大
幅に向上させることが可能となる。As is clear from the comparison between Examples 1 to 3 according to the present invention and Comparative Example 1 which is a conventional technique, according to the present invention, the coercive force is significantly increased while maintaining a high σ (saturation magnetization). It is possible to improve.
【００３１】[0031]
【発明の効果】以上、詳述したように本発明によれば、
高い飽和磁化を維持したまま、良好な保磁力を有する永
久磁石粉を、従来のように粉砕工程を必要としない簡便
なプロセスで実現することが可能となり、コストパフォ
ーマンスに優れたボンド磁石用磁粉を提供することが出
来る。As described above in detail, according to the present invention,
It is possible to realize permanent magnet powder with good coercive force while maintaining high saturation magnetization by a simple process that does not require a crushing step as in the past, and to provide magnetic powder for bonded magnets with excellent cost performance. Can be provided.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ２２Ｃ 33/02 Ｇ Ｈ０１Ｆ 1/04 1/08 Ａ // Ｈ０１Ｆ 7/02 Ａ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Internal reference number FI Technical display location C22C 33/02 G H01F 1/04 1/08 A // H01F 7/02 A
Claims (8)
の金属塩と溶液中に溶解または分散させた沈殿剤とを混
合し、溶液中に前駆体として沈殿微粒子を生成させた後
に、前記微粒子を還元する方法で生成せしめた０．００
１〜１．０μｍの平均粒子径を有する合金微粒子の集合
体であり、前記集合粒子の平均粒子径が１．０〜５００
μｍであるボンド磁石用磁粉。1. A mixture of one or more kinds of metal salts dissolved in a solution and a precipitant dissolved or dispersed in the solution to form fine particles of a precipitate as a precursor in the solution, 0.00 produced by the method of reducing the fine particles
It is an aggregate of alloy fine particles having an average particle diameter of 1 to 1.0 μm, and the average particle diameter of the aggregate particles is 1.0 to 500.
Magnetic powder for bonded magnets having a size of μm.
の金属塩または前記金属塩と非金属塩及び／または錯化
剤を溶液中に溶解または分散させた溶液と、還元剤を溶
液中に溶解または分散させた溶液を混合し反応せしめる
方法で生成せしめた０．００１〜１．０μｍの平均粒子
径を有する合金微粒子の集合体であり、前記集合粒子の
平均粒子径が１．０〜５００μｍであるボンド磁石用磁
粉。2. A solution in which one or more metal salts dissolved in a solution, or a solution in which the metal salt and a non-metal salt and / or a complexing agent are dissolved or dispersed in a solution, and a reducing agent in solution It is an aggregate of alloy fine particles having an average particle diameter of 0.001 to 1.0 μm produced by a method of mixing and reacting a solution dissolved or dispersed therein, and the average particle diameter of the aggregate particles is 1.0. Magnetic powder for a bonded magnet having a size of 500 μm.
が一方向に整列されている請求項１または請求項２記載
のボンド磁石用磁粉。3. The magnetic powder for a bonded magnet according to claim 1 or 2, wherein the direction of easy magnetization of the aggregate of alloy fine particles is aligned in one direction.
ｎの少なくとも１種以上を主成分とし、Ｂ、Ｃ、Ｎ、
Ｐ、Ｓｉ、Ａｌ、Ｔｉ、Ｖ、Ｍｏ、Ｐｔ、Ｐｄ、Ｇｅ、
Ｇａ、Ｓｎ、Ｚｒ、Ｎｂ、Ａｓ、Ｔａ、Ｈｆ、Ｂｉまた
はＣｒの内から選択される１種以上の元素を含有する請
求項１、２または請求項３記載のボンド磁石用磁粉。4. The fine alloy particles are Fe, Co, Ni, M.
n, at least one or more of the main components, B, C, N,
P, Si, Al, Ti, V, Mo, Pt, Pd, Ge,
The magnetic powder for bonded magnets according to claim 1, 2 or 3, which contains at least one element selected from the group consisting of Ga, Sn, Zr, Nb, As, Ta, Hf, Bi and Cr.
Ｉ型、ＡｕＣｕ3 Ｉ型、ＭｎＢｉ型、Ｗ2 Ｃ型、ＣｕＰ
ｔ型、Ｎｉ2 Ｃｒ型、Ｃｒ2 Ａｌ型、ＣｕＡｕII型、Ｆ
ｅ2 Ｐ型、ＺｎＳ型、ＰｂＯ型、ＴｉＯ2 型、ＦｅＳ2
型、β−Ｕ型、Ａｇ3 Ｍｇ型、Ｎｉ3 Ｖ型、Ｎｉ2 Ｉｎ
型、Ｆｅ3 Ｃ型のいずれか１種または複数の組合せであ
る請求項１、２、３または請求項４記載のボンド磁石用
磁粉。5. The crystal structure of the alloy fine particles is AuCu
I type, AuCu 3 I type, MnBi type, W 2 C type, CuP
t type, Ni 2 Cr type, Cr 2 Al type, CuAuII type, F
e 2 P type, ZnS type, PbO type, TiO 2 type, FeS 2
Type, β-U type, Ag 3 Mg type, Ni 3 V type, Ni 2 In
5. The magnetic powder for a bonded magnet according to claim 1, 2, 3 or 4, which is one type or a combination of a plurality of types of Fe 3 C type and Fe 3 C type.
の金属塩と溶液中に溶解または分散させた沈殿剤とを混
合し、溶液中に前駆体として沈殿微粒子を生成させた後
に、前記微粒子を還元する方法で０．００１〜１．０μ
ｍの平均粒子径を有する合金微粒子を生成せしめ、前記
合金微粒子を一次粒子として１．０〜５００μｍの平均
粒子径を有する集合体粒子としたボンド磁石用磁粉の製
造方法。6. A mixture of one or more kinds of metal salts dissolved in a solution and a precipitant dissolved or dispersed in the solution to form fine particles of a precipitate as a precursor in the solution, 0.001-1.0μ by the method of reducing the fine particles
A method for producing magnetic powder for a bonded magnet, wherein alloy fine particles having an average particle diameter of m are produced, and the alloy fine particles are used as primary particles to form aggregate particles having an average particle diameter of 1.0 to 500 μm.
の金属塩または前記金属塩と非金属塩及び／または錯化
剤を溶液中に溶解または分散させた溶液と、還元剤を溶
液中に溶解または分散させた溶液を混合し反応せしめる
方法で０．００１〜１．０μｍの平均粒子径を有する合
金微粒子を生成せしめ、前記合金微粒子を一次粒子とし
て１．０〜５００μｍの平均粒子径を有する集合体粒子
としたボンド磁石用磁粉の製造方法。7. A solution in which one or more metal salts dissolved in a solution or a solution in which the metal salt and a non-metal salt and / or a complexing agent are dissolved or dispersed in a solution, and a reducing agent in solution An alloy fine particle having an average particle diameter of 0.001 to 1.0 μm is produced by a method of mixing and reacting a solution dissolved or dispersed therein, and the alloy fine particle is a primary particle and an average particle diameter of 1.0 to 500 μm. A method for producing a magnetic powder for a bonded magnet, which is an aggregate particle having:
性もしくは不活性雰囲気中での熱処理である請求項６ま
たは請求項７記載のボンド磁石用磁粉の製造方法。8. The method for producing magnetic powder for a bonded magnet according to claim 6, wherein the method of forming the aggregate particles is a heat treatment in a reducing or inert atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4341284A JPH06163231A (en) | 1992-11-26 | 1992-11-26 | Magnetic powder for bonded magnet and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4341284A JPH06163231A (en) | 1992-11-26 | 1992-11-26 | Magnetic powder for bonded magnet and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06163231A true JPH06163231A (en) | 1994-06-10 |
Family
ID=18344866
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4341284A Pending JPH06163231A (en) | 1992-11-26 | 1992-11-26 | Magnetic powder for bonded magnet and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06163231A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000212610A (en) * | 1999-01-27 | 2000-08-02 | Tsurumi Soda Co Ltd | Production of alloy powder and iron powder |
| JP2004056091A (en) * | 2002-05-31 | 2004-02-19 | Fuji Photo Film Co Ltd | Magnetic particle and its manufacturing method, and magnetic recording medium and its manufacturing method |
-
1992
- 1992-11-26 JP JP4341284A patent/JPH06163231A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000212610A (en) * | 1999-01-27 | 2000-08-02 | Tsurumi Soda Co Ltd | Production of alloy powder and iron powder |
| JP2004056091A (en) * | 2002-05-31 | 2004-02-19 | Fuji Photo Film Co Ltd | Magnetic particle and its manufacturing method, and magnetic recording medium and its manufacturing method |
| JP4524078B2 (en) * | 2002-05-31 | 2010-08-11 | 富士フイルム株式会社 | Magnetic particle and method for manufacturing the same, and magnetic recording medium and method for manufacturing the same |
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