WO2016009926A1 - 磁性合金粒子が担持された磁性材料及び該磁性材料の製造方法 - Google Patents
磁性合金粒子が担持された磁性材料及び該磁性材料の製造方法 Download PDFInfo
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- WO2016009926A1 WO2016009926A1 PCT/JP2015/069692 JP2015069692W WO2016009926A1 WO 2016009926 A1 WO2016009926 A1 WO 2016009926A1 JP 2015069692 W JP2015069692 W JP 2015069692W WO 2016009926 A1 WO2016009926 A1 WO 2016009926A1
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- alloy
- magnetic
- particles
- magnetic material
- solution
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- 239000002245 particle Substances 0.000 title claims abstract description 136
- 239000000696 magnetic material Substances 0.000 title claims abstract description 91
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 133
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 96
- 239000000956 alloy Substances 0.000 claims abstract description 96
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 64
- 229910005335 FePt Inorganic materials 0.000 claims abstract description 46
- 230000005291 magnetic effect Effects 0.000 claims abstract description 44
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 229910018979 CoPt Inorganic materials 0.000 claims abstract description 23
- -1 silicic acid compound Chemical class 0.000 claims abstract description 15
- 229910001260 Pt alloy Inorganic materials 0.000 claims abstract description 13
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910015187 FePd Inorganic materials 0.000 claims abstract description 7
- 229910052788 barium Inorganic materials 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 82
- 239000000693 micelle Substances 0.000 claims description 59
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 59
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 54
- 229910052751 metal Inorganic materials 0.000 claims description 41
- 239000002184 metal Substances 0.000 claims description 41
- 239000002131 composite material Substances 0.000 claims description 33
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 29
- 150000004692 metal hydroxides Chemical class 0.000 claims description 29
- 239000011259 mixed solution Substances 0.000 claims description 25
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 24
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000004094 surface-active agent Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 239000012071 phase Substances 0.000 claims description 17
- 229910052697 platinum Inorganic materials 0.000 claims description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 15
- 239000008346 aqueous phase Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000003921 oil Substances 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 10
- 150000003377 silicon compounds Chemical class 0.000 claims description 10
- 230000003472 neutralizing effect Effects 0.000 claims description 9
- 239000010420 shell particle Substances 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 8
- 150000002736 metal compounds Chemical class 0.000 claims description 8
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000007771 core particle Substances 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 2
- LMSDCGXQALIMLM-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;iron Chemical compound [Fe].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O LMSDCGXQALIMLM-UHFFFAOYSA-N 0.000 claims description 2
- YNVZDODIHZTHOZ-UHFFFAOYSA-K 2-hydroxypropanoate;iron(3+) Chemical compound [Fe+3].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O YNVZDODIHZTHOZ-UHFFFAOYSA-K 0.000 claims description 2
- HKMVWLQFAYGKSI-UHFFFAOYSA-N 3-triethoxysilylpropyl thiocyanate Chemical compound CCO[Si](OCC)(OCC)CCCSC#N HKMVWLQFAYGKSI-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- CTUFHBVSYAEMLM-UHFFFAOYSA-N acetic acid;platinum Chemical compound [Pt].CC(O)=O.CC(O)=O CTUFHBVSYAEMLM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000941 alkaline earth metal alloy Inorganic materials 0.000 claims description 2
- 229960000686 benzalkonium chloride Drugs 0.000 claims description 2
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims description 2
- 229940115457 cetyldimethylethylammonium bromide Drugs 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 2
- BTMQKQSSEQVSAS-UHFFFAOYSA-N cobalt;ethane-1,2-diamine Chemical compound [Co].NCCN BTMQKQSSEQVSAS-UHFFFAOYSA-N 0.000 claims description 2
- HEWFKXVSWQSSAT-UHFFFAOYSA-M cyclopenta-1,3-diene;cyclopenta-2,4-dien-1-ylidenemethanolate;iron(2+) Chemical compound [Fe+2].C=1C=C[CH-]C=1.[O-]C=C1C=CC=C1 HEWFKXVSWQSSAT-UHFFFAOYSA-M 0.000 claims description 2
- XWEQEWRSGBDFPF-UHFFFAOYSA-N ethane-1,2-diamine;iron Chemical compound [Fe].NCCN XWEQEWRSGBDFPF-UHFFFAOYSA-N 0.000 claims description 2
- WMNIETDRLRTYFX-UHFFFAOYSA-N ethane-1,2-diamine;platinum Chemical compound [Pt].NCCN WMNIETDRLRTYFX-UHFFFAOYSA-N 0.000 claims description 2
- VUFOSBDICLTFMS-UHFFFAOYSA-M ethyl-hexadecyl-dimethylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CC VUFOSBDICLTFMS-UHFFFAOYSA-M 0.000 claims description 2
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 2
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- UQPUONNXJVWHRM-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 UQPUONNXJVWHRM-UHFFFAOYSA-N 0.000 claims description 2
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 2
- XAKYZBMFCZISAU-UHFFFAOYSA-N platinum;triphenylphosphane Chemical compound [Pt].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 XAKYZBMFCZISAU-UHFFFAOYSA-N 0.000 claims description 2
- 229940096992 potassium oleate Drugs 0.000 claims description 2
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 2
- YLLIGHVCTUPGEH-UHFFFAOYSA-M potassium;ethanol;hydroxide Chemical compound [OH-].[K+].CCO YLLIGHVCTUPGEH-UHFFFAOYSA-M 0.000 claims description 2
- 229960005480 sodium caprylate Drugs 0.000 claims description 2
- NRHMKIHPTBHXPF-TUJRSCDTSA-M sodium cholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 NRHMKIHPTBHXPF-TUJRSCDTSA-M 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- BYKRNSHANADUFY-UHFFFAOYSA-M sodium octanoate Chemical compound [Na+].CCCCCCCC([O-])=O BYKRNSHANADUFY-UHFFFAOYSA-M 0.000 claims description 2
- 229940080350 sodium stearate Drugs 0.000 claims description 2
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims 1
- YJUCUHWJIRKDCB-UHFFFAOYSA-N NCCNCCNC(C)O[Si](OCC)(OCC)CCC Chemical compound NCCNCCNC(C)O[Si](OCC)(OCC)CCC YJUCUHWJIRKDCB-UHFFFAOYSA-N 0.000 claims 1
- 239000007983 Tris buffer Substances 0.000 claims 1
- YHKQKQUREYJYDC-UHFFFAOYSA-J [Co+4].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O Chemical compound [Co+4].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O YHKQKQUREYJYDC-UHFFFAOYSA-J 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 229920000136 polysorbate Polymers 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 230000001568 sexual effect Effects 0.000 claims 1
- 229940083542 sodium Drugs 0.000 claims 1
- 229910021296 Co3Pt Inorganic materials 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 25
- 239000000203 mixture Substances 0.000 description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 230000005415 magnetization Effects 0.000 description 17
- 239000002243 precursor Substances 0.000 description 16
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000000921 elemental analysis Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000010419 fine particle Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 150000002739 metals Chemical class 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000003917 TEM image Methods 0.000 description 8
- 239000011575 calcium Substances 0.000 description 8
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- 239000000470 constituent Substances 0.000 description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000003991 Rietveld refinement Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 241000238366 Cephalopoda Species 0.000 description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 239000006247 magnetic powder Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000007605 air drying Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 150000004696 coordination complex Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000003302 ferromagnetic material Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
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- 101001094831 Homo sapiens Phosphomannomutase 2 Proteins 0.000 description 1
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- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- ICSSIKVYVJQJND-UHFFFAOYSA-N calcium nitrate tetrahydrate Chemical compound O.O.O.O.[Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ICSSIKVYVJQJND-UHFFFAOYSA-N 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- VNRDAMBPFDPXSM-UHFFFAOYSA-N n'-[2-(3-triethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCNCCN VNRDAMBPFDPXSM-UHFFFAOYSA-N 0.000 description 1
- DIOQZVSQGTUSAI-UHFFFAOYSA-N n-butylhexane Natural products CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 1
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- 229910000077 silane Inorganic materials 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
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Abstract
Description
(a)原料ミセル溶液の作製
6mLの純水に、FeとPtとの合計で0.12Mとなるように、硝酸鉄(Fe(NO3)3・9H2O)と塩化白金酸(H2[PtCl6]・xH2O)を添加した。更に、硝酸バリウム(Ba(NO3)2)を18.82mg(Ba:0.012M)を添加した。アルカリ土類金属であるバリウムの仕込み量は、金属(Fe+Pt)に対してモル比で0.1となる。この水溶液に油相となる有機溶媒としてオクタン18.3mLとブタノール3.6mLを添加し、界面活性剤としてCTAB3.52gを添加した。この溶液を均一になるまで30分間攪拌し、原料ミセル溶液を作製した。以上の操作は室温で行っている。尚、原料ミセル溶液は、FeとPtの比率(Fe:Pt)が、5:5(実施例1)、10:0(参考例1)、9:1(参考例2)、0:10(参考例3)となるように複数の溶液を作製した。また、比較例1としてBa添加のない原料ミセル溶液も作製した(Fe:Ptは5:5である。)。
3.74mLの純水に中和剤としてアンモニア(25%-NH3水溶液)を2.26mL添加した。この溶液に、オクタン18.3mLとブタノール3.6mLを添加し、更に、CTAB3.52gを添加した。この溶液を均一になるまで30分間攪拌し、中和剤ミセル溶液を作製した。
作製した原料ミセル溶液に、中和剤ミセル溶液を1滴/secで滴下した。中和剤ミセル溶液の添加の際は、混合溶液を攪拌しつつ行い、添加完了後も30分間攪拌した。
上記で作製した混合溶液に、TEOS1.5mLを2滴/secで滴下して添加した。このときSiの添加量は、原料ミセル溶液中の金属(Fe+Pt)の量に対してモル比で9.4となる。添加完了後、混合溶液を攪拌しつつ20時間かけて反応させた。これにより水酸化物粒子表面にシリカが析出して粒子を被覆し、沈殿が生じた。そこで、溶液を遠心分離(3500rpm、5分間)して固形分を回収し、これをメタノールとクロロホルムとの混合液で洗浄して遠心分離し、更にメタノールで洗浄して遠心分離した。得られた固形分について乾燥(大気乾燥後に真空乾燥)して磁性材料の前駆体となる複合水酸化物粒子/シリカのコア/シェル粒子を得た。
前駆体について、水素雰囲気中980℃で4時間加熱する焼成熱処理を行った。
第1実施形態の磁性材料(FePt合金粒子)の製造工程と同様の工程にてCoPt合金粒子をシリカ被覆した磁性材料を製造した。原料ミセル溶液の作製工程において、6mLの純水に、CoとPtとの合計で0.12Mとなるように、硝酸コバルト(Co(NO3)2・6H2O)と塩化白金酸を添加した。ここに、第1実施形態と同様に、硝酸バリウムを添加し、その後、油相(オクタン+ブタノール)、界面活性剤(CTAB)を添加した。バリウム及び各添加剤の添加量は第1実施形態と同様としている。そして、この溶液を攪拌して原料ミセル溶液とした。原料ミセル溶液のCoとPtの比率(Co:Pt)が、5:5(実施例2)、10:0(参考例4)、9:1(参考例5)、0:10(参考例6)となるように複数の溶液を作製した。比較例2としてBa添加のない原料ミセル溶液も作製した(Co:Ptは5:5である。)。
この実施形態は、第1実施形態のFePt合金粒子を基本としつつ、原料の使用量等を4倍量にしてFePt合金粒子(実施例3)を製造した。
(a)原料ミセル溶液の作製
24mLの純水に、FeとPtとの合計で0.12Mとなるように、硝酸鉄(Fe(NO3)3・9H2O)と塩化白金酸(H2[PtCl6]・xH2O)を添加した。更に、硝酸バリウム(Ba(NO3)2)を75.32mg(Ba:0.012M)を添加した。アルカリ土類金属であるバリウムの仕込み量は、金属(Fe、Pt)に対してモル比([A]/[M+PM])で0.1となる。この水溶液に油相となる有機溶媒としてオクタン73.2mLとブタノール14.4mLを添加し、界面活性剤としてCTAB14.08gを添加した。この溶液を均一になるまで90分間攪拌し、原料ミセル溶液を作製した。以上の操作は室温で行っている。この原料ミセル溶液は、FeとPtの比率(Fe:Pt)が、実施例1と同様に5:5である。
14.96mLの純水に中和剤としてアンモニア(25%-NH3水溶液)を9.04mL添加した。この溶液に、オクタン73.2mLとブタノール14.4mLを添加し、更に、CTAB14.08gを添加した。この溶液を均一になるまで90分間攪拌し、中和剤ミセル溶液を作製した。
作製した原料ミセル溶液に、中和剤ミセル溶液を1滴/secで滴下した。中和剤ミセル溶液の添加の際は、混合溶液を攪拌しつつ行い、添加完了後も30分間攪拌した。
上記で作製した混合溶液に、TEOS6.0mLを2滴/secで滴下して添加した。このときSiの添加量([Si])は、原料ミセル溶液中の金属(Fe、Pt)のモル数([M+PM])に対してモル比率9.4となる。添加完了後、混合溶液を攪拌しつつ20時間かけて反応させた。これにより水酸化物粒子表面にシリカが析出して粒子を被覆し、沈殿が生じた。そこで、溶液を遠心分離(3500rpm、5分間)して固形分を回収し、これをメタノールとクロロホルムとの混合液で洗浄して遠心分離し、更にメタノールで洗浄して遠心分離した。得られた固形分について乾燥(大気乾燥後に真空乾燥)して磁性材料の前駆体となる複合水酸化物粒子/シリカのコア/シェル粒子を得た。
前駆体について、水素雰囲気中980℃で4時間加熱する焼成熱処理を行った。
この実施形態で、第1実施形態のFePt合金粒子を基本としつつ、原料ミセル溶液を作製する工程で添加するアルカリ土類金属として、カルシウムを適用しFePt合金粒子(実施例4)を製造した。
(a)原料ミセル溶液の作製
24mLの純水に、FeとPtとの合計で0.12Mとなるように、硝酸鉄(Fe(NO3)3・9H2O)と塩化白金酸(H2[PtCl6]・xH2O)を添加した。更に、硝酸カルシウム(Ca(NO3)2・4H2O)を68.01mg(Ca:0.012M)を添加した。アルカリ土類金属であるカルシウムの仕込み量は、金属(Fe、Pt)に対してモル比([A]/[M+PM])で0.1となる。この水溶液に油相となる有機溶媒としてオクタン73.2mLとブタノール14.4mLを添加し、界面活性剤としてCTAB14.08gを添加した。この溶液を均一になるまで90分間攪拌し、原料ミセル溶液を作製した。以上の操作は室温で行っている。この原料ミセル溶液は、FeとPtの比率(Fe:Pt)が、実施例1と同様に5:5である。
14.96mLの純水に中和剤としてアンモニア(25%-NH3水溶液)を9.04mL添加した。この溶液に、オクタン73.2mLとブタノール14.4mLを添加し、更に、CTAB14.08gを添加した。この溶液を均一になるまで90分間攪拌し、中和剤ミセル溶液を作製した。
作製した原料ミセル溶液に、中和剤ミセル溶液を1滴/secで滴下した。中和剤ミセル溶液の添加の際は、混合溶液を攪拌しつつ行い、添加完了後も30分間攪拌した。
上記で作製した混合溶液に、TEOS6.0mLを2滴/secで滴下して添加した。このときSiの添加量([Si])は、原料ミセル溶液中の金属(Fe、Pt)のモル数([M+PM])に対してモル比率9.4となる。添加完了後、混合溶液を攪拌しつつ20時間かけて反応させた。これにより水酸化物粒子表面にシリカが析出して粒子を被覆し、沈殿が生じた。そこで、溶液を遠心分離(3500rpm、5分間)して固形分を回収し、これをメタノールとクロロホルムとの混合液で洗浄して遠心分離し、更にメタノールで洗浄して遠心分離した。得られた固形分について乾燥(大気乾燥後に真空乾燥)して磁性材料の前駆体となる複合水酸化物粒子/シリカのコア/シェル粒子を得た。
前駆体について、水素雰囲気中980℃で4時間加熱する焼成熱処理を行った。
Claims (13)
- 結晶磁気異方性を有する磁性合金粒子と、前記磁性合金粒子を被覆するシリカ担体とからなる磁性材料において、
前記シリカ担体は、アルカリ土類金属化合物を含むものである磁性材料。 - アルカリ土類金属化合物は、Ba、Ca、Srの酸化物、水酸化物、ケイ酸化合物の少なくともいずれかよりなる請求項1記載の磁性材料。
- アルカリ土類金属の合計モル数と、磁性合金粒子を構成する金属の合計モル数との比(アルカリ土類金属/磁性合金粒子)が0.001以上0.8以下である請求項1又は請求項2記載の磁性材料。
- 磁性合金粒子は、FePt合金、CoPt合金、FePd合金、Co3Pt合金、Fe3Pt合金、CoPt3合金、FePt3合金のいずれかよりなる請求項1~請求項3のいずれかに記載の磁性材料。
- 磁性合金粒子はその粒径が1nm以上100nm以下である請求項1~請求項4のいずれかに記載の磁性材料。
- 請求項1~請求項5のいずれかに記載の磁性材料の製造方法であって、
2種以上の金属化合物を含み界面活性剤と結合した水相が油相中で分散する原料ミセル溶液と、中和剤を含み界面活性剤と結合した水相が油相中で分散する中和剤ミセル溶液とを混合することにより、混合液中の水相で複合金属水酸化物粒子を生成する工程と、
前記混合液にケイ素化合物を添加することにより、前記複合金属水酸化物粒子をシリカで被覆して、複合金属水酸化物粒子/シリカからなるコア/シェル粒子を形成する工程と、
前記複合金属水酸化物粒子/シリカからなるコア/シェル粒子を前駆体として焼成熱処理することにより、前記複合金属水酸化物粒子を還元すると共に、結晶構造を規則化して磁性合金粒子を直接的に生成する工程と、
を含み、
更に、前記原料ミセル溶液は、その水相中にアルカリ土類金属塩を含むものである、磁性材料の製造方法。 - 原料ミセル溶液の金属化合物は、FePt合金、CoPt合金、FePd合金、Co3Pt合金、Fe3Pt合金、CoPt3合金、FePt3合金を形成させるための2種以上の金属化合物であり、硝酸鉄、硫酸鉄、塩化鉄、酢酸鉄、鉄アンミン錯体、鉄エチレンジアミン錯体、エチレンジアミン四酢酸鉄、トリス(アセチルアセトナート)鉄、乳酸鉄、シュウ酸鉄、クエン酸鉄、フェロセン及びフェロセンアルデヒド、硝酸コバルト、硫酸コバルト、塩化コバルト、酢酸コバルト、コバルトアンミン錯体、コバルトエチレンジアミン錯体、エチレンジアミン四酢酸コバルト、コバルトアセチルアセトナート錯体、塩化白金酸、酢酸白金、硝酸白金、白金エチレンジアミン錯体、白金トリフェニルホスフィン錯体、白金アンミン錯体及び白金アセチルアセトナート錯体、酢酸パラジウム、硝酸パラジウム、硫酸パラジウム、塩化パラジウム、パラジウムトリフェニルホスフィン錯体、パラジウムアンミン錯体、パラジウムエチレンジアミン錯体及びパラジウムアセチルアセトナート錯体より選択される2種以上の金属化合物である請求項6記載の磁性材料の製造方法。
- 中和剤ミセル溶液の中和剤は、アンモニア、水酸化ナトリウム、水酸化カリウム、水酸化テトラメチルアンモニウムの少なくともいずれかである請求項6又は請求項7記載の磁性材料の製造方法。
- 原料ミセル溶液及び中和剤ミセル溶液の界面活性剤は、臭化セチルトリメチルアンモニウム、塩化セチルトリメチルアンモニウム、オレイン酸カリウム、オレイン酸ナトリウム、塩化セチルピリジウム、塩化ベンズアルコニウム、臭化セチルジメチルエチルアンモニウム、ジ-2-エチルヘキシルスルホコハク酸ナトリウム、コール酸ナトリウム、カプリル酸ナトリウム、ステアリン酸ナトリウム、ラウリル硫酸ナトリウム、ポリオキシエチレンエステル、ポリオキシエチレンエーテル、ポリオキシエチレンソルビタンエステル、ソルビタンエステル、ポリオキシエチレンノニルフェニルエーテル、N-アルキル-N,N-ジメチルアンモニオ-1-プロパンスルホン酸の少なくともいずれかである請求項6~請求項8のいずれかに記載の磁性材料の製造方法。
- ケイ素化合物は、テトラアルコキシシラン、メルカプトアルキルトリアルコキシシラン、アミノアルキルトリアルコキシシラン、3-チオシアナトプロピルトリエトキシシラン、3-グリシジルオキシプロピルトリエトキシシラン、3-イソシアナトプロピルトリエトイシシラン、3-[2-(2-アミノエチルアミノ)エチルアミノ]プロピルトリエトキシシランの少なくともいずれかである請求項6~請求項9のいずれかに記載の磁性材料の製造方法。
- 複合金属水酸化物粒子/シリカからなるコア/シェル粒子の焼成熱処理は、還元雰囲気中、300℃以上1300℃以下で加熱処理するものである請求項6~請求項10のいずれかに記載の磁性材料の製造方法。
- 結晶磁気異方性を有する磁性合金粒子の製造方法であって、
請求項6~請求項11のいずれかに記載の方法により製造した磁性材料をアルカリ溶液でエッチング処理することで、シリカ被覆を除去する方法。 - アルカリ溶液は水酸化ナトリウム水溶液、水酸化テトラメチルアンモニウム水溶液、水酸化カリウムエタノール溶液の少なくともいずれかである請求項12記載の磁性合金粒子の製造方法。
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