CN104889386B - 具有氧化硅壳和金属硅酸盐界面的铁钴三元合金纳米颗粒 - Google Patents
具有氧化硅壳和金属硅酸盐界面的铁钴三元合金纳米颗粒 Download PDFInfo
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- CN104889386B CN104889386B CN201510166097.8A CN201510166097A CN104889386B CN 104889386 B CN104889386 B CN 104889386B CN 201510166097 A CN201510166097 A CN 201510166097A CN 104889386 B CN104889386 B CN 104889386B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052914 metal silicate Inorganic materials 0.000 title claims abstract description 29
- 229910002058 ternary alloy Inorganic materials 0.000 title claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 18
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000011258 core-shell material Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000005291 magnetic effect Effects 0.000 claims description 40
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052720 vanadium Inorganic materials 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 15
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000010941 cobalt Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 229910052723 transition metal Inorganic materials 0.000 claims description 12
- -1 transition metal salt Chemical class 0.000 claims description 12
- 229910017052 cobalt Inorganic materials 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 claims description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 239000011651 chromium Substances 0.000 claims description 10
- 229910052635 ferrosilite Inorganic materials 0.000 claims description 10
- 238000005275 alloying Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000003446 ligand Substances 0.000 claims description 7
- 239000008188 pellet Substances 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 150000003624 transition metals Chemical class 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052987 metal hydride Inorganic materials 0.000 claims description 3
- 150000004681 metal hydrides Chemical group 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 claims description 3
- 229910000326 transition metal silicate Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 125000005270 trialkylamine group Chemical group 0.000 claims description 2
- 239000011162 core material Substances 0.000 description 34
- 239000010410 layer Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000005389 magnetism Effects 0.000 description 6
- 239000000306 component Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000005294 ferromagnetic effect Effects 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 239000006249 magnetic particle Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- SSHPBHBFGZLRRS-UHFFFAOYSA-N [V].[Si](O)(O)(O)O Chemical compound [V].[Si](O)(O)(O)O SSHPBHBFGZLRRS-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 239000008358 core component Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000005307 ferromagnetism Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910001339 C alloy Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 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 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 229910000583 Nd alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910001096 P alloy Inorganic materials 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
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- ABEXMJLMICYACI-UHFFFAOYSA-N [V].[Co].[Fe] Chemical compound [V].[Co].[Fe] ABEXMJLMICYACI-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 125000004848 alkoxyethyl group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- GSOLWAFGMNOBSY-UHFFFAOYSA-N cobalt Chemical compound [Co][Co][Co][Co][Co][Co][Co][Co] GSOLWAFGMNOBSY-UHFFFAOYSA-N 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical group 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 150000004762 orthosilicates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 239000011574 phosphorus Substances 0.000 description 1
- 239000006223 plastic coating Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940124597 therapeutic agent Drugs 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
-
- 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
- H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/005—Impregnating or encapsulating
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biomedical Technology (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
本发明涉及具有氧化硅壳和金属硅酸盐界面的铁钴三元合金纳米颗粒。具体地,提供了一种超顺磁核‑壳纳米颗粒,其具有铁钴三元合金核、该核上的硅氧化物壳和在该核与壳层之间的金属硅酸盐界面层。还提供了制备该纳米颗粒的方法。
Description
相关申请的交叉引用
本申请要求2014年3月5日提交的美国申请号61/948,276的优先权,通过引用以其全文将其公开内容并入本文。
发明背景
发明领域
本发明涉及新型的经涂覆的超顺磁合金纳米颗粒及制备这样的材料的方法。特别地,本发明涉及涂覆氧化硅的铁钴三元合金纳米颗粒,其在金属合金与氧化硅涂层的界面上具有金属硅酸盐层。
背景讨论
铁钴合金常规应用于发动机、发电机和变压器的磁芯构造中。常规地,由磁性合金(典型地为铁-钴-钒或铁-钴铬合金)的层合体结构构造这样的磁芯。这样的层合体结构通常由夹有层间绝缘和粘结剂层的合金金属层构成。这些层间的层对于确保磁芯的高电效率是必要的。
然而,对于发动机、发电机和变压器更高和更有效的性能的日益增长的需求,激励研究新型材料,用该新型材料能构造出具有最大的饱和感应和极少或没有磁滞损耗的紧凑磁芯。
这样的软磁芯部件最重要的特性在于其最大感应、导磁性和芯损耗特性。当磁性材料暴露于快速变化的磁场时,出现由此导致的芯材料的能量损耗。这些芯损耗通常分为两种要素贡献的现象:磁滞和涡流损耗。磁滞损耗源自于克服芯部件中保留的磁力而花费的能量。涡流损耗是由于交流(AC)条件导致的通量改变而在芯部件中产生感应电流引起。
粉末状磁性材料的使用允许制造具有多种多样的形状和尺寸的磁性零件。然而,这些由压实的粉末状磁性材料制得的材料被常规限制于用于涉及直流的应用中。与交流应用不同,直流应用不需要使磁性颗粒彼此绝缘以减少涡流。
常规地,用热塑性材料涂覆磁性颗粒以在颗粒之间起屏障作用,从而减少感应涡流损耗。然而,除了这样的涂层的相对高成本之外,塑料具有的机械强度差,并且因此使用经塑料涂覆的颗粒制得的零件具有相对低的机械强度。此外,许多这些经塑料涂覆的粉末在压制时需要高程度的粘结剂。这导致压制的芯零件密度下降,从而导致导磁性下降和感应降低。此外并且显著地是,这样的塑料涂层通常在150-200℃的温度下降解。因此,经热塑性涂覆的磁性颗粒具有有限的使用。
常规地,铁磁性粉末用于制备软磁芯装置。这样的粉末通常处于以微米测量的尺寸范围,并通过块体材料的机械研磨减小获得。颗粒尺寸小于100nm的超顺磁纳米颗粒材料被发现用于磁记录成像、作为用于医学成像的探针,并应用于治疗剂的定向投放。然而,这些使用通常限于超顺磁氧化铁纳米颗粒,并且极少涉及尝试开发适合用于制备芯磁性零件的铁-钴三元合金钠米颗粒。
Brunner(US7532099)描述了经涂覆的合金颗粒,其与铁磁性合金粉末和热塑性或硬塑料聚合物用于制备注射成型或铸造的软磁芯。对铁、铜、铌、硅和硼的合金进行热处理以形成纳米晶结构,然后在磨机中粉碎以获得约0.01-1.0mm尺度的颗粒。将150-400nm的铁和硅氧化物的耐磨层涂覆在这些颗粒上。
Anand等人(US6808807)描述了包封的铁磁性粉末,其通过用聚有机硅氧烷或聚有机硅烷涂覆铁磁性核、并热处理经涂覆的核以将聚合物转化为含有硅和氧的残留物而获得。该核合金可以是任何与硅、铝、镍、钴、硼、磷、锆、钕和碳合金化的铁。平均直径小于2mm的铁磁性核颗粒适于这种组合物。
Gay等人(US6193903)描述了经陶瓷涂覆的铁磁性粉末。该粉末为铁或铁合金,并且颗粒上的包封层可以是陶瓷组中的一种,例如金属氧化物、金属氮化物、金属硅酸盐和金属磷酸盐。颗粒尺寸为5-1000微米。将氧化硅列为适合作为涂层的一大组陶瓷材料中的一种。
Moorhead等人(US6051324)描述了颗粒尺寸小于44微米的铁/钴/钒的合金颗粒,其涂覆有玻璃、陶瓷或陶瓷玻璃,包括二氧化硅。
Atarashi等人(US5763085)描述了在其表面上具有多层的磁性颗粒,其作为彩色磁性材料例如磁性调色剂的起始材料是有用的。这些颗粒的尺寸为0.01-200μm。二氧化硅描述为金属氧化物涂层连同通过溶胶凝胶法制备。提供对通过在络合剂存在下还原可溶性金属盐来制备颗粒上的金属层的描述。
Yamanaka等人(US4983231)描述了经表面处理的磁性粉末,其通过用碱改性的氧化硅颗粒对铁-稀土金属合金进行处理而获得。合金颗粒的平均颗粒直径为20-200μm。在加热时,碱硅酸盐脱水并浓缩,以形成“聚硅氧烷”涂层。
Uozumi等人(JP2007-123703)描述了将硅酸盐涂层施加到包括铁、钴和钒的合金的软磁性粉末,该粉末的平均颗粒尺寸为70微米。对经涂覆的颗粒进行热处理,导致Si和O迁移到软磁性核中,以在外氧化物层与软磁性核之间形成扩散区。
Yamada等人(JP03-153838)(摘要)描述了用含有硅和烷氧基的化合物(例如乙烯基三乙氧基硅烷)对铁/钴/钒粉末进行表面处理。没有提供颗粒尺寸或制备合金颗粒的方法的描述。
Sun等人(J.Am.Chem.Soc.,2002,124,8204-8205)描述了制备单分散磁铁矿纳米颗粒的方法,该纳米颗粒可用作生长尺寸为至多20nm的较大纳米颗粒的晶种。
Bumb等人(Nanotechnology,19,2008,335601)描述了10-40nm的超顺磁氧化铁纳米颗粒的合成,该氧化铁纳米颗粒包封在约2nm的氧化硅涂覆层中。提及在电源变压器中的使用,但没有提供芯结构的制备的描述。
Zhang等人(Nanotechnology,19,2008,085601)描述了经氧化硅涂覆的氧化铁颗粒的合成。该待涂覆的氧化铁颗粒的平均尺寸为8-10nm,氧化硅核为约2nm。
Hattori等人(US2006/0283290)描述了平均颗粒直径为5-25nm的经氧化硅涂覆的氮化的铁颗粒。这些颗粒为“基本上球形”,并且对于磁性层例如磁性记录介质为有用的。
Yu等人(J.Phys.Chem.C 2009.113,537-543)描述了包封在氧化硅壳中的磁性氧化铁纳米颗粒的制备。研究了这些颗粒作为蛋白质的磁性粘合剂的使用。
因此,需要新型的磁性粉末来制备软磁零件,其提供提高的生坯强度、高温耐受性和良好的机械性质,并且其零件具有最小或基本没有芯损耗。
该研究之前的成果在2012年7月26日提交的在先美国申请号13/558,397中进行了描述,通过引用以其全文将其公开内容并入本文。对于磁芯的应用在2012年8月2日提交的在先美国申请号13/565,250中进行了描述,通过引用以其全文将其公开内容并入本文。
然而,仍然需要新型和/或改进的磁性粉末来制备软磁零件,其提供提高的生坯强度、高温耐受性和良好的机械性质,并且其零件具有最小或基本没有芯损耗。
因此,本发明的目的在于提供一种超顺磁粉末,其具有适于制备软磁零件的可调磁性质,同时具有用于制备高性能磁芯的提高的生坯强度、高温耐受性和良好的机械性质。
本发明的第二个目的在于提供一种制备这样的超顺磁粉末的粉末纳米颗粒的方法。
发明概述
申请人继续致力于研究对制备磁芯有用的材料,该磁芯具有对于制备未来高性能发动机、发电机和变压器所需的性质。通过两步化学合成制备了一系列核-壳FeCoV/SiO2纳米颗粒。由X射线光电子能谱学确定该FeCoV核和金属硅酸盐界面相。这些金属硅酸盐相的存在导致磁各向异性(即矫顽力)的显著增高。这一效果可随着SiO2壳更厚而增强,这导致更多金属硅酸盐的形成。控制该磁性活性或磁致旋光的(magnetically active)金属硅酸盐界面层金属硅酸盐界面层的结构和尺寸对于这些材料的使用可以允许调整磁性质。
因此,根据本发明实现了上述和其它目的,其第一实施方案提供了核-壳纳米颗粒,包含:
铁钴三元合金的核;
涂覆该核的硅氧化物壳;和
在该核与壳之间的区域中的金属硅酸盐界面;其中
该三元合金的第三组分为选自钪、钛、钒、铬、锰、镍、铜和锌的过渡金属,该纳米颗粒的颗粒尺寸为2-200nm,并且该金属硅酸盐界面的金属硅酸盐包含硅酸铁、硅酸钴和该第三组分过渡金属硅酸盐中的至少一种。
在根据本发明的一个优选实施方案中,该金属硅酸盐界面为磁性活性或磁致旋光的。
在根据本发明的另一优选实施方案中,该金属硅酸盐界面包含硅酸铁、硅酸钴和硅酸钒。
在又一优选实施方案中,该核-壳纳米颗粒的界面区域的宽度为0.1-10nm。
在又一实施方案中,本发明提供了制备根据第一实施方案的核壳纳米颗粒的方法,包括:
将铁盐、钴盐和过渡金属盐各自溶解于碱性醇溶液,以获得铁盐、钴盐和除了铁和钴以外的过渡金属盐的溶液;用还原剂处理该溶液以制备铁钴三元合金的纳米颗粒;用硅氧化物壳涂覆合金颗粒以获得核壳纳米颗粒;以及分离并干燥所制备的核-壳纳米颗粒。
通过一般介绍提供了前述段落,但其并不旨在限制以下权利要求的范围。参照结合附图的以下详细描述将会最好地理解目前的优选实施方案连同进一步的优点。
附图简要描述
图1示出了在实施例中制备的核-壳纳米颗粒的TEM图像。
图2示出了在实施例中制备的核-壳纳米颗粒的XPS能谱,其示出了硅酸钒的细节。
图3示出了在实施例中制备的核-壳纳米颗粒的XPS能谱,其示出了硅酸铁的细节。
图4示出了在实施例中制备的核-壳纳米颗粒的XPS能谱,其示出了硅酸钴的细节。
发明详述
在整个说明书中所描述的所有范围包括其中的所有值及其子范围,除非另有说明。
如本文中使用的,词语“一个(a)”和“一个(an)”等带有“一个或多个”的含义。词组“选自由...组成的组”、“选自”等包括特定材料的混合物。术语“包含”等为意指“包括至少”的开放性术语,除非另有特别说明。
发明人认识到,为了增加由芯损耗测量的磁芯效率,磁芯必须展示减少量度的磁滞以及降低的涡流形成。虽然不受理论限制,但据认为将晶粒尺寸控制到与颗粒磁畴的晶粒尺寸相似是有助于磁芯降低的滞后的因素。此外,如本文中发现和报告的那样,在绝缘氧化硅壳与核晶粒的界面上的磁性活性或磁致旋光的金属硅酸盐层的存在显著影响核-壳纳米颗粒的整体磁性质,导致磁各向异性(即矫顽力)的显著增加。控制SiO2壳厚度允许控制金属硅酸盐层的厚度。然后,可以通过制备具有不同壳厚度的核-壳纳米颗粒而在限度内调整磁性质。
因此,本发明的第一实施方案为核-壳纳米颗粒,包含:铁钴三元合金的核;涂覆该核的硅氧化物壳;和在该核与壳之间的区域中的金属硅酸盐界面。该三元合金的第三组分为选自钪、钛、钒、铬、锰、镍、铜和锌的过渡金属。在优选实施方案中,该第三合金组分可以是钒或钴,并且最优选该第三合金组分为钒。纳米颗粒的整体尺寸可以为1-200nm,优选2-160nm,最优选为3-30nm。
该金属硅酸盐界面的金属硅酸盐包含硅酸铁、硅酸钴和该第三组分过渡金属硅酸盐中的至少一种,更优选地该界面包含硅酸铁和硅酸钴,并且最优选地该界面包含硅酸铁、硅酸钴和该三元金属的硅酸盐。在非常优选的实施方案中,该合金的三元金属为钒或钴,且该金属硅酸盐层包含硅酸钒或硅酸钴。
该界面层的金属硅酸盐为磁性活性或磁致旋光的,且该界面层的宽度取决于氧化硅壳涂层的宽度。
该界面区域的宽度为0.1-10nm,优选0.1-5nm。然而,如上所述,其它宽度对于获得具有特定目标性质的核-壳纳米颗粒可为优选的。
根据本发明,合金组成没有限制,并且可以采用任何常规已知的组成。通常,三元组分可以构成0.1-5%摩尔浓度的合金纳米颗粒。
在优选实施方案中,该三元合金由铁钴和钒构成,并且钒含量为2%摩尔浓度或更低。
在另一优选实施方案中,该三元合金为铁钴铬合金,并且铬含量为1%摩尔浓度或更低。
硅氧化物壳直接涂覆到合金纳米颗粒上并可以为任何合适的宽度。在非常优选的实施方案中,该壳的硅氧化物为二氧化硅。
根据本发明的三元合金核壳纳米颗粒可以通过如下方法制备,包括:
在配体存在下将铁盐、钴盐和除了铁和钴以外的过渡金属盐各自溶解于碱性醇溶液,以获得金属盐的溶液;
用还原剂处理该溶液以制备铁钴三元合金的纳米颗粒;
用硅氧化物壳涂覆该合金颗粒以获得核壳纳米颗粒,并且分离和干燥所制备的核-壳纳米颗粒。
在优选实施方案中,该还原剂为金属氢化物,最优选为硼氢化钠。
该合金纳米颗粒可以直接用半导体材料或非导体材料涂覆;优选硅氧化物壳:通过在三烷基胺水溶液中分散该合金纳米颗粒;向该分散液添加原硅酸四烷基酯;以及使该原硅酸酯反应以在该纳米颗粒上形成硅氧化物涂层。
不限制所采用的铁、钴和过渡金属盐,只要它们可溶于碱性醇溶剂。除了铁和钴以外的过渡金属选自钪、钛、钒、铬、锰、镍、铜和锌。盐可优选为卤化物,更优选为氯化物。
在非常优选的实施方案中,除了铁和钴以外的过渡金属为钒或铬,并且采用钒或铬的卤化物盐作为金属源。
碱性醇溶液包含选自甲醇、乙醇、正丙醇、2-丙醇、正丁醇和2-丁醇中的至少一种醇。在优选实施方案中,该醇为乙醇。
可以采用对于与金属纳米颗粒表面配合为有效的任何配体。在优选实施方案中,柠檬酸钠为络合剂,优选为柠檬酸三钠。在另一个实施方案中,采用了四烷基卤化铵配体,优选该四烷基卤化物铵配体为四丁基氯化铵或四辛基溴化铵。
可以利用能够将金属离子还原成金属态的任何还原剂。在优选实施方案中,该还原剂为硼氢化钠。
已经整体上描述了本发明,可以参照一些特定实施例获得进一步的理解,这些特定实施例仅用于说明目的而提供,而不是进行限制,除非另外指明。
本发明的额外优点和其它特征将部分在接下来的描述中得到阐述,并且部分在审阅以下内容时对于本领域普通技术人员来说将变得清楚或者可以通过实践本发明而获悉。可以如所附权利要求特别指出的那样实现和获得本发明的优点。如将认识到的,本发明能够具有其它和不同的实施方案,并且其多个细节能够在各种显而易见的方面具有改变而均不脱离本发明。在此方面,本文中的描述应该理解为本质上为说明性而非限制性的。
实施例
向1L的五口圆底烧瓶中添加105mL乙醇、0.043g NaOH、1.201g四辛基溴化铵、2.100g四水合二氯化铁、2.401g六水合二氯化钴和0.0763g三氯化钒。搅拌该混合物直至完全溶解。在冰浴中并置于氩惰性气氛中冷却该反应物。然后,缓慢地添加溶解于90mL乙醇中的2.4448g硼氢化钠的溶液。在添加全部硼氢化钠溶液后又搅拌该反应物10分钟。然后用水与乙醇的70/30的混合物洗涤所得的浆料四次(每次洗涤200mL)。向反应烧杯中添加处于126mL水中的3.3mL三乙胺溶液。将所得的混合物搅拌另外10分钟,以分散Fe49%Co49%V2%纳米颗粒。然后,添加处于78mL乙醇中的0.3mL原硅酸四乙酯,并使其反应另外10分钟。用200mL乙醇最后洗涤3次。然后,分离和干燥经氧化硅涂覆的纳米颗粒。
然后,用X射线光电子能谱学分析干燥的核-壳颗粒,并且如图2、3和4所示,确定了在FeCoV/SiO2纳米颗粒中存在金属硅酸盐。
Claims (19)
1.一种核壳纳米颗粒,包含:
铁钴三元合金的核;
涂覆该核的硅氧化物壳;和
在该核与壳之间的区域中的金属硅酸盐界面;
其中
该三元合金的第三组分为选自钪、钛、钒、铬、锰、镍、铜和锌的过渡金属,
该纳米颗粒的颗粒尺寸为2-200nm,且
该金属硅酸盐界面的金属硅酸盐包含硅酸铁、硅酸钴和该第三组分过渡金属硅酸盐中的至少一种。
2.如权利要求1所述的核壳纳米颗粒,其中该金属硅酸盐界面为磁性活性或磁致旋光的(magnetically active)。
3.如权利要求1所述的核壳纳米颗粒,其中该金属硅酸盐界面包含硅酸铁和硅酸钴。
4.如权利要求1所述的核壳纳米颗粒,其中界面区域的宽度为0.1-10nm。
5.如权利要求1所述的核壳纳米颗粒,其中该铁钴三元合金为铁钴钒合金。
6.如权利要求5所述的核壳纳米颗粒,其中该金属硅酸盐界面包含硅酸铁、硅酸钴和硅酸钒。
7.如权利要求1所述的核壳纳米颗粒,其中该铁钴三元合金为铁钴铬合金。
8.如权利要求7所述的核壳纳米颗粒,其中该金属硅酸盐界面包含硅酸铁、硅酸钴和硅酸铬。
9.如权利要求1所述的核壳纳米颗粒,其中该壳的硅氧化物为二氧化硅。
10.如权利要求1所述的核壳纳米颗粒,其中该纳米颗粒的颗粒尺寸为2-160nm。
11.一种制备如权利要求1所述核壳纳米颗粒的方法,该方法包括:
在配体存在下将铁盐、钴盐和过渡金属盐各自溶解于碱性醇溶液;
在惰性气氛下用还原剂处理该溶液以制备铁钴三元合金的纳米颗粒;
用硅氧化物壳涂覆该合金颗粒以获得核壳纳米颗粒;
分离和干燥所获得的核壳纳米颗粒。
12.如权利要求11所述的方法,其中该还原剂为金属氢化物。
13.如权利要求12所述的方法,其中该金属氢化物为硼氢化钠。
14.如权利要求11所述的方法,其中涂覆该合金颗粒包括:
在三烷基胺的水溶液中分散该合金纳米颗粒;
向分散液中添加原硅酸四烷基酯;以及
使原硅酸酯反应以在纳米颗粒上形成硅氧化物涂层。
15.如权利要求11所述的方法,其中除了铁和钴以外的该过渡金属选自钪、钛、钒、铬、锰、镍、铜和锌。
16.如权利要求15所述的方法,其中该过渡金属为钒或铬。
17.如权利要求11所述的方法,其中该碱性醇溶液包含选自甲醇、乙醇、正丙醇、2-丙醇、正丁醇和2-丁醇中的至少一种。
18.如权利要求11所述的方法,其中该配体为四烷基卤化铵。
19.如权利要求11所述的方法,其中该配体为四辛基溴化铵。
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