JP4993276B2 - Alloy nanocrystal, method for producing alloy nanocrystal, and alloy nanocrystal dispersion - Google Patents
Alloy nanocrystal, method for producing alloy nanocrystal, and alloy nanocrystal dispersion Download PDFInfo
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- JP4993276B2 JP4993276B2 JP2006355245A JP2006355245A JP4993276B2 JP 4993276 B2 JP4993276 B2 JP 4993276B2 JP 2006355245 A JP2006355245 A JP 2006355245A JP 2006355245 A JP2006355245 A JP 2006355245A JP 4993276 B2 JP4993276 B2 JP 4993276B2
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- 239000002159 nanocrystal Substances 0.000 title claims description 184
- 239000000956 alloy Substances 0.000 title claims description 114
- 229910045601 alloy Inorganic materials 0.000 title claims description 114
- 239000006185 dispersion Substances 0.000 title claims description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 30
- -1 alkyl monocarboxylic acid Chemical class 0.000 claims description 38
- 125000004432 carbon atom Chemical group C* 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 31
- 239000002904 solvent Substances 0.000 claims description 31
- 229910052723 transition metal Inorganic materials 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 27
- 229910000510 noble metal Inorganic materials 0.000 claims description 24
- 150000003839 salts Chemical class 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 17
- 125000000217 alkyl group Chemical group 0.000 claims description 14
- 229910052763 palladium Inorganic materials 0.000 claims description 13
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 13
- 239000003638 chemical reducing agent Substances 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 11
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 10
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical class NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 4
- 150000007942 carboxylates Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 claims description 4
- 229910000103 lithium hydride Inorganic materials 0.000 claims description 4
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 4
- 239000012312 sodium hydride Substances 0.000 claims description 4
- RRKODOZNUZCUBN-CCAGOZQPSA-N (1z,3z)-cycloocta-1,3-diene Chemical class C1CC\C=C/C=C\C1 RRKODOZNUZCUBN-CCAGOZQPSA-N 0.000 claims description 3
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 150000003003 phosphines Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 45
- 229910005335 FePt Inorganic materials 0.000 description 39
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 27
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 27
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000013078 crystal Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 20
- 239000012298 atmosphere Substances 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 235000021355 Stearic acid Nutrition 0.000 description 17
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 17
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 17
- 239000008117 stearic acid Substances 0.000 description 17
- 239000007789 gas Substances 0.000 description 16
- 239000002244 precipitate Substances 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 13
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 12
- VEJOYRPGKZZTJW-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;platinum Chemical compound [Pt].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O VEJOYRPGKZZTJW-FDGPNNRMSA-N 0.000 description 11
- FRVCGRDGKAINSV-UHFFFAOYSA-L iron(2+);octadecanoate Chemical compound [Fe+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O FRVCGRDGKAINSV-UHFFFAOYSA-L 0.000 description 11
- 229910018979 CoPt Inorganic materials 0.000 description 10
- 229910015187 FePd Inorganic materials 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- BTOOAFQCTJZDRC-UHFFFAOYSA-N 1,2-hexadecanediol Chemical compound CCCCCCCCCCCCCCC(O)CO BTOOAFQCTJZDRC-UHFFFAOYSA-N 0.000 description 9
- 229910018936 CoPd Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 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 description 9
- 239000002253 acid Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 8
- 230000007704 transition Effects 0.000 description 8
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 5
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 5
- 239000005642 Oleic acid Substances 0.000 description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 5
- 238000000015 thermotherapy Methods 0.000 description 5
- AMFIJXSMYBKJQV-UHFFFAOYSA-L cobalt(2+);octadecanoate Chemical compound [Co+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AMFIJXSMYBKJQV-UHFFFAOYSA-L 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 4
- ISYWECDDZWTKFF-UHFFFAOYSA-N nonadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(O)=O ISYWECDDZWTKFF-UHFFFAOYSA-N 0.000 description 4
- 229910052787 antimony Inorganic materials 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 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 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 235000003441 saturated fatty acids Nutrition 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 125000002960 margaryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 2
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 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 description 1
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
- 229910002836 PtFe Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 125000005595 acetylacetonate group Chemical group 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- USJRLGNYCQWLPF-UHFFFAOYSA-N chlorophosphane Chemical class ClP USJRLGNYCQWLPF-UHFFFAOYSA-N 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
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- XSWSEQPWKOWORN-UHFFFAOYSA-N dodecan-2-ol Chemical compound CCCCCCCCCCC(C)O XSWSEQPWKOWORN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical class N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- LXNAVEXFUKBNMK-UHFFFAOYSA-N palladium(II) acetate Substances [Pd].CC(O)=O.CC(O)=O LXNAVEXFUKBNMK-UHFFFAOYSA-N 0.000 description 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- XAFJSPPHVXDRIE-UHFFFAOYSA-L platinum(2+);triphenylphosphane;dichloride Chemical compound [Cl-].[Cl-].[Pt+2].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 XAFJSPPHVXDRIE-UHFFFAOYSA-L 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- ISPSHPOFLYFIRR-UHFFFAOYSA-N trihexylsilicon Chemical compound CCCCCC[Si](CCCCCC)CCCCCC ISPSHPOFLYFIRR-UHFFFAOYSA-N 0.000 description 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical class C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
本発明は、合金ナノ結晶、合金ナノ結晶の製造方法および合金ナノ結晶分散液に関する。
さらに詳しくは、本発明は、基板上に配列したときに、高密度磁気記録媒体、磁気抵抗効果素子、燃料電池の電極用の触媒または磁気温熱療法用の発熱体等として好適に使用し得る合金ナノ結晶、該合金ナノ結晶を効率よく製造する方法および上記合金ナノ結晶を有する分散液に関する。
The present invention relates to an alloy nanocrystal, a method for producing the alloy nanocrystal, and an alloy nanocrystal dispersion.
More specifically, the present invention relates to an alloy that can be suitably used as a high-density magnetic recording medium, a magnetoresistive effect element, a catalyst for a fuel cell electrode or a heating element for magnetic thermotherapy when arranged on a substrate. The present invention relates to a nanocrystal, a method for efficiently producing the alloy nanocrystal, and a dispersion having the alloy nanocrystal.
ＦｅＰｔ、ＦｅＰｄおよびＣｏＰｔ等の合金結晶からなる磁性材料は、ｆａｃｅ−ｃｅｎｔｅｒｅｄ ｔｅｔｒａｇｏｎａｌ(ｆｃｔ)相において大きな結晶磁気異方性を示し、粒子径が１０ｎｍ以下の合金ナノ結晶であっても磁気記録情報を安定に維持できるので、高密度磁気記録材料として注目されている。 Magnetic materials composed of alloy crystals such as FePt, FePd, and CoPt exhibit large crystal magnetic anisotropy in the face-centered tetragonal (fct) phase, and magnetic recording information can be obtained even for alloy nanocrystals having a particle size of 10 nm or less. It is attracting attention as a high-density magnetic recording material because it can be stably maintained.
近年、上記合金ナノ結晶の製造例として、白金アセチルアセトナト（Ｐｔ（ａｃａｃ）２）および鉄アセチルアセトナト（Ｆｅ（ａｃａｃ）３）を、窒素雰囲気下、オレイン酸とオレイルアミンの混合液中で還元することにより、表面がオレイン酸やオレイルアミンで覆われたＰｔＦｅ合金ナノ結晶を製造した例が報告されるに至っている（非特許文献１参照）。 In recent years, platinum acetylacetonate (Pt (acac) 2 ) and iron acetylacetonate (Fe (acac) 3 ) are reduced in a mixed solution of oleic acid and oleylamine under a nitrogen atmosphere as an example of producing the above-mentioned alloy nanocrystal. As a result, an example of producing a PtFe alloy nanocrystal whose surface is covered with oleic acid or oleylamine has been reported (see Non-Patent Document 1).
この合金ナノ結晶は、表面がオレイン酸やオレイルアミンといった有機分子で覆われているため、有機溶媒中に容易に単分散させることができ、また、その結晶構造は、通常ｆａｃｅ−ｃｅｎｔｅｒｅｄ ｃｕｂｉｃ（ｆｃｃ）相であるため、５５０℃〜７００℃で熱処理することによってｆｃｔ相に相転移させることができる。 Since the surface of this alloy nanocrystal is covered with organic molecules such as oleic acid and oleylamine, it can be easily monodispersed in an organic solvent, and its crystal structure is usually face-centered cubic (fcc). Since it is a phase, it can be transformed into the fct phase by heat treatment at 550 ° C. to 700 ° C.
しかしながら、上記合金ナノ結晶を製造する場合、原料であるＦｅ（ａｃａｃ）３を構成するＦｅ３＋が還元されにくいため、強力な還元剤（例えば水素化ホウ素ナトリウム）を用いたり、Ｐｔに対してＦｅが過剰になるように原料を加える必要があり、このため、原料コストが高くなるとともに、単離精製処理が煩雑になってしまう。 However, when producing the above alloy nanocrystals, Fe 3+ constituting Fe (acac) 3 as a raw material is difficult to be reduced. Therefore, a strong reducing agent (for example, sodium borohydride) is used, or Fe is used against Pt. Therefore, it is necessary to add the raw material so as to be excessive, which increases the raw material cost and makes the isolation and purification process complicated.
また、上記合金ナノ結晶は、表面が炭素−炭素二重結合（不飽和結合）を持つオレイン酸とオレイルアミンで覆われているため、空気酸化を受けやすいという課題や、オレイン酸やオレイルアミンの重合により合金ナノ結晶同士が凝集し、有機溶媒中に安定して分散させることができなくなるという課題を有している。 In addition, the above-mentioned alloy nanocrystals are covered with oleic acid and oleylamine having a carbon-carbon double bond (unsaturated bond), so that they are susceptible to air oxidation and polymerization of oleic acid and oleylamine. There is a problem that alloy nanocrystals aggregate and cannot be dispersed stably in an organic solvent.
一方、原料である鉄の供給源として、鉄ペンタカルボニル（Ｆｅ（ＣＯ）５）を用いたり（非特許文献２参照）、塩化第一鉄（ＦｅＣｌ２）を用いる（非特許文献３参照）製造法も報告されている。 On the other hand, iron pentacarbonyl (Fe (CO) 5 ) is used as a source of iron as a raw material (see Non-Patent Document 2) or ferrous chloride (FeCl 2 ) is used (see Non-Patent Document 3) Laws have also been reported.
しかし、Ｆｅ（ＣＯ）５は、毒性が強く引火性の液体であり、また反応の過程で有害な一酸化炭素が発生するので、安全性および環境保全の観点から使用するのは好ましくなく、さらに、揮発性が高いので反応中に揮発してしまい得られる合金ナノ粒子の組成がばらつき易い。一方、ＦｅＣｌ２の場合は吸湿性があり、空気酸化を受けやすいので取り扱いが容易でないという課題を有している。
本発明は、このような事情のもとで、製造コストを低減しつつ容易かつ効率よく製造することができ、溶媒中に容易かつ長期間安定して分散可能で、基板上に配列したときに、高密度磁気記録媒体、磁気抵抗効果素子、燃料電池の電極用の触媒または磁気温熱療法用の発熱体等として好適に使用し得る新規合金ナノ結晶を提供することを第１の目的とする。また、本発明は、上記合金ナノ結晶を製造する方法および上記合金ナノ結晶の分散液を提供することを第２および第３の目的とする。 Under such circumstances, the present invention can be easily and efficiently manufactured while reducing the manufacturing cost, and can be easily and stably dispersed in a solvent for a long period of time when arranged on a substrate. It is a first object to provide a novel alloy nanocrystal that can be suitably used as a high-density magnetic recording medium, a magnetoresistive effect element, a catalyst for a fuel cell electrode, a heating element for magnetic thermotherapy, or the like. The second and third objects of the present invention are to provide a method for producing the alloy nanocrystal and a dispersion of the alloy nanocrystal.
本発明者が鋭意検討したところ、ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素とを含むコア部と、該コア部の表面に付着した長鎖飽和脂肪酸とを有する合金ナノ結晶により、上記第１の目的を達成し得ることを見出した。 As a result of intensive studies by the present inventors, a core part including at least one transition metal element selected from Fe and Co and at least one noble metal element selected from Pt and Pd is attached to the surface of the core part. It has been found that the first object can be achieved by an alloy nanocrystal having a long-chain saturated fatty acid.
また、上記第２の目的は、ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素を含む長鎖飽和脂肪酸塩と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体とを、溶媒中、還元剤の存在下に加熱することを特徴とする合金ナノ結晶の製造方法により達成し得ることを見出した。 The second object is to provide a long-chain saturated fatty acid salt containing at least one transition metal element selected from Fe and Co, and a salt or complex of at least one noble metal element selected from Pt and Pd. It has been found that this can be achieved by a method for producing alloy nanocrystals characterized by heating in a solvent in the presence of a reducing agent.
また、上記第３の目的は、上記合金ナノ結晶が、該合金ナノ結晶と反応しない溶媒中に分散していることを特徴とする合金ナノ結晶分散液により達成し得ることを見出した。 Moreover, it has been found that the third object can be achieved by an alloy nanocrystal dispersion liquid in which the alloy nanocrystals are dispersed in a solvent that does not react with the alloy nanocrystals.
すなわち、本発明は、
（１）ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素とを含むコア部と、該コア部の表面に付着した長鎖飽和脂肪酸とを有することを特徴とする合金ナノ結晶、
（２）前記遷移金属元素および貴金属元素の合計含有量に対する前記遷移金属元素の合計含有量の比がモル比で０．４以上０．７以下である上記（１）に記載の合金ナノ結晶、
（３）前記コア部が粒子形状を有し、その平均粒径が１ｎｍ以上１５ｎｍ以下である上記（１）または（２）に記載の合金ナノ結晶、
（４）前記長鎖飽和脂肪酸が、アルキル基の炭素数が７〜２３のアルキルモノカルボン酸である上記（１）〜（３）のいずれかに記載の合金ナノ結晶、
（５）上記（１）〜（４）のいずれかに記載の合金ナノ結晶を製造する方法であって、
ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素を含む長鎖飽和脂肪酸塩と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体とを、溶媒中、還元剤の存在下に加熱することを特徴とする合金ナノ結晶の製造方法、
（６）前記遷移金属元素を含む長鎖飽和脂肪酸塩が、アルキル基の炭素数が７〜２３のアルキルモノカルボン酸の塩である上記（５）に記載の合金ナノ結晶の製造方法、
（７）前記貴金属元素の塩または錯体が、ハロゲン化物、カルボン酸塩、硝酸塩、β−ジケトナト錯体、エチレンジアミン錯体、アンミン錯体、ホスフィン錯体、ニトリル錯体、π−アリル錯体およびシクロオクタジエン錯体から選ばれる少なくとも１種の塩または錯体である上記（５）または（６）に記載の合金ナノ結晶の製造方法、
（８）前記溶媒が、前記遷移金属元素を含む長鎖飽和脂肪酸塩および前記貴金属元素の塩または錯体と反応しないものである上記（５）〜（７）のいずれかに記載の合金ナノ結晶の製造方法、
（９）前記溶媒が、２００〜４００℃の範囲の沸点を有するものである前記（５）〜（８）のいずれかに記載の合金ナノ結晶の製造方法、
（１０）前記還元剤が、炭素数が８〜２４のアルコール、炭素数が８〜２４のホスフィン
、水素化ホウ素化合物、シラン化合物、水素化リチウム、水素化ナトリウムおよびヒドラジンから選ばれる少なくとも１種である上記（５）〜（９）のいずれかに記載の合金ナノ結晶の製造方法、
（１１）上記（１）〜（４）のいずれかに記載の合金ナノ結晶が、該合金ナノ結晶と反応しない溶媒中に分散していることを特徴とする合金ナノ結晶分散液、
（１２）前記溶媒が、前記合金ナノ結晶を単分散し得るものである上記（１１）に記載の合金ナノ結晶分散液、および
（１３）前記溶媒が、炭素数が６〜１２の芳香族炭化水素、炭素数が１〜３の塩素化炭化水素、炭素数が５〜１８の飽和炭化水素および炭素数が４〜１８のエーテルから選ばれる少なくとも１種を５０容量％以上含むものである上記（１１）または（１２）に記載の合金ナノ結晶分散液
を提供するものである。
That is, the present invention
(1) a core portion including at least one transition metal element selected from Fe and Co, and at least one noble metal element selected from Pt and Pd, and a long-chain saturated fatty acid attached to the surface of the core portion Alloy nanocrystals characterized by having,
(2) The alloy nanocrystal according to (1), wherein the ratio of the total content of the transition metal element to the total content of the transition metal element and the noble metal element is 0.4 to 0.7 in terms of molar ratio,
(3) The alloy nanocrystal according to (1) or (2), wherein the core portion has a particle shape, and an average particle diameter thereof is 1 nm or more and 15 nm or less,
(4) The alloy nanocrystal according to any one of (1) to (3), wherein the long-chain saturated fatty acid is an alkyl monocarboxylic acid having 7 to 23 carbon atoms in the alkyl group,
(5) A method for producing the alloy nanocrystal according to any one of (1) to (4) above,
A long-chain saturated fatty acid salt containing at least one transition metal element selected from Fe and Co and a salt or complex of at least one noble metal element selected from Pt and Pd in a solvent in the presence of a reducing agent A method for producing an alloy nanocrystal, characterized by heating,
(6) The method for producing an alloy nanocrystal according to (5), wherein the long-chain saturated fatty acid salt containing the transition metal element is a salt of an alkyl monocarboxylic acid having 7 to 23 carbon atoms in the alkyl group,
(7) The salt or complex of the noble metal element is selected from a halide, carboxylate, nitrate, β-diketonato complex, ethylenediamine complex, ammine complex, phosphine complex, nitrile complex, π-allyl complex, and cyclooctadiene complex. The method for producing alloy nanocrystals according to (5) or (6) above, which is at least one salt or complex,
(8) The alloy nanocrystal according to any one of (5) to (7), wherein the solvent does not react with a long-chain saturated fatty acid salt containing the transition metal element and a salt or complex of the noble metal element. Production method,
(9) The method for producing an alloy nanocrystal according to any one of (5) to (8), wherein the solvent has a boiling point in a range of 200 to 400 ° C.
(10) The reducing agent is at least one selected from alcohol having 8 to 24 carbon atoms, phosphine having 8 to 24 carbon atoms, borohydride compound, silane compound, lithium hydride, sodium hydride and hydrazine. A method for producing an alloy nanocrystal according to any one of the above (5) to (9),
(11) An alloy nanocrystal dispersion, wherein the alloy nanocrystal according to any one of (1) to (4) is dispersed in a solvent that does not react with the alloy nanocrystal,
(12) The alloy nanocrystal dispersion liquid according to (11), wherein the solvent is capable of monodispersing the alloy nanocrystals, and (13) the aromatic carbonization having 6 to 12 carbon atoms. The above (11), containing at least 50% by volume of hydrogen, chlorinated hydrocarbons having 1 to 3 carbon atoms, saturated hydrocarbons having 5 to 18 carbon atoms, and ethers having 4 to 18 carbon atoms Or the alloy nanocrystal dispersion liquid as described in (12) is provided.
本発明によれば、製造コストを低減しつつ容易かつ効率よく製造することができ、溶媒中に容易かつ長期間安定して分散可能で、基板上に配列したときに、高密度磁気記録媒体、磁気抵抗効果素子、燃料電池の電極用の触媒または磁気温熱療法用の発熱体等として好適に使用し得る新規合金ナノ結晶を提供することができる。また、本発明によれば、上記合金ナノ結晶を製造する方法および上記合金ナノ結晶の分散液を提供することができる。 According to the present invention, the high-density magnetic recording medium can be easily and efficiently manufactured while reducing the manufacturing cost, can be easily and stably dispersed in a solvent for a long period of time, and is arranged on a substrate. It is possible to provide a novel alloy nanocrystal that can be suitably used as a magnetoresistive element, a catalyst for an electrode of a fuel cell, a heating element for magnetic thermotherapy, or the like. Moreover, according to this invention, the manufacturing method of the said alloy nanocrystal and the dispersion liquid of the said alloy nanocrystal can be provided.
先ず、本発明の合金ナノ結晶について説明する。
本発明の合金ナノ結晶は、ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素とを含むコア部と、該コア部の表面に付着した長鎖飽和脂肪酸とを有することを特徴とする。
First, the alloy nanocrystal of the present invention will be described.
The alloy nanocrystal of the present invention is attached to the surface of the core portion including at least one transition metal element selected from Fe and Co and at least one noble metal element selected from Pt and Pd, and the core portion. It has a long-chain saturated fatty acid.
本発明の合金ナノ結晶を構成するコア部は、ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素とを含むものであり、例えば、ＦｅＰｔ、ＦｅＰｄ、ＣｏＰｔ、ＣｏＰｄからなるものである。上記遷移金属元素および貴金属元素は、実質的にｆｃｔ相を有するかまたはｆｃｔ相に相転移させることができるものであれば、それぞれコア部に２種づつ含まれていてもよく、例えば、ＦｅとＣｏの両者が含まれていてもよく、ＰｔとＰｄの両者が含まれていてもよい。 The core part constituting the alloy nanocrystal of the present invention contains at least one transition metal element selected from Fe and Co and at least one noble metal element selected from Pt and Pd. For example, FePt , FePd, CoPt, CoPd. The transition metal element and the noble metal element may be included in the core part in two types as long as they have substantially the fct phase or can be phase-shifted into the fct phase. Both Co and Pt and Pd may be included.
上記コア部は、実質的にｆｃｔ相を有するかまたはｆｃｔ相に相転移させることができるものであれば、上記遷移金属元素および貴金属元素以外に、さらに、Ａｕ、Ａｇ、Ｃｕ、Ｖ、Ｂｉ、Ｓｂ及びＭｎからなる群から選ばれる少なくも１種の第３金属元素を含んでもよい。コア部が上記第３金属元素を含む場合、合金ナノ結晶のｆｃｔ相への相転移温度を低くすることができる。 As long as the core portion substantially has an fct phase or can undergo phase transition to the fct phase, in addition to the transition metal element and the noble metal element, Au, Ag, Cu, V, Bi, It may contain at least one third metal element selected from the group consisting of Sb and Mn. When the core part contains the third metal element, the phase transition temperature of the alloy nanocrystal to the fct phase can be lowered.
上記遷移金属元素および貴金属元素の合計含有量に対する上記遷移金属元素の合計含有量の比は、モル比で０．４以上０．７以下であることが好ましく、０．４５以上０．６０以下であることがより好ましく、０．５０以上０．５５以下であることがさらに好ましい。遷移金属元素および貴金属元素の合計含有量に対する遷移金属元素の合計含有量の比が、上記範囲内にある場合、得られる合金ナノ結晶が実質的にｆｃｔ相を有するかまたはｆｃｔ相に容易に相転移することができる。 The ratio of the total content of the transition metal elements to the total content of the transition metal elements and noble metal elements is preferably 0.4 or more and 0.7 or less in terms of molar ratio, and is 0.45 or more and 0.60 or less. More preferably, it is 0.50 or more and 0.55 or less. When the ratio of the total content of the transition metal element to the total content of the transition metal element and the noble metal element is within the above range, the obtained alloy nanocrystal has substantially the fct phase or is easily phased into the fct phase. Can metastasize.
コア部が、Ａｕ、Ａｇ、Ｃｕ、Ｖ、Ｂｉ、Ｓｂ及びＭｎからなる群から選ばれる少なくも１種の第３金属元素を含む場合、第３金属元素の合計含有量は、コア部を構成する全金属元素量に対して５〜５０ａｔ％であることが好ましく、１０〜４０ａｔ％であることが
より好ましく、１５〜２０ａｔ％であることがさらに好ましい。第３金属元素の合計量がコア部を構成する全金属元素量に対して５ａｔ％未満では、合金ナノ結晶のｆｃｔ相への相転移温度を十分に低くすることができず、また、第３金属元素の合計量がコア部を構成する全金属元素量に対して５０ａｔ％を超えると、所望の磁気特性を得ることができなくなる。
When the core part includes at least one third metal element selected from the group consisting of Au, Ag, Cu, V, Bi, Sb and Mn, the total content of the third metal elements constitutes the core part It is preferable that it is 5-50 at% with respect to the total amount of metal elements to perform, It is more preferable that it is 10-40 at%, It is further more preferable that it is 15-20 at%. If the total amount of the third metal element is less than 5 at% with respect to the total amount of metal elements constituting the core portion, the phase transition temperature of the alloy nanocrystal to the fct phase cannot be sufficiently lowered, and the third When the total amount of metal elements exceeds 50 at% with respect to the total amount of metal elements constituting the core portion, desired magnetic properties cannot be obtained.
上記コア部は、通常、粒子形状を有しており、その平均粒径は１ｎｍ以上１５ｎｍ以下であることが好ましく、１ｎｍ以上１０ｎｍ以下であることがより好ましく、２ｎｍ以上８ｎｍ以下であることがさらに好ましい。上記平均粒径が１ｎｍ未満であると、高い結晶磁気異方性を有するｆｃｔ相においても合金ナノ結晶個々の異方性エネルギーが熱エネルギーに近接し、熱擾乱の影響が増大して磁気記録媒体材料として十分な熱安定性が得られない。また、上記平均粒径が１５ｎｍを越えると、有機溶媒に対する分散性が失われ、基板上へのナノ結晶単層膜の作製に適さなくなる。 The core part usually has a particle shape, and the average particle diameter is preferably 1 nm or more and 15 nm or less, more preferably 1 nm or more and 10 nm or less, and further preferably 2 nm or more and 8 nm or less. preferable. When the average particle size is less than 1 nm, even in the fct phase having high magnetocrystalline anisotropy, the anisotropy energy of individual alloy nanocrystals is close to the thermal energy, and the influence of thermal disturbance is increased, and the magnetic recording medium As a material, sufficient thermal stability cannot be obtained. On the other hand, when the average particle size exceeds 15 nm, the dispersibility with respect to the organic solvent is lost and the nanocrystal monolayer film on the substrate is not suitable.
なお、本明細書において、平均粒径とは、透過型電子顕微鏡写真により求めたものを意味する。 In addition, in this specification, an average particle diameter means what was calculated | required with the transmission electron micrograph.
本発明の合金ナノ結晶は、コア部の表面に付着した長鎖飽和脂肪酸を有している。長鎖飽和脂肪酸としては、アルキル基の炭素数が７〜２３のアルキルモノカルボン酸が好ましく、アルキル基の炭素数が７〜１９のアルキルモノカルボン酸がより好ましく、アルキル基の炭素数が１１〜１７のアルキルモノカルボン酸がさらに好ましい。このようなアルキルモノカルボン酸としては、例えば、ウンデシル酸（アルキル基の炭素数１０）、ラウリン酸（同１１）、トリデシル酸（同１２）、パルミチン酸（同１５）、へプタデシル酸（同１６）、ステアリン酸（同１７）、ノナデカン酸（同１８）、アラキン酸（炭素数１９）等を挙げることができる。アルキル基の炭素数が７未満であると、有機溶媒への分散性が落ちるので、有機溶媒中で合金ナノ結晶が沈殿、凝集しやすくなる。また、アルキル基の炭素数が２３を超えると、アルコールなどの極性溶媒に対する長鎖飽和脂肪酸
の溶解度が低下するので、合金ナノ結晶の単離、精製が困難になる。
The alloy nanocrystal of the present invention has long-chain saturated fatty acids attached to the surface of the core part. As long-chain saturated fatty acids, alkyl monocarboxylic acids having 7 to 23 carbon atoms in the alkyl group are preferable, alkyl monocarboxylic acids having 7 to 19 carbon atoms in the alkyl group are more preferable, and carbon atoms in the alkyl group having 11 to 11 carbon atoms. 17 alkyl monocarboxylic acids are more preferred. Examples of such alkyl monocarboxylic acids include undecyl acid (alkyl group having 10 carbon atoms), lauric acid (11), tridecyl acid (12), palmitic acid (15), heptadecyl acid (16). ), Stearic acid (17), nonadecanoic acid (18), arachidic acid (19 carbon atoms), and the like. When the carbon number of the alkyl group is less than 7, the dispersibility in an organic solvent is lowered, so that alloy nanocrystals are likely to precipitate and aggregate in the organic solvent. In addition, when the carbon number of the alkyl group exceeds 23, the solubility of the long-chain saturated fatty acid in a polar solvent such as alcohol decreases, so that it becomes difficult to isolate and purify the alloy nanocrystal.
上記長鎖飽和脂肪酸は、コア部表面を構成する金属元素に配位することにより付着していることが好ましい。 The long-chain saturated fatty acid is preferably attached by coordination with the metal element constituting the surface of the core part.
本発明の合金ナノ結晶は、相転移温度が３５０〜８００℃であることが好ましく、５５０〜７５０℃であることがより好ましく、６００〜７００℃であることがさらに好ましい。コア部が第３金属元素を含むものである場合、相転移温度は３００〜６００℃であることが好ましく、３５０〜５５０℃であることがより好ましく、４００〜５００℃であることがさらに好ましい。 The alloy nanocrystal of the present invention preferably has a phase transition temperature of 350 to 800 ° C, more preferably 550 to 750 ° C, and further preferably 600 to 700 ° C. When the core portion contains the third metal element, the phase transition temperature is preferably 300 to 600 ° C, more preferably 350 to 550 ° C, and further preferably 400 to 500 ° C.
本発明の合金ナノ結晶は、コア部表面に長鎖飽和脂肪酸を有しているため、有機溶媒、特に極性の小さな有機溶媒中に容易に単分散可能である。また、コア部表面の脂肪酸が不飽和結合を有さないことから、脂肪酸の重合による合金ナノ結晶同士の凝集を防止し、合金ナノ結晶を有機溶媒中に安定して分散させることができる。また、本発明の合金ナノ結晶は、コア部表面に長鎖飽和脂肪酸を有しているため、本発明の合金ナノ結晶を含む分散液を基板上に塗布すること等により、自己組織化現象を利用して基板上に安定して合金ナノ結晶を配列することが可能になる。 Since the alloy nanocrystal of the present invention has a long-chain saturated fatty acid on the surface of the core portion, it can be easily monodispersed in an organic solvent, particularly an organic solvent having a small polarity. Moreover, since the fatty acid on the surface of the core portion does not have an unsaturated bond, aggregation of the alloy nanocrystals due to polymerization of the fatty acid can be prevented, and the alloy nanocrystals can be stably dispersed in the organic solvent. In addition, since the alloy nanocrystal of the present invention has a long-chain saturated fatty acid on the surface of the core portion, the self-organization phenomenon can be prevented by applying a dispersion containing the alloy nanocrystal of the present invention on the substrate. It becomes possible to arrange alloy nanocrystals stably on the substrate.
本発明の合金ナノ結晶は、好ましくは、本発明の合金ナノ結晶の製造方法により製造することができる。 The alloy nanocrystals of the present invention can be preferably produced by the method for producing alloy nanocrystals of the present invention.
本発明の合金ナノ結晶の製造方法は、本発明の合金ナノ結晶を製造する方法であって、
ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素を含む長鎖飽和脂肪酸塩と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体とを、溶媒中、還元剤の存在下に加熱することを特徴とするものである。
The method for producing an alloy nanocrystal of the present invention is a method for producing an alloy nanocrystal of the present invention,
A long-chain saturated fatty acid salt containing at least one transition metal element selected from Fe and Co and a salt or complex of at least one noble metal element selected from Pt and Pd in a solvent in the presence of a reducing agent It is characterized by heating.
上記遷移金属元素を含む長鎖飽和脂肪酸塩は、アルキル基の炭素数が７〜２３のアルキルモノカルボン酸の塩であることが好ましく、アルキル基の炭素数が７〜１９のアルキルモノカルボン酸の塩であることがより好ましく、アルキル基の炭素数が１１〜１７のアルキルモノカルボン酸の塩であることがさらに好ましい。アルキルモノカルボン酸としては、例えば、ウンデシル酸（アルキル基の炭素数１０）、ラウリン酸（同１１）、トリデシル酸（同１２）、パルミチン酸（同１５）、へプタデシル酸（同１６）、ステアリン酸（同１７）、ノナデカン酸（同１８）、アラキン酸（炭素数１９）等を挙げることができる。 The long chain saturated fatty acid salt containing the transition metal element is preferably a salt of an alkyl monocarboxylic acid having an alkyl group having 7 to 23 carbon atoms, and an alkyl monocarboxylic acid having an alkyl group having 7 to 19 carbon atoms. A salt is more preferable, and a salt of an alkyl monocarboxylic acid having an alkyl group with 11 to 17 carbon atoms is further preferable. Examples of the alkyl monocarboxylic acid include undecyl acid (alkyl group having 10 carbon atoms), lauric acid (11), tridecyl acid (12), palmitic acid (15), heptadecyl acid (16), stearin. Examples include acid (17), nonadecanoic acid (18), and arachidic acid (19 carbon atoms).
このような長鎖脂肪酸塩としては、一般式（Ｉ）
（ＣｎＨ２ｎ＋２ＣＯＯ）２Ｆｅ （ただし、７≦ｎ≦２３） （Ｉ）
で示される２価のＦｅ脂肪酸塩や、一般式（II）
（ＣｎＨ２ｎ＋２ＣＯＯ）２Ｃｏ （ただし、７≦ｎ≦２３） （II）
で示される２価のＣｏ脂肪酸塩を挙げることができる。一般式（Ｉ）で表されるＦｅ脂肪酸塩および一般式（II）で表されるＣｏ脂肪酸塩は単独で使用してもよいし、２種類以上を組み合わせて使用してもよい。
Such long chain fatty acid salts include those represented by the general formula (I)
(C n H 2n + 2 COO) 2 Fe (where 7 ≦ n ≦ 23) (I)
Or a divalent Fe fatty acid salt represented by the general formula (II)
(C n H 2n + 2 COO) 2 Co (7 ≦ n ≦ 23) (II)
And a divalent Co fatty acid salt represented by the formula: The Fe fatty acid salt represented by the general formula (I) and the Co fatty acid salt represented by the general formula (II) may be used alone or in combination of two or more.
一般式（Ｉ）および一般式（II）で表される脂肪酸塩は毒性が低く、反応中に一酸化炭素のような有害な分解生成物を放出しない。また、酸素や水に対して安定であり、使用する前に精製を必要としないため、容易に合金ナノ結晶を製造することが可能になる。 The fatty acid salts represented by the general formula (I) and the general formula (II) have low toxicity and do not release harmful decomposition products such as carbon monoxide during the reaction. Moreover, since it is stable with respect to oxygen and water and does not require purification before use, alloy nanocrystals can be easily produced.
また、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体は、ハロゲン化物、酢酸塩等のカルボン酸塩、硝酸塩、アセチルアセトナト錯体等のβ−ジケトナト錯体、エチレンジアミン錯体、アンミン錯体、トリフェニルホスフィン錯体等のホスフィン錯体、ニトリル錯体、π−アリル錯体およびシクロオクタジエン錯体から選ばれる少なくとも１種の塩または錯体であることが好ましい。上記錯体としては、配位子中に炭素原子、窒素原子、酸素原子またはリン原子を電子供与原子として有する錯体や、配位子中の塩素原子、臭素原子またはヨウ素原子が白金またはパラジウムに配位した錯体であれば、特に制限なく使用することができ、このような錯体としては、上記錯体の他、例えば、クロロアンミン錯体、ブロモアンミン錯体、クロロホスフィン錯体等を挙げることができる。 Further, a salt or complex of at least one kind of noble metal element selected from Pt and Pd is a carboxylate such as a halide or acetate, a β-diketonate complex such as a nitrate or an acetylacetonato complex, an ethylenediamine complex, an ammine complex, It is preferably at least one salt or complex selected from phosphine complexes such as triphenylphosphine complexes, nitrile complexes, π-allyl complexes, and cyclooctadiene complexes. Examples of the complex include a complex having a carbon atom, nitrogen atom, oxygen atom or phosphorus atom as an electron donor atom in a ligand, or a chlorine atom, bromine atom or iodine atom in the ligand coordinated to platinum or palladium. The complex can be used without particular limitation. Examples of such a complex include chloroammine complexes, bromoammine complexes, and chlorophosphine complexes in addition to the above complexes.
上記遷移金属元素を含む長鎖飽和脂肪酸塩と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体の使用量は、遷移金属元素を含む長鎖飽和脂肪酸塩の使用量が、貴金属元素の塩または錯体の使用量に対してモル換算で０．５〜３．０倍であることが好ましく、０．８〜２．０倍であることがより好ましく、１．０〜１．５倍であることがさらに好ましい。 The amount of the long-chain saturated fatty acid salt containing the transition metal element and the salt or complex of at least one noble metal element selected from Pt and Pd is the same as that of the long-chain saturated fatty acid salt containing the transition metal element. The molar amount is preferably 0.5 to 3.0 times, more preferably 0.8 to 2.0 times, and more preferably 1.0 to 1.5 times the amount of the element salt or complex used. More preferably, it is double.
また、得られる合金ナノ結晶が、Ａｕ、Ａｇ、Ｃｕ、Ｖ、Ｂｉ、ＳｂおよびＭｎからなる群から選ばれる少なくも１種の第３金属元素を含む場合、第３元素の原料としては、上記各元素のハロゲン化物、硫酸塩、硝酸塩、カルボン酸塩等の塩や、アルコキシド、アンミン錯体、エチレンジアミン錯体、シアン錯体等の錯体を用いることができる。 Further, when the obtained alloy nanocrystal contains at least one third metal element selected from the group consisting of Au, Ag, Cu, V, Bi, Sb, and Mn, Salts such as halides, sulfates, nitrates, and carboxylates of each element, and complexes such as alkoxides, ammine complexes, ethylenediamine complexes, and cyanogen complexes can be used.
本発明の方法において用いられる溶媒としては、上記遷移金属元素を含む長鎖飽和脂肪酸塩および上記貴金属元素の塩または錯体と反応しないものが好ましい。また、上記溶媒としては、２００〜４００℃の範囲の沸点を有するものが好ましく、このような溶媒とし
ては、沸点が上記範囲内にある炭化水素、エーテル、アルコール、アルキルカルボン酸およびアルキルアミンから選ばれる少なくとも１種を挙げることができ、例えば、沸点が上記範囲内にある炭素数が１２〜２４のアルキルカルボン酸や、沸点が上記範囲内にある炭素数が１２〜２４のアルキルアミンを挙げることができる。
The solvent used in the method of the present invention is preferably a solvent that does not react with the long-chain saturated fatty acid salt containing the transition metal element and the salt or complex of the noble metal element. The solvent preferably has a boiling point in the range of 200 to 400 ° C., and such a solvent is selected from hydrocarbons, ethers, alcohols, alkylcarboxylic acids and alkylamines having a boiling point within the above range. For example, mention may be made of alkyl carboxylic acids having 12 to 24 carbon atoms having a boiling point within the above range, and alkylamines having 12 to 24 carbon atoms having a boiling point within the above range. Can do.
本発明の方法で用いられる還元剤としては、炭素数が８〜２４のアルコール、炭素数が８〜２４のホスフィン、水素化ホウ素化合物、シラン化合物、水素化リチウム、水素化ナトリウムおよびヒドラジンから選ばれる少なくとも１種を挙げることができ、特に炭素数が８〜２４のアルコール、炭素数が８〜２４のホスフィンが好ましい。上記水素化ホウ素化合物として、具体的には、リチウム塩またはナトリウム塩等が挙げられる。還元剤の使用量は、用いる還元剤の種類、遷移金属元素と貴金属元素の組合せ、反応温度等によって適宜規定することができる。 The reducing agent used in the method of the present invention is selected from alcohol having 8 to 24 carbon atoms, phosphine having 8 to 24 carbon atoms, borohydride compound, silane compound, lithium hydride, sodium hydride and hydrazine. At least one kind can be mentioned, and an alcohol having 8 to 24 carbon atoms and a phosphine having 8 to 24 carbon atoms are particularly preferable. Specific examples of the borohydride compound include lithium salts and sodium salts. The amount of the reducing agent used can be appropriately determined depending on the kind of the reducing agent used, the combination of the transition metal element and the noble metal element, the reaction temperature, and the like.
本発明の方法においては、例えば、上記遷移金属元素を含む長鎖飽和脂肪酸塩、上記貴金属元素の塩または錯体、および場合により第３金属元素の塩または錯体を、還元剤とともに溶媒中に加え、好ましくは２００〜４００℃、より好ましくは２５０〜３５０℃、さらに好ましくは２９０〜３２０℃の温度に加熱する。加熱処理は、マイクロ波加熱装置等の電磁波加熱装置、マントルヒーター、オイルバス等により行うことができ、加熱時間は、電磁波加熱装置による場合は１分間以上が好ましく、マントルヒーターやオイルバス等による場合は３０分間以上が好ましい。この加熱処理は、希ガスや窒素ガス等の不活性ガス雰囲気下で行うことが好ましい。 In the method of the present invention, for example, a long-chain saturated fatty acid salt containing the transition metal element, a salt or complex of the noble metal element, and optionally a salt or complex of a third metal element are added to a solvent together with a reducing agent, Preferably it heats to the temperature of 200-400 degreeC, More preferably, it is 250-350 degreeC, More preferably, it is 290-320 degreeC. The heat treatment can be performed with an electromagnetic heating device such as a microwave heating device, a mantle heater, an oil bath or the like, and the heating time is preferably 1 minute or more when using an electromagnetic heating device, or when using a mantle heater or an oil bath. Is preferably 30 minutes or longer. This heat treatment is preferably performed in an inert gas atmosphere such as a rare gas or nitrogen gas.
加熱処理することにより得られた合金ナノ結晶含有液に、アルコール等の合金ナノ結晶を沈殿し得る溶媒を加えて遠心分離すること等により、合金ナノ結晶を分離することができる。また、上記溶媒が、合金ナノ結晶を分散し得るものである場合は、合金ナノ結晶含有液を、そのまま合金ナノ結晶分散液とすることもできる。 The alloy nanocrystals can be separated by adding a solvent capable of precipitating the alloy nanocrystals such as alcohol and centrifuging the alloy nanocrystal-containing liquid obtained by the heat treatment. Moreover, when the said solvent can disperse | distribute an alloy nanocrystal, an alloy nanocrystal containing liquid can also be made into an alloy nanocrystal dispersion liquid as it is.
得られた合金ナノ結晶がｆｃｃ相を有するものである場合、不活性雰囲気中で、好ましくは３５０℃〜８００℃、より好ましくは５５０〜７５０℃、さらに好ましくは６００〜７００℃の温度範囲で加熱処理することにより、ｆｃｔ相に相転移させることができる。加熱処理は、例えば、電気炉、赤外線ヒーターまたはレーザー等により行うことができる。ｆｃｔ相への相転移は、Ｘ線回折法等により確認することができる。 When the obtained alloy nanocrystal has an fcc phase, it is heated in an inert atmosphere, preferably in a temperature range of 350 ° C to 800 ° C, more preferably 550 to 750 ° C, and even more preferably 600 to 700 ° C. By processing, the phase can be changed to the fct phase. The heat treatment can be performed by, for example, an electric furnace, an infrared heater, a laser, or the like. The phase transition to the fct phase can be confirmed by an X-ray diffraction method or the like.
本発明の合金ナノ結晶の製造方法においては、安全性が高く取り扱いの容易な原料を、原料量を低減しつつ使用できるとともに、安価な還元剤を使用することができ、また、得られる合金ナノ結晶を容易に単離精製することができるので、製造コストを低減しつつ、容易かつ効率的に合金ナノ結晶を製造することが可能になる。 In the method for producing alloy nanocrystals of the present invention, a safe and easy-to-handle raw material can be used while reducing the amount of the raw material, and an inexpensive reducing agent can be used. Since crystals can be easily isolated and purified, alloy nanocrystals can be easily and efficiently produced while reducing production costs.
次に、本発明の合金ナノ結晶分散液について説明する。
本発明の合金ナノ結晶分散液は、本発明の合金ナノ結晶が、該合金ナノ結晶と反応しない溶媒中に分散していることを特徴とする。
Next, the alloy nanocrystal dispersion liquid of the present invention will be described.
The alloy nanocrystal dispersion liquid of the present invention is characterized in that the alloy nanocrystals of the present invention are dispersed in a solvent that does not react with the alloy nanocrystals.
上記溶媒としては、本発明の合金ナノ結晶と反応せず、これを単分散し得るものであれば特に制限されず、例えば、炭素数が６〜１２の芳香族炭化水素、炭素数が１〜３の塩素化炭化水素、炭素数が５〜１８の飽和炭化水素および炭素数が４〜１８のエーテルから選ばれる少なくとも１種を挙げることができ、特に、トルエン、クロロホルム、ヘキサン、ジエチルエーテル等であることが好ましい。また、上記各溶媒から選ばれる少なくとも１種を５０容量％以上含むものが好ましく、８０容量％以上含むものがより好ましく、上記溶媒のみからなるものが特に好ましい。 The solvent is not particularly limited as long as it does not react with the alloy nanocrystals of the present invention and can be monodispersed. For example, an aromatic hydrocarbon having 6 to 12 carbon atoms, 1 to 1 carbon atoms. 3 chlorinated hydrocarbons, saturated hydrocarbons having 5 to 18 carbon atoms, and ethers having 4 to 18 carbon atoms, particularly toluene, chloroform, hexane, diethyl ether, etc. Preferably there is. Moreover, what contains 50 volume% or more of at least 1 sort (s) chosen from said each solvent is preferable, what contains 80 volume% or more is more preferable, and what consists only of the said solvent is especially preferable.
本発明の合金ナノ結晶分散液は、本発明の合金ナノ結晶を溶媒中に混合、分散することにより容易に得ることができる。 The alloy nanocrystal dispersion liquid of the present invention can be easily obtained by mixing and dispersing the alloy nanocrystals of the present invention in a solvent.
本発明の合金ナノ結晶分散液を用いて、高密度磁気記録媒体を製造する方法としては、例えば、本発明の合金ナノ結晶分散液をディップコート法等により基板上に塗布し、溶媒を乾燥処理する方法を挙げることができる。分散液中に含まれる合金ナノ結晶が、ｆｃｃ相を有するものである場合は、分散液を基板上に滴下した後、不活性雰囲気中で、好ましくは３５０℃〜８００℃、より好ましくは５５０〜７５０℃、さらに好ましくは６００〜７００℃の温度に加熱処理することにより、ｆｃｔ相に相転移させることができる。加熱処理は、例えば、電気炉、赤外線ヒーターまたはレーザー等により行うことができる。ｆｃｔ相への相転移は、Ｘ線回折法等により確認することができる。 As a method for producing a high-density magnetic recording medium using the alloy nanocrystal dispersion liquid of the present invention, for example, the alloy nanocrystal dispersion liquid of the present invention is applied on a substrate by a dip coating method or the like, and the solvent is dried. The method of doing can be mentioned. When the alloy nanocrystals contained in the dispersion have an fcc phase, after dropping the dispersion onto the substrate, in an inert atmosphere, preferably 350 ° C. to 800 ° C., more preferably 550 to 500 ° C. By heat treatment at a temperature of 750 ° C., more preferably 600 to 700 ° C., the phase can be changed to the fct phase. The heat treatment can be performed by, for example, an electric furnace, an infrared heater, a laser, or the like. The phase transition to the fct phase can be confirmed by an X-ray diffraction method or the like.
以下、本発明を実施例によりさらに詳細に説明するが、本発明は、これらの例によってなんら限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited at all by these examples.
実施例1
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 1
To 4 mL of dioctyl ether, 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 400 mg of 1,2-hexadecanediol are added, and the mixture is heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere. It was.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、上記ＦｅＰｔナノ結晶をトルエンに単分散させることによりＦｅＰｔナノ結晶のトルエン分散液を作製した。 In addition, a toluene dispersion of FePt nanocrystals was prepared by monodispersing the FePt nanocrystals in toluene.
上記ＦｅＰｔナノ結晶において、コア部の組成、コア部の平均粒径、コア部の結晶相を以下の方法で測定し、得られた結果を表１に示す。 In the FePt nanocrystal, the composition of the core part, the average particle diameter of the core part, and the crystal phase of the core part were measured by the following methods, and the obtained results are shown in Table 1.
（１）コア部の組成
ＩＣＰ発光分光分析装置（セイコー電子工業（株）製ＳＰＳ４０００）を用いて、誘導結合プラズマ原子発光法により、測定した。
（２）コア部の平均粒径
粒子像を透過型電子顕微鏡（日本電子（株）製、ＪＥＭ２０００ＥＸ）で観察することにより、測定した。
（３）コア部の結晶相
Ｘ線回折装置（（株）マックサイエンス製、ＭＸＰ−１８）により、確認した。
(1) Composition of core part It measured by the inductively coupled plasma atomic emission method using the ICP emission-spectral-analysis apparatus (Seiko Electronics Co., Ltd. product SPS4000).
(2) Average particle diameter of core part It measured by observing a particle image with a transmission electron microscope (the JEOL Co., Ltd. make, JEM2000EX).
(3) Crystal phase of core part It confirmed with the X-ray-diffraction apparatus (Corporation | KK MacScience make, MXP-18).
また、得られたＦｅＰｔナノ結晶を、１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Further, the obtained FePt nanocrystal was heat-treated at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, and confirmed to undergo phase transition to the fct phase by X-ray diffraction.
実施例２
オクタデセン４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら３２０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 2
To 4 mL of octadecene, 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 400 mg of 1,2-hexadecanediol were added, and the mixture was heated at 320 ° C. for 30 minutes with stirring in an Ar gas atmosphere. .
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、上記ＦｅＰｔナノ結晶をトルエンに単分散させることにより、ＦｅＰｔナノ結晶のトルエン分散液を作製した。 In addition, a toluene dispersion of FePt nanocrystals was prepared by monodispersing the FePt nanocrystals in toluene.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1.
実施例３
２−ドデカノール４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら３００℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 3
Add 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 400 mg of 1,2-hexadecanediol to 4 mL of 2-dodecanol, and heat at 300 ° C. for 30 minutes with stirring in an Ar gas atmosphere. I did it.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、上記ＦｅＰｔナノ結晶をクロロホルムに単分散させることによりＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 Also, a chloroform dispersion of FePt nanocrystals was prepared by monodispersing the FePt nanocrystals in chloroform.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例４
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ｃｉｓ−ジクロロビス（トリフェニルホスフィン）白金（II）８０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることによりステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 4
To 4 mL of dioctyl ether, 90 mg of iron (II) stearate, 80 mg of cis-dichlorobis (triphenylphosphine) platinum (II) and 400 mg of 1,2-hexadecanediol are added and heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere. Was done.
After cooling the reaction solution to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をジエチルエーテルに分散させることによりＦｅＰｔナノ結晶のジエチルエーテル分散液を作製した。 Further, the obtained FePt nanocrystals were dispersed in diethyl ether to prepare a diethyl ether dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例５
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよびトリオクチルホスフィン５６０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることによりステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 5
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 560 mg of trioctylphosphine, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After cooling the reaction solution to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をクロロホルムに単分散させることにより、ＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 The obtained FePt nanocrystals were monodispersed in chloroform to prepare a chloroform dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例６
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよびトリヘキシルシラン４３０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 6
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 430 mg of trihexylsilane, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をクロロホルムに単分散させることにより、ＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 The obtained FePt nanocrystals were monodispersed in chloroform to prepare a chloroform dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例７
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよびトリ−２−ブチル水素化ホウ素リチウム２９０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 7
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 290 mg of lithium tri-2-butylborohydride, and the mixture was stirred at 280 ° C. for 30 minutes in an Ar gas atmosphere. Heating was performed.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をクロロホルムに単分散させることにより、ＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 The obtained FePt nanocrystals were monodispersed in chloroform to prepare a chloroform dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例８
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび水素化リチウム３０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 8
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 30 mg of lithium hydride, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をクロロホルムに単分散させることにより、ＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 The obtained FePt nanocrystals were monodispersed in chloroform to prepare a chloroform dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例９
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび水素化ナトリウム６０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｔナノ結晶を得た。
Example 9
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 60 mg of sodium hydride, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePt nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｔナノ結晶をクロロホルムに単分散させることにより、ＦｅＰｔナノ結晶のクロロホルム分散液を作製した。 The obtained FePt nanocrystals were monodispersed in chloroform to prepare a chloroform dispersion of FePt nanocrystals.
得られたＦｅＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained FePt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例１０
ジオクチルエーテル４ｍＬにステアリン酸コバルト（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＣｏＰｔナノ結晶を得た。
Example 10
To 4 mL of dioctyl ether, 90 mg of cobalt (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 400 mg of 1,2-hexadecanediol are added, and the mixture is heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere. It was.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain CoPt nanocrystals with stearic acid attached to the surface.
また、得られたＣｏＰｔナノ結晶をトルエンに単分散させることにより、ＣｏＰｔナノ結晶のトルエン分散液を作製した。 Further, the obtained CoPt nanocrystals were monodispersed in toluene to prepare a CoPt nanocrystal toluene dispersion.
得られたＣｏＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained CoPt nanocrystals in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例１１
オクタデセン４ｍＬにステアリン酸コバルト（II）９０ｍｇ、ビス（アセチルアセトナト）白金（II）４０ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら３２０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＣｏＰｔナノ結晶を得た。
Example 11
To 4 mL of octadecene, 90 mg of cobalt (II) stearate, 40 mg of bis (acetylacetonato) platinum (II) and 400 mg of 1,2-hexadecanediol were added, and the mixture was heated at 320 ° C. for 30 minutes with stirring in an Ar gas atmosphere. .
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain CoPt nanocrystals with stearic acid attached to the surface.
また、得られたＣｏＰｔナノ結晶をトルエンに単分散させることによりステアリン酸で表面を保護されたＣｏＰｔナノ結晶のトルエン分散液を作製した。 Further, the obtained CoPt nanocrystals were monodispersed in toluene to prepare a toluene dispersion of CoPt nanocrystals whose surface was protected with stearic acid.
得られたＣｏＰｔナノ結晶における、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。 Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core part in the obtained CoPt nanocrystals in the same manner as in Example 1.
実施例１２
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、ビス（アセチルアセトナト）パラジウム（II）３１ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加えて遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｄナノ結晶を得た。
Example 12
To 4 mL of dioctyl ether, 90 mg of iron (II) stearate, 31 mg of bis (acetylacetonato) palladium (II) and 400 mg of 1,2-hexadecanediol were added, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere. It was.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePd nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｄナノ結晶をヘキサンに溶解することにより、ＦｅＰｄナノ結晶のヘキサン溶液を作製した。 Moreover, the hexane solution of FePd nanocrystal was produced by melt | dissolving the obtained FePd nanocrystal in hexane.
得られたＦｅＰｄナノ結晶において、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線
回折により確認した。
Table 1 shows the results obtained by examining the composition, average particle diameter, and crystal phase of the core portion of the obtained FePd nanocrystal in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例１３
ジオクチルエーテル４ｍＬにステアリン酸鉄（II）９０ｍｇ、酢酸パラジウム（II）２３ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加え遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＦｅＰｄナノ結晶を得た。
Example 13
To 4 mL of dioctyl ether were added 90 mg of iron (II) stearate, 23 mg of palladium (II) acetate and 400 mg of 1,2-hexadecanediol, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain FePd nanocrystals with stearic acid attached to the surface.
また、得られたＦｅＰｄナノ結晶をヘキサンに溶解することにより、ＦｅＰｄナノ結晶のヘキサン溶液を作製した。 Moreover, the hexane solution of FePd nanocrystal was produced by melt | dissolving the obtained FePd nanocrystal in hexane.
得られたＦｅＰｄナノ結晶において、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。また、得られたナノ結晶を１０−５Ｔｏｒｒの真空中で７００℃，３０分加熱処理をすることにより、ｆｃｔ相へ相転移することをＸ線回折により確認した。 Table 1 shows the results obtained by examining the composition, average particle diameter, and crystal phase of the core portion of the obtained FePd nanocrystal in the same manner as in Example 1. Moreover, it was confirmed by X-ray diffraction that the obtained nanocrystal was subjected to a heat treatment at 700 ° C. for 30 minutes in a vacuum of 10 −5 Torr, thereby transitioning to the fct phase.
実施例１４
ジオクチルエーテル４ｍＬにステアリン酸コバルト（II）９０ｍｇ、ビス（アセチルアセトナト）パラジウム（II）３１ｍｇおよび１，２−ヘキサデカンジオール４００ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加え遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＣｏＰｄナノ結晶を得た。
Example 14
To 4 mL of dioctyl ether, 90 mg of cobalt (II) stearate, 31 mg of bis (acetylacetonato) palladium (II) and 400 mg of 1,2-hexadecanediol were added, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere. It was.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain CoPd nanocrystals with stearic acid attached to the surface.
また、得られたＣｏＰｄナノ結晶をヘキサンに溶解することにより、ＣｏＰｄナノ結晶のヘキサン溶液を作製した。 Further, the obtained CoPd nanocrystal was dissolved in hexane to prepare a hexane solution of CoPd nanocrystal.
得られたＣｏＰｄナノ結晶において、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。 In the obtained CoPd nanocrystal, Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core portion in the same manner as in Example 1.
実施例１５
ジオクチルエーテル４ｍＬにステアリン酸コバルト（II）９０ｍｇ、硝酸パラジウム（II）２３ｍｇおよびトリオクチルホスフィン５６０ｍｇを加え、Ａｒガス雰囲気下で撹拌しながら２８０℃で３０分加熱を行なった。
反応溶液を室温まで冷却した後、エタノールを加え遠心分離を行い、沈殿物を集めることにより、ステアリン酸が表面に付着したＣｏＰｄナノ結晶を得た。
Example 15
To 4 mL of dioctyl ether were added 90 mg of cobalt stearate (II), 23 mg of palladium nitrate (II) and 560 mg of trioctylphosphine, and the mixture was heated at 280 ° C. for 30 minutes with stirring in an Ar gas atmosphere.
After the reaction solution was cooled to room temperature, ethanol was added and the mixture was centrifuged, and the precipitate was collected to obtain CoPd nanocrystals with stearic acid attached to the surface.
また、得られたＣｏＰｄナノ結晶をヘキサンに溶解することにより、ＣｏＰｄナノ結晶のヘキサン溶液を作製した。 Further, the obtained CoPd nanocrystal was dissolved in hexane to prepare a hexane solution of CoPd nanocrystal.
得られたＣｏＰｄナノ結晶において、コア部の組成、平均粒径および結晶相を実施例１と同様の方法で調べた結果を表１に示す。 In the obtained CoPd nanocrystal, Table 1 shows the results of examining the composition, average particle diameter, and crystal phase of the core portion in the same manner as in Example 1.
実施例１〜１５より、本発明においては、新規な合金ナノ結晶を、取り扱いの容易な原料を用い、製造コストを低減しつつ、反応液から容易に単離精製して作製できることが分かる。また、得られた合金ナノ結晶は、表面に長鎖飽和脂肪酸を有していることから、溶媒中に容易に分散することができ、空気酸化を受けたり合金ナノ結晶同士の凝集が起きることなく長期間安定して分散できることが分かる。さらに、本発明の合金ナノ結晶は、そのほとんどがｆｃｔ相を有するかまたはｆｃｔ相に相転移させることができるものであるため、基板上に配列したときに、高密度磁気記録媒体、磁気抵抗効果素子、燃料電池の電極用の触媒または磁気温熱療法用の発熱体等として好適に使用し得るものであることが分かる。 From Examples 1 to 15, it can be seen that in the present invention, novel alloy nanocrystals can be easily isolated and purified from the reaction solution while using raw materials that are easy to handle and reducing manufacturing costs. In addition, since the obtained alloy nanocrystals have long-chain saturated fatty acids on the surface, they can be easily dispersed in a solvent without being subjected to air oxidation or aggregation of alloy nanocrystals. It can be seen that it can be dispersed stably for a long time. Furthermore, most of the alloy nanocrystals of the present invention have an fct phase or can be transformed into the fct phase. Therefore, when arranged on a substrate, the alloy nanocrystal has a high-density magnetic recording medium and a magnetoresistive effect. It can be seen that it can be suitably used as an element, a catalyst for fuel cell electrodes, a heating element for magnetic thermotherapy, or the like.
本発明によれば、製造コストを低減しつつ容易かつ効率よく製造することができ、溶媒中に容易かつ長期間安定して分散可能で、基板上に配列したときに、高密度磁気記録媒体、磁気抵抗効果素子、燃料電池の電極用の触媒または磁気温熱療法用の発熱体等として好適に使用し得る新規合金ナノ結晶を提供することができる。また、本発明によれば、上記合金ナノ結晶を製造する方法および上記合金ナノ結晶の分散液を提供することができる。 According to the present invention, the high-density magnetic recording medium can be easily and efficiently manufactured while reducing the manufacturing cost, can be easily and stably dispersed in a solvent for a long period of time, and is arranged on a substrate. It is possible to provide a novel alloy nanocrystal that can be suitably used as a magnetoresistive element, a catalyst for an electrode of a fuel cell, a heating element for magnetic thermotherapy, or the like. Moreover, according to this invention, the manufacturing method of the said alloy nanocrystal and the dispersion liquid of the said alloy nanocrystal can be provided.
Claims (13)
ＦｅおよびＣｏから選ばれる少なくとも１種の遷移金属元素を含む長鎖飽和脂肪酸塩と、ＰｔおよびＰｄから選ばれる少なくとも１種の貴金属元素の塩または錯体とを、溶媒中、還元剤の存在下に加熱することを特徴とする合金ナノ結晶の製造方法。 A method for producing the alloy nanocrystal according to any one of claims 1 to 4,
A long-chain saturated fatty acid salt containing at least one transition metal element selected from Fe and Co and a salt or complex of at least one noble metal element selected from Pt and Pd in a solvent in the presence of a reducing agent The manufacturing method of the alloy nanocrystal characterized by heating.
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