WO2014196785A1 - 중공 금속 나노입자 - Google Patents
중공 금속 나노입자 Download PDFInfo
- Publication number
- WO2014196785A1 WO2014196785A1 PCT/KR2014/004934 KR2014004934W WO2014196785A1 WO 2014196785 A1 WO2014196785 A1 WO 2014196785A1 KR 2014004934 W KR2014004934 W KR 2014004934W WO 2014196785 A1 WO2014196785 A1 WO 2014196785A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- metal
- hollow
- metal nanoparticles
- present specification
- surfactant
- Prior art date
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- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 179
- 229910052751 metal Inorganic materials 0.000 claims description 173
- 239000002184 metal Substances 0.000 claims description 173
- 239000004094 surface-active agent Substances 0.000 claims description 130
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 53
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 40
- 239000002245 particle Substances 0.000 claims description 39
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 36
- -1 lanthanum group metals Chemical class 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 27
- 239000011651 chromium Substances 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
- 239000010948 rhodium Substances 0.000 claims description 18
- 239000011669 selenium Substances 0.000 claims description 18
- 239000010936 titanium Substances 0.000 claims description 18
- 239000010931 gold Substances 0.000 claims description 16
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- 229910052763 palladium Inorganic materials 0.000 claims description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 9
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052797 bismuth Inorganic materials 0.000 claims description 9
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 9
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 229910052741 iridium Inorganic materials 0.000 claims description 9
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 239000011733 molybdenum Substances 0.000 claims description 9
- 229910052762 osmium Inorganic materials 0.000 claims description 9
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 9
- 229910052702 rhenium Inorganic materials 0.000 claims description 9
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 9
- 229910052703 rhodium Inorganic materials 0.000 claims description 9
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 9
- 229910052707 ruthenium Inorganic materials 0.000 claims description 9
- 229910052711 selenium Inorganic materials 0.000 claims description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 229910052752 metalloid Inorganic materials 0.000 claims description 4
- 150000002738 metalloids Chemical class 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 description 60
- 150000003839 salts Chemical class 0.000 description 59
- 239000000693 micelle Substances 0.000 description 44
- 150000002500 ions Chemical class 0.000 description 32
- 238000004519 manufacturing process Methods 0.000 description 27
- 239000003638 chemical reducing agent Substances 0.000 description 20
- 239000002105 nanoparticle Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000002904 solvent Substances 0.000 description 15
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 14
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 14
- 239000002736 nonionic surfactant Substances 0.000 description 13
- 230000008901 benefit Effects 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 10
- 239000003945 anionic surfactant Substances 0.000 description 9
- 150000001450 anions Chemical class 0.000 description 9
- 239000003093 cationic surfactant Substances 0.000 description 9
- 150000001768 cations Chemical class 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- IZWSFJTYBVKZNK-UHFFFAOYSA-N lauryl sulfobetaine Chemical compound CCCCCCCCCCCC[N+](C)(C)CCCS([O-])(=O)=O IZWSFJTYBVKZNK-UHFFFAOYSA-N 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 230000009467 reduction Effects 0.000 description 7
- 244000060011 Cocos nucifera Species 0.000 description 6
- 235000013162 Cocos nucifera Nutrition 0.000 description 6
- 239000003381 stabilizer Substances 0.000 description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 5
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000002356 single layer Substances 0.000 description 5
- 239000001509 sodium citrate Substances 0.000 description 5
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 5
- 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 5
- 229940038773 trisodium citrate Drugs 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229960003237 betaine Drugs 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 3
- 229960000686 benzalkonium chloride Drugs 0.000 description 3
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 3
- QWSZRRAAFHGKCH-UHFFFAOYSA-M sodium;hexane-1-sulfonate Chemical compound [Na+].CCCCCCS([O-])(=O)=O QWSZRRAAFHGKCH-UHFFFAOYSA-M 0.000 description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 2
- YJHSJERLYWNLQL-UHFFFAOYSA-N 2-hydroxyethyl(dimethyl)azanium;chloride Chemical compound Cl.CN(C)CCO YJHSJERLYWNLQL-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- FXJNQQZSGLEFSR-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride;hydrate Chemical compound O.[Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 FXJNQQZSGLEFSR-UHFFFAOYSA-M 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 description 2
- 229960001927 cetylpyridinium chloride Drugs 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- KXGVEGMKQFWNSR-UHFFFAOYSA-N deoxycholic acid Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 KXGVEGMKQFWNSR-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 125000005908 glyceryl ester group Chemical group 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
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- 239000002563 ionic surfactant Substances 0.000 description 2
- HICYUNOFRYFIMG-UHFFFAOYSA-N n,n-dimethyl-1-naphthalen-1-ylmethanamine;hydrochloride Chemical compound [Cl-].C1=CC=C2C(C[NH+](C)C)=CC=CC2=C1 HICYUNOFRYFIMG-UHFFFAOYSA-N 0.000 description 2
- ZHALDANPYXAMJF-UHFFFAOYSA-N octadecanoate;tris(2-hydroxyethyl)azanium Chemical compound OCC[NH+](CCO)CCO.CCCCCCCCCCCCCCCCCC([O-])=O ZHALDANPYXAMJF-UHFFFAOYSA-N 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
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- 239000002243 precursor Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- REFMEZARFCPESH-UHFFFAOYSA-M sodium;heptane-1-sulfonate Chemical compound [Na+].CCCCCCCS([O-])(=O)=O REFMEZARFCPESH-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
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- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 description 1
- PSBDWGZCVUAZQS-UHFFFAOYSA-N (dimethylsulfonio)acetate Chemical compound C[S+](C)CC([O-])=O PSBDWGZCVUAZQS-UHFFFAOYSA-N 0.000 description 1
- PORPENFLTBBHSG-MGBGTMOVSA-N 1,2-dihexadecanoyl-sn-glycerol-3-phosphate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(O)=O)OC(=O)CCCCCCCCCCCCCCC PORPENFLTBBHSG-MGBGTMOVSA-N 0.000 description 1
- TZCPCKNHXULUIY-RGULYWFUSA-N 1,2-distearoyl-sn-glycero-3-phosphoserine Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(=O)OC[C@H](N)C(O)=O)OC(=O)CCCCCCCCCCCCCCCCC TZCPCKNHXULUIY-RGULYWFUSA-N 0.000 description 1
- QAQSNXHKHKONNS-UHFFFAOYSA-N 1-ethyl-2-hydroxy-4-methyl-6-oxopyridine-3-carboxamide Chemical compound CCN1C(O)=C(C(N)=O)C(C)=CC1=O QAQSNXHKHKONNS-UHFFFAOYSA-N 0.000 description 1
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- DBRHJJQHHSOXCQ-UHFFFAOYSA-N 2,2-dihydroxyethyl(methyl)azanium;chloride Chemical compound [Cl-].C[NH2+]CC(O)O DBRHJJQHHSOXCQ-UHFFFAOYSA-N 0.000 description 1
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 1
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- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
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- 229910010082 LiAlH Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- RFDAIACWWDREDC-UHFFFAOYSA-N Na salt-Glycocholic acid Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(=O)NCC(O)=O)C)C1(C)C(O)C2 RFDAIACWWDREDC-UHFFFAOYSA-N 0.000 description 1
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- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 1
- 229920000691 Poly[bis(2-chloroethyl) ether-alt-1,3-bis[3-(dimethylamino)propyl]urea] Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
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Images
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
- Y10S977/775—Nanosized powder or flake, e.g. nanosized catalyst
- Y10S977/777—Metallic powder or flake
Definitions
- the present disclosure relates to hollow metal nanoparticles.
- Nanoparticles are nanoscale particle size particles, which are completely different from bulk materials due to their large specific surface area and quantumconfinement effect, in which the energy required for electron transfer varies with the size of the material. Electrical and magnetic properties. Therefore, because of these properties, much attention has been focused on its application in the field of catalysts, electromagnetism, optics, medicine, and the like. Nanoparticles are intermediates between bulk and molecules, and are capable of synthesizing nanoparticles in terms of a two-way approach, a "top-down” approach and a “bottom-up” approach.
- Synthesis methods of metal nanoparticles include a method of reducing metal ions with a reducing agent in a solution, a method using gamma rays, and an electrochemical method, but conventional methods are difficult to synthesize nanoparticles having a uniform size and shape, or organic solvents.
- the economical mass production of high quality nanoparticles has been difficult due to various reasons, such as environmental pollution and high cost. Therefore, development of high quality nanoparticles of uniform size has been required.
- the problem to be solved by the present specification is to provide a high quality hollow metal nanoparticles of uniform size.
- Hollow core portion A shell part including a first metal and a second metal; And a cavity extending from the outer surface of the shell portion to the hollow core in at least one region of the shell portion.
- one embodiment of the present specification provides a catalyst including the hollow metal nanoparticles.
- Hollow metal nanoparticles of the present specification has the advantage that can be applied in various fields by providing hollow metal nanoparticles of uniform size to a few nanometers. Furthermore, since the hollow metal nanoparticles of the present specification include a cavity and can utilize a contact area up to the inner surface area of the shell through the cavity, the hollow metal nanoparticles have an advantage of increasing catalyst efficiency when included in a catalyst.
- FIG 1 illustrates an example of the hollow metal nanoparticles according to one embodiment of the present specification.
- TEM 4 and 5 show transmission electron microscope (TEM) images of the hollow metal nanoparticles prepared by Example 2 of the present specification.
- FIGS 6 and 7 show transmission electron microscope (TEM) images of the hollow metal nanoparticles prepared by Example 3 of the present specification.
- TEM 8 and 9 show transmission electron microscope (TEM) images of the hollow metal nanoparticles prepared by Example 4 of the present specification.
- One embodiment of the present specification comprises a hollow core; A shell part including a first metal and a second metal; And a cavity extending from the outer surface of the shell portion to the hollow core in at least one region of the shell portion.
- a surfactant may be included in the inner hollow, or the surfactant may be removed in the inner hollow.
- FIG. 1 illustrates an example in which two or more surfactants are mixed in an internal hollow as a step before forming a shell part by a reducing agent in the manufacture of the hollow metal nanoparticles of the present specification.
- the hollow may include a surfactant.
- the hollow may have a surfactant removed.
- the hollow means that the core portion of the metal nanoparticle is empty.
- the hollow may be used in the same sense as the hollow core.
- the hollow may include terms such as hollow, hole, void, and the like.
- the hollow core may be 50% by volume or more and less than 100% by volume of the hollow metal nanoparticles. Specifically, the hollow core may be 70 volume% or more, more specifically 80 volume% or more of the hollow metal nanoparticles.
- the hollow may include a space in which no internal material is present at 50% by volume or more, specifically 70% by volume or more, more specifically 80% by volume or more.
- at least 50% by volume, specifically 70% by volume, more specifically 80% by volume may include an empty space.
- it may include a space having an internal porosity of at least 50 vol%, specifically at least 70 vol%, more specifically at least 80 vol%.
- the hollow metal nanoparticles may have a spherical shape.
- the spherical shape of the present specification does not mean only a perfect spherical shape, but may include an approximately spherical shape.
- the hollow metal nanoparticles may not have a flat outer surface, and the radius of curvature of one hollow metal nanoparticle may not be constant.
- the hollow metal nanoparticles may have a particle diameter of 1 nm or more and 30 nm or less, more specifically 20 nm or less, or 12 nm or less, or 10 nm or less.
- the average particle diameter of the metal nanoparticles may be 6 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more.
- the particle diameter of the hollow metal nanoparticles is 30 nm or less, there is a great advantage that the nanoparticles can be used in various fields.
- the particle diameter of a hollow metal nanoparticle is 20 nm or less, it is more preferable.
- the particle diameter of the hollow metal nanoparticles is 10 nm or less, the surface area of the particles becomes wider, and thus, there is an advantage in that the application possibility that can be used in various fields becomes larger.
- the efficiency can be significantly increased.
- the average particle diameter of the hollow metal nanoparticles is measured for 200 or more hollow metal nanoparticles using graphic software (MAC-View), and the average particle diameter is measured through the obtained statistical distribution. It means the value.
- MAC-View graphic software
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 30 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 20 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 12 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 10 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 6 nm or less.
- the thickness of the shell part in the hollow metal nanoparticle may be greater than 0 nm and 5 nm or less, more specifically greater than 0 nm and 3 nm or less.
- the average particle diameter may be 30 nm or less
- the thickness of the shell portion may be more than 0 nm and 5 nm or less
- the average particle diameter of the hollow metal nanoparticles is 20 It may be less than or equal to 10 nm and less than a thickness of the shell portion greater than 0 nm and less than or equal to 3 nm.
- the hollow particle diameter of the hollow metal nanoparticles may be 1 nm or more and 10 nm or less, specifically 1 nm or more and 4 nm or less.
- each shell may be 0.2 nm or more and 5 nm or less, specifically 0.25 nm or more and 3 nm or less.
- the shell portion may be a shell formed by mixing the first metal and the second metal, or may be a plurality of shells including a first shell and a second shell, each having a different mixing ratio of the first metal and the second metal.
- the plurality of shells may include a first shell including only the first metal and a second shell including only the second metal.
- one or more hollow metal nanoparticles may be manufactured when the hollow metal nanoparticles are prepared.
- the particle diameter of the hollow metal nanoparticles may be within a range of 80% to 120% of the average particle diameter of the hollow metal nanoparticles.
- the particle diameter of the hollow metal nanoparticles may be in the range of 90% to 110% of the average particle diameter of the hollow metal nanoparticles. If it is out of the above range, since the size of the hollow metal nanoparticles becomes entirely non-uniform, it may be difficult to secure the unique physical properties required by the hollow metal nanoparticles.
- the effect of improving the efficiency may be somewhat insufficient. Therefore, when within the range of 80% to 120% of the average particle diameter of the hollow metal nanoparticles of the present disclosure, by forming a nanoparticle of a uniform size, it can exhibit excellent physical properties as nanoparticles.
- the content of the hollow metal nanoparticles including a cavity from the outer surface of the shell portion to the hollow core is contained in one or two or more regions of the shell portion of the present specification. It may be more than 50% and less than 100% of the total nanoparticles. Specifically, the content of the hollow metal nanoparticles including a cavity continuous from the outer surface of the shell portion to the hollow core portion may be 70% or more and 100% or less of the total nanoparticles.
- the hollow metal nanoparticle may include one cavity.
- the shell part may be a single layer.
- the shell portion of the single layer may include both the first metal and the second metal.
- the first metal and the second metal when the shell part is a single layer, the first metal and the second metal may be present in a mixed form. Further, when the shell portion is a single layer, the first metal and the second metal may be mixed uniformly or non-uniformly.
- the shell part may be two or more layers. Specifically, according to one embodiment of the present specification, when the shell portion is two or more layers, a first shell including the first metal; And a second shell including the second metal.
- the first shell may include the first metal and may not include the second metal.
- the second shell may include the second metal and may not include the first metal.
- the first shell may have a higher content of the first metal than the content of the second metal.
- the second shell may have a higher content of the second metal than that of the first metal.
- the first shell may be formed to surround the hollow, and the second shell may be formed to surround the first shell.
- the shell part may include: a first shell having a content of the first metal higher than that of the second metal; And a second shell in which the content of the second metal is higher than the content of the first metal.
- the content of the first metal in the first shell is the highest in the region close to the center of the hollow, and the content of the first metal gradually increases as the distance from the center of the hollow is increased. Can be small.
- the content of the second metal in the first shell may increase as the distance from the center of the hollow.
- the content of the second metal in the second shell is the highest in the region farthest from the center of the hollow, and the closer to the center of the hollow, the content of the second metal is gradually increased. Can be small.
- the content of the first metal in the second shell may decrease as the distance from the center of the hollow.
- the shell portion may be present in a state in which the first metal and the second metal are gradated, and the portion of the shell portion adjacent to the core may be present in a volume of 50 vol% or more, or 70 vol% or more. In the surface portion in contact with the outside of the nanoparticles in the second metal may be present in more than 50% by volume, or more than 70% by volume.
- an atomic percentage ratio of the first metal and the second metal of the shell part may be 1: 5 to 10: 1.
- the atomic percentage ratio may be an atomic percentage ratio of the first metal of the first shell and the second metal of the second shell when the shell portion is formed of the first shell and the second shell.
- the atomic percentage ratio may be an atomic percentage ratio of the first metal and the second metal when the shell portion is formed of a single layer including the first metal and the second metal.
- the shell part of the present specification may mean an outer material layer surrounding the hollow.
- the shape of the hollow metal nanoparticles may be determined by the shell portion.
- the thickness of the shell part may be greater than 0 nm and 5 nm or less.
- the thickness of the shell portion may be greater than 0 nm and 3 nm or less.
- the thickness of the shell portion may be greater than 0 nm and 5 nm or less.
- the thickness of the shell portion may be greater than 0 nm and 3 nm or less.
- the first metal may be selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to Groups 3 to 15 of the periodic table.
- the first metal is platinum (Pt); Ruthenium (Ru); Rhodium (Rh); Molybdenum (Mo); Osmium (Os); Iridium (Ir); Rhenium (Re); Palladium (Pd); Vanadium (V); Tungsten (W); Cobalt (Co); Iron (Fe); Selenium (Se); Nickel (Ni); Bismuth (Bi); Tin (Sn); Chromium (Cr); Titanium (Ti); Gold (Au); Cerium (Ce); Silver (Ag); And it may be selected from the group consisting of copper (Cu).
- the second metal may be different from the first metal.
- the second metal may be selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to groups 3 to 15 of the periodic table.
- the second metal is platinum (Pt); Ruthenium (Ru); Rhodium (Rh); Molybdenum (Mo); Osmium (Os); Iridium (Ir); Rhenium (Re); Palladium (Pd); Vanadium (V); Tungsten (W); Cobalt (Co); Iron (Fe); Selenium (Se); Nickel (Ni); Bismuth (Bi); Tin (Sn); Chromium (Cr); Titanium (Ti); Gold (Au); Cerium (Ce); Silver (Ag); And it may be selected from the group consisting of copper (Cu).
- the first metal may be selected from the group consisting of platinum (Pt), silver (Ag), palladium (Pd), and gold (Au), and more specifically, platinum (Pt).
- the second metal is ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten ( W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), chromium (Cr), titanium (Ti), cerium (Ce), silver ( Ag) and copper (Cu) may be selected from the group consisting of, and more specifically, may be nickel (Ni).
- the first metal may be ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten (W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), chromium (Cr), titanium It may be selected from the group consisting of (Ti), cerium (Ce), silver (Ag) and copper (Cu), more specifically may be nickel (Ni).
- the second metal may be selected from the group consisting of platinum (Pt), silver (Ag), palladium (Pd), and gold (Au), and more specifically, platinum (Pt).
- the first metal or the second metal may be different from each other, and the first metal or the second metal may be nickel.
- the first metal or the second metal may be different from each other, and the first metal or the second metal may be platinum.
- the first metal may be nickel, and the second metal may be platinum.
- the cavity may mean an empty space continuous from one region of the outer surface of the hollow metal nanoparticle.
- the cavity of the present specification may be formed in the form of one tunnel from the outer surface of the shell portion to the hollow core in one or more regions of the shell portion.
- the tunnel form may be a straight line, a continuous form of a curve or a straight line, it may be a continuous form of a mixture of curves and straight lines.
- the cavity may be an empty space extending from the outer surface of the shell portion to the hollow.
- the hollow metal nanoparticles may include a hollow region connected to the center of the hollow nanoparticles by at least one surface of the outside by the cavity.
- the cavity of the present specification may serve to utilize the inner surface area of the hollow metal nanoparticles. Specifically, when the hollow metal nanoparticles are used for the purpose of a catalyst or the like, the cavity may serve to increase the surface area in contact with the reactants. Therefore, the cavity may serve to exhibit high activity of the hollow metal nanoparticles.
- the hollow metal nanoparticles of the present disclosure may increase the surface area by 20% to 100% compared to the hollow metal nanoparticles when there is no cavity due to the inclusion of the cavity.
- the diameter of the cavity may be 5% or more and 30% or less of the hollow metal nanoparticle particle diameter.
- the diameter of the cavity is less than 5% of the particle diameter of the hollow metal nanoparticles, the activity of the hollow metal nanoparticles may not be sufficiently exhibited.
- the cavity diameter exceeds 30% of the particle diameter of the hollow metal nanoparticles, the shape of the hollow metal nanoparticles may not be maintained. Therefore, when the diameter of the cavity is 5% or more and 30% or less of the particle diameter of the hollow metal nanoparticles, the contact area with the reactant material through the cavity may be sufficiently widened.
- One embodiment of the present specification is a solvent; A first metal salt which provides a first metal ion or an atomic group ion containing the first metal ion in the solvent; A second metal salt which provides a second metal ion or an atomic group ion containing the second metal ion in the solvent; A first surfactant forming a micelle in the solvent; And forming a solution comprising the second surfactant together with the first surfactant to form a micelle in the solvent; And
- It provides a method for producing metal nanoparticles comprising the step of adding a reducing agent to the solution to form metal nanoparticles.
- the manufacturing method may include forming an inner region of the micelle formed by the first surfactant in a hollow form.
- the method of manufacturing metal nanoparticles according to the exemplary embodiment of the present specification does not use a reduction potential, there is an advantage in that the reduction potential between the first metal ion and the second metal ion forming the shell is not considered. Since the manufacturing method of the present specification uses a charge between metal ions, it is simpler than the manufacturing method of metal nanoparticles using a conventional reduction potential. Therefore, the production method of the metal nanoparticles of the present specification is easy to mass production, it is possible to produce metal nanoparticles at a low cost. Furthermore, since the reduction potential is not used, there is an advantage in that various metal salts can be used because the restriction of the metal salt to be used is reduced as compared with the conventional method for preparing metal nanoparticles.
- the manufacturing method may be one in which a hollow core is formed inside the metal nanoparticle.
- the forming of the solution may include forming the micelle in the solution by the first and second surfactants.
- the manufacturing method may include an atomic group ion including the first metal ion or the first metal ion; And the atomic group ion including the second metal ion or the second metal ion may form a shell portion of the metal nanoparticle.
- the first metal ion or the atomic group ion including the first metal ion has a charge opposite to that of the outer end portion of the first surfactant
- the second metal ion or the first ion Atomic ion, including the bimetallic ion may have a charge equal to that at the outer end of the first surfactant
- the first metal ion or the atomic group ion including the first metal ion may be positioned at an outer end of the first surfactant forming the micelle in a solution to surround the outer surface of the micelle. Furthermore, the atomic group ion including the second metal ion or the second metal ion may have a form surrounding the outer surface of the atomic group ion including the first metal ion or the first metal ion.
- the first metal salt and the second metal salt may form a shell part including the first metal and the second metal, respectively, by a reducing agent.
- the surfactant outer end may refer to the micelle outer part of the first or second surfactant forming the micelle.
- the surfactant outer end of the present specification may mean the head of the surfactant.
- the outer end of the present specification can determine the charge of the surfactant.
- the surfactant herein may be classified as ionic or nonionic according to the type of the outer end, and the ionicity may be positive, negative, zwitterionic or amphoteric.
- the zwitterionic surfactant contains both positive and negative charges. If the positive and negative charge of a surfactant herein is pH dependent, it may be an amphoteric surfactant, which may be zwitterionic in a range of pH.
- the anionic surfactant in the present specification may mean that the outer end of the surfactant is negatively charged, the cationic surfactant may mean that the outer end of the surfactant is positively charged.
- the metal nanoparticles manufactured by the manufacturing method may have a cavity formed in one or two or more regions of the shell portion.
- the cavity of the present specification may mean an empty space continuous from one region of the outer surface of the metal nanoparticle.
- the cavity of the present specification may be formed in the form of a tunnel from one region of the outer surface of the shell portion.
- the tunnel form may be a straight line, a continuous form of a curve or a straight line, it may be a continuous form of a mixture of curves and straight lines.
- the cavity may be an empty space extending from the outer surface of the shell portion to the hollow.
- the preparation method may include a concentration of the second surfactant; Chain length; The size of the outer end; Alternatively, by adjusting the type of charge, a cavity may be formed in one or two or more regions of the shell portion.
- the shell part may mean a region of the nanoparticle including a metal.
- the shell part may mean a region of the metal particles except for the hollow and the cavity.
- the first surfactant may serve to form a micelle in a solution such that the metal ion or the atomic group ion including the metal ion forms a shell portion, and the second surfactant It may serve to form a cavity of the metal nanoparticles.
- the shell portion of the metal nanoparticles is formed in the micelle region formed by the first surfactant, and the metal nanoparticles are formed in the micelle region formed by the second surfactant.
- the cavity may be formed.
- the forming of the solution may include adjusting the size or number of the cavities by varying concentrations of the first and second surfactants.
- the molar concentration of the second surfactant may be 0.01 to 1 times the molar concentration of the first surfactant.
- the molar concentration of the second surfactant may be 1/30 to 1 times the molar concentration of the first surfactant.
- the first surfactant and the second surfactant may form micelles according to the concentration ratio.
- the cavity size or the number of the cavity of the metal nanoparticles may be adjusted.
- the metal nanoparticles including one or more bowl-type particles may be prepared by continuously forming the cavity.
- the forming of the solution may include adjusting the size of the cavity by adjusting the size of the outer end of the second surfactant.
- the forming of the solution may include adjusting the chain length of the second surfactant differently from the chain length of the first surfactant to form a cavity in the second surfactant region. It may include the step.
- the chain length of the second surfactant may be 0.5 to 2 times the chain length of the first surfactant. Specifically, the chain length may be determined by the number of carbons.
- the chain length of the second surfactant is different from the chain length of the first surfactant, so that the metal salt bonded to the outer end of the second surfactant forms the shell portion of the metal nanoparticle. It can be prevented from forming.
- the forming of the solution may include controlling the charge of the second surfactant differently from the charge of the first surfactant to form a cavity.
- a first metal ion or a first metal ion having a charge opposite to the first and second surfactants is formed at the outer ends of the first and second surfactants that form micelles in a solvent.
- Atom containing ion may be located.
- the second metal ion opposite to the charge of the first metal ion may be positioned on an outer surface of the first metal ion.
- the first metal ion and the second metal ion formed at the outer end of the first surfactant may form a shell portion of the metal nanoparticle, and the outer side of the second surfactant
- the first metal ion and the second metal ion positioned at the end may not form the shell and may form a cavity.
- the first surfactant when the first surfactant is an anionic surfactant, in the forming of the solution, the first surfactant forms a micelle, and the micelle is a first metal ion or a first It may be surrounded by cations of atomic monoions including metal ions. Furthermore, atomic monoions including the second metal ion of the anion may surround the cation. Further, in the step of forming a metal nanoparticle by adding a reducing agent, the cation surrounding the micelles may form a first shell, the anion surrounding the cation may form a second shell.
- the first surfactant when the first surfactant is a cationic surfactant, in the forming of the solution, the first surfactant forms a micelle, and the micelle is a first metal ion. It may be surrounded by the anion of the atom containing ion. Further, the atomic monoion including the second metal ion or the second metal ion of the cation may surround the anion. In addition, in the step of forming a metal nanoparticle by adding a reducing agent, the anion surrounding the micelle may form a first shell, the cation surrounding the anion may form a second shell.
- the forming of the metal nanoparticle may include forming the first and second surfactant regions forming the micelle in the hollow.
- both the first surfactant and the second surfactant may be cationic surfactants.
- both the first surfactant and the second surfactant may be an anionic surfactant.
- micelles may be formed by making the chain length of the second surfactant different from the chain length of the first surfactant. Specifically, due to the difference in the chain length of the second surfactant, the first and second metal ions located at the outer end of the second surfactant are positioned at the outer ends of the first surfactant. It is not adjacent to the ions and no shell portion is formed.
- any one of the first surfactant and the second surfactant may be an anionic surfactant, and the other may be a cationic surfactant. That is, in one embodiment of the present specification, the first and second surfactants may have different charges.
- the length of the chain may be different to form a cavity of the metal nanoparticle.
- the principle in which the cavities are formed is the same as when the aforementioned first and second surfactants have the same charge.
- the cavity of the metal nanoparticles may be formed even if the chains of the first and second surfactants have the same length. have.
- the outer end of the first surfactant adjacent to the second end of the second surfactant of the micelle is charged with each other to form a neutral, the metal ion is not located. Therefore, the portion where the metal ion is not located does not form the shell portion, thereby forming the cavity of the metal nanoparticles.
- the first surfactant may be an anionic surfactant or a cationic surfactant
- the second surfactant may be a nonionic surfactant
- the second surfactant when the second surfactant is a nonionic surfactant, since the metal ion is not positioned at the outer end of the second surfactant, the cavity of the metal nanoparticle may be formed. Therefore, when the second surfactant is nonionic, it is possible to form a cavity of the metal nanoparticle even when the length of the chain is the same or different from the first surfactant.
- the first surfactant may be an anionic surfactant or a cationic surfactant
- the second surfactant may be an amphoteric ionic surfactant
- the second surfactant is an amphoteric ionic surfactant
- the metal ion since the metal ion is not located at the outer end of the second surfactant, the cavity of the metal nanoparticle may be formed. . Therefore, when the second surfactant is zwitterionic, it is possible to form a cavity of the metal nanoparticle even when the length of the chain is the same or different from the first surfactant.
- the anionic surfactants herein are ammonium lauryl sulfate, sodium 1-heptanesulfonate, sodium hexanesulfonate, Sodium dodecyl sulfate, triethanol ammonium dodecylbenzene sulfate, potassium laurate, triethanolamine stearate, lithium dodecyl sulfate, sodium lauryl sulfate, alkyl polyoxyethylene sulfate, sodium alginate, dioctyl sodium sulfosuccinate, phosphatidyl Glycerol, phosphatidyl inositol, phosphatidylserine, phosphatidic acid and salts thereof, glyceryl esters, sodium carboxymethylcellulose, bile acids and salts thereof, cholic acid, deoxycholic acid, glycocholic acid, taurocholic acid, glycodeoxycholic acid, alkyl sulfonates , Aryl sul
- the cationic surfactants herein are quaternary ammonium compounds, benzalkonium chloride, cetyltrimethylammonium bromide, chitosan, lauryldimethylbenzylammonium chloride, acyl carnitine hydrochloride, alkylpyridinium halides, cetyl pyridinium chloride , Cationic lipids, polymethylmethacrylate trimethylammonium bromide, sulfonium compounds, polyvinylpyrrolidone-2-dimethylaminoethyl methacrylate dimethyl sulfate, hexadecyltrimethyl ammonium bromide, phosphonium compounds, benzyl-di ( 2-chloroethyl) ethylammonium bromide, coconut trimethyl ammonium chloride, coconut trimethyl ammonium bromide, coconut methyl dihydroxyethyl ammonium chloride, coconut methyl dihydroxyethyl am
- the nonionic surfactants herein are SPAN 60, polyoxyethylene fatty alcohol ethers, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene fatty acid esters, polyoxyethylene alkyl ethers, polyoxyethylene castor oil derivatives, sorbents Non-ester, glyceryl ester, glycerol monostearate, polyethylene glycol, polypropylene glycol, polypropylene glycol ester, cetyl alcohol, cetostearyl alcohol, stearyl alcohol, arylalkyl polyether alcohol, polyoxyethylene polyoxypropylene copolymer , Poloxamer, poloxamine, methylcellulose, hydroxycellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxy propylcellulose, hydroxy propylmethylcellulose, hydroxypropylmethylcellulose phthalate, amorphous cellulose, polysaccharides, starch, I'm It may be selected from a derivative, hydroxyethyl starch, polyvinyl alcohol,
- the zwitterionic surfactants herein are N-dodecyl-N, N-dimethyl-3-ammonio-1-propanesulfonate, betaine, alkyl betaine, alkylamido betaine, amido propyl betaine , Coco ampocarboxyglycinate, sacosinate aminopropionate, aminoglycinate, imidazolinium betaine, zwitteridamidolin, N-alkyl-N, N-dimethylammonio-1-propanesulfone Ate, 3-cholamido-1-propyldimethylammonio-1-propanesulfonate, dodecylphosphocholine and sulfo-betaine.
- the present invention is not limited thereto.
- the concentration of the first surfactant may be at least 1 times and at most 5 times the critical micelle concentration with respect to the solvent. Specifically, the concentration of the first surfactant may be two times the critical micelle concentration with respect to the solvent.
- the critical micelle concentration means a lower limit of the concentration at which the surfactant forms a group of molecules or ions (micro micelles) in a solution.
- the most important property of a surfactant is that the surfactant has a tendency to adsorb on the interface, such as the air-liquid interface, the air-solid interface and the liquid-solid interface. If the surfactants are free in the sense that they do not exist in agglomerated form, they are called monomers or unimers, and as the unimer concentration is increased they aggregate to form the entity of small agglomerates, ie Form micelles. Such concentration may be referred to as critical micelle concentration.
- the concentration of the first surfactant When the concentration of the first surfactant is less than one times the critical micelle concentration, the concentration of the first surfactant adsorbed to the first metal salt may be relatively low. Accordingly, the amount of core particles formed may also be reduced as a whole.
- the concentration of the first surfactant exceeds 5 times the critical micelle concentration, the concentration of the first surfactant is relatively increased so that the metal nanoparticles forming the hollow core and the metal particles not forming the hollow core are mixed and aggregated. Can be. Therefore, when the concentration of the first surfactant is not less than 1 times and not more than 5 times the critical micelle concentration with respect to the solvent, the formation of the metal nanoparticles may be smoothly performed.
- the size of the metal nanoparticles may be controlled by adjusting the first and second metal salts surrounding the first surfactant and / or micelle forming the micelle.
- the size of the metal nanoparticle may be adjusted by the chain length of the first surfactant forming the micelle. Specifically, when the chain length of the first surfactant is short, the size of the micelle is reduced, and thus the size of the metal nanoparticles may be reduced.
- the number of carbon atoms of the chain of the first surfactant may be 15 or less.
- the carbon number of the chain may be 8 or more and 15 or less.
- the carbon number of the chain may be 10 or more and 12 or less.
- the size of the metal nanoparticle may be adjusted by adjusting the type of counter ions of the first surfactant forming the micelle. Specifically, the larger the size of the counter ion of the first surfactant, the weaker the bonding force with the head portion of the outer end of the first surfactant may be the size of the micelle, thereby increasing the size of the metal nanoparticles. .
- the first surfactant when the first surfactant is an anionic surfactant, the first surfactant includes NH 4 + , K + , Na + or Li + as a counter ion. It may be.
- the first surfactant when the counter ion of the first surfactant is NH 4 + , when the counter ion of the first surfactant is K + , when the counter ion of the first surfactant is Na + , the first surfactant
- the size of the metal nanoparticles may be reduced in the order of the counter ion of Li + .
- the first surfactant when the first surfactant is a cationic surfactant, the first surfactant may include I ⁇ , Br ⁇ , or Cl ⁇ as a counter ion.
- the metal nanoparticles in the order of the counter ion of the first surfactant is Cl ⁇
- the size of can be made smaller.
- the size of the metal nanoparticle may be controlled by adjusting the size of the head portion of the outer end of the first surfactant forming the micelle. Furthermore, when the size of the head portion of the first surfactant formed on the outer surface of the micelle is increased, the repulsive force between the head portions of the first surfactant is increased, thereby increasing the micelle, and thus the size of the metal nanoparticles is increased. Can grow.
- the size of the metal nanoparticles may be determined by the complex action of the above-described elements.
- the metal salt is not particularly limited as long as it can be ionized in a solution to provide metal ions.
- the metal salt may be ionized in a solution state to provide an anion of a cation including a metal ion or an atomic monoion including a metal ion.
- the first metal salt and the second metal salt may be different from each other.
- the first metal salt may provide a cation including a metal ion
- the second metal salt may provide an anion of atomic group ions including a metal ion.
- the first metal salt may provide a cation of Ni 2+
- the second metal salt may provide an anion of PtCl 4 2 ⁇ .
- the first metal salt and the second metal salt are not particularly limited as long as they can be ionized in a solution to provide a metal ion or an atomic group ion including a metal ion.
- the first metal salt and the second metal salt are each independently selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to Groups 3 to 15 of the periodic table. It may be a salt of the thing.
- the first metal salt and the second metal salt are different from each other, and each independently, platinum (Pt), ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir) , Rhenium (Re), palladium (Pd), vanadium (V), tungsten (W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn) It may be a salt of a metal selected from the group consisting of Cr (chromium), titanium (Ti), gold (Au), cerium (Ce), silver (Ag) and copper (Cu).
- the first metal salt is ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir), rhenium (Re), palladium ( Pd), vanadium (V), tungsten (W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), chromium (Cr), titanium ( It may be a salt of a metal selected from the group consisting of Ti), cerium (Ce), silver (Ag), and copper (Cu), and more particularly, may be a salt of nickel (Ni).
- the second metal salt is platinum (Pt), ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir), rhenium ( Re), palladium (Pd), vanadium (V), tungsten (W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), chromium ( It may be a salt of a metal selected from the group consisting of Cr), titanium (Ti), gold (Au), cerium (Ce), silver (Ag) and copper (Cu). More specifically, it may be a salt of a metal consisting of platinum (Pt), palladium (Pd) and gold (Au), and even more specifically, may be a salt of platinum (Pt).
- the first metal salt and the second metal salt may each independently be a halide such as nitrate, chloride, bromide, or iodide of a metal.
- Halide such as nitrate, chloride, bromide, or iodide of a metal.
- Halide nitrate, chloride, bromide, or iodide of a metal.
- Halide hydroxide
- sulfur oxides Sulfate
- the molar ratio of the first metal salt and the second metal salt in the forming of the solution may be 1: 5 to 10: 1.
- the molar ratio of the first metal salt and the second metal salt may be 2: 1 to 5: 1.
- the first and second metal ions may smoothly form the shell portion of the metal nanoparticles.
- the shell unit may include a first shell including the first metal ion; And a second shell including the second metal ion.
- an atomic percentage ratio of the first metal and the second metal of the shell part may be 1: 5 to 10: 1.
- the atomic percentage ratio may be an atomic percentage ratio of the first metal of the first shell and the second metal of the second shell when the shell portion is formed of the first shell and the second shell.
- the atomic percentage ratio may be an atomic percentage ratio of the first metal and the second metal when the shell portion is formed of one shell including the first metal and the second metal.
- the forming of the solution may further include adding a stabilizer.
- the stabilizer may be, for example, one or two or more mixtures selected from the group consisting of disodium phosphate, dipotassium phosphate, disodium citrate and trisodium citrate.
- the forming of the metal nanoparticles may include adding a nonionic surfactant together with the reducing agent.
- the nonionic surfactant is adsorbed on the surface of the shell, and serves to uniformly disperse the metal nanoparticles formed in the solution. Therefore, the metal particles are prevented from being agglomerated or precipitated, and the metal nanoparticles can be formed to a uniform size.
- Specific examples of the nonionic surfactant are the same as those of the nonionic surfactant described above.
- the solvent may be a solvent including water.
- the solvent may be water or a mixture of water and an alcohol having 1 to 6 carbon atoms by dissolving the first metal salt and the second metal salt, and more specifically, may be water. . Since the manufacturing method according to the present specification does not use an organic solvent as a solvent, a post-treatment step of treating an organic solvent in a manufacturing process is not required, and thus, there is a cost saving effect and an environmental pollution prevention effect.
- the manufacturing method may be performed at room temperature.
- the temperature may be performed at a temperature in the range of 4 ° C to 35 ° C, more specifically at 12 ° C to 28 ° C.
- Forming the solution in one embodiment of the present specification may be carried out at room temperature, specifically 4 ° C or more and 35 ° C or less, more specifically 12 ° C or more and 28 ° C or less.
- the solvent is an organic solvent, there is a problem that the solvent must be prepared at a high temperature of more than 100 ° C. Since the present application can be manufactured at room temperature, the manufacturing method is simple, there is a process advantage, and the cost reduction effect is large.
- the forming of the solution may be performed for 5 minutes to 120 minutes, more specifically for 10 minutes to 90 minutes, and even more specifically for 20 minutes to 60 minutes.
- the step of forming a metal nanoparticle comprising a cavity for adding a reducing agent and / or a nonionic surfactant to the solution may also be carried out at room temperature, specifically 4 ° C. to 35 ° C., More specifically, it may be performed at 12 ° C. or higher and 28 ° C. or lower. Since the manufacturing method of the present specification can be manufactured at room temperature, the manufacturing method is simple, there are advantages in the process, and the cost reduction effect is large.
- Forming the metal nanoparticles comprising the cavity may react the solution with a reducing agent and / or a nonionic surfactant for a period of time, specifically for 5 to 120 minutes, more specifically for 10 to 90 minutes, even more Specifically, the reaction can be carried out for 20 to 60 minutes.
- the standard reduction potential of the reducing agent may be -0.23V or less.
- the reducing agent is not particularly limited as long as it is a standard reducing agent of -0.23V or less, specifically, -4V or more and -0.23V or less, and has a reducing power capable of reducing dissolved metal ions to precipitate as metal particles.
- the reducing agent may be at least one selected from the group consisting of NaBH 4 , NH 2 NH 2 , LiAlH 4 and LiBEt3H.
- the manufacturing method may further include removing a surfactant inside the hollow after forming the metal nanoparticle including the cavity.
- the removal method is not particularly limited and may be, for example, a method of washing with water.
- the surfactant may be an anionic surfactant and / or a cationic surfactant.
- adding acid to the metal nanoparticles to remove the cationic metal may further include.
- adding acid to the metal nanoparticle when an acid is added to the metal nanoparticle, a 3d band metal is eluted.
- the cationic metal is specifically ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (Os), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten (W) ), Cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), Cr (chromium), titanium (Ti), cerium (Ce), silver (Ag) ) And copper (Cu).
- the acid is not particularly limited, and for example, one selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, perchloric acid, hydroiodic acid and hydrobromic acid may be used.
- the solution including the metal nanoparticles may be centrifuged to precipitate the metal nanoparticles included in the solution. Only metal nanoparticles separated after centrifugation can be recovered. If necessary, the firing process of the metal nanoparticles may be additionally performed.
- metal nanoparticles having a uniform size in the order of several nanometers may be manufactured. Conventional methods have made it difficult to produce nanoscale metal nanoparticles, as well as to produce uniform sizes.
- the metal nanoparticles of the present specification may generally be used to replace existing nanoparticles in the field where nanoparticles may be used. Since the metal nanoparticles of the present specification are very small in size and have a larger specific surface area than the conventional nanoparticles, the metal nanoparticles may exhibit excellent activity as compared to the conventional nanoparticles. Specifically, the metal nanoparticles of the present specification may be used in various fields such as catalysts, drug delivery, gas sensors, and the like. The metal nanoparticles may be used as active substance preparations in cosmetics, pesticides, animal nutrition or food supplements as catalysts, and may also be used as pigments in electronics, optical articles or polymers.
- One embodiment of the present specification provides a catalyst including the hollow metal nanoparticles.
- the first metal salt may be a salt including a first metal ion, which is a precursor of the first metal, or an atomic group ion including the first metal ion, and may serve to provide a first metal.
- the second metal salt is a salt including a second metal ion that is a precursor of the second metal or an atomic group ion including the second metal ion, and may serve to provide a second metal.
- NaBH 4 as a reducing agent and polyvinylpyrrolidone (PVP) as a nonionic surfactant were added and reacted for 30 minutes.
- the supernatant of the upper layer was discarded by centrifugation at 10,000 rpm for 10 minutes, and the remaining precipitate was redispersed in distilled water, followed by repeated centrifugation to prepare hollow metal nanoparticles including the cavity of the present specification.
- the manufacturing process of the metal nanoparticles was carried out in an atmosphere of 14 °C.
- FIGS. 2 and 3 Transmission electron microscope (TEM) images of the hollow metal nanoparticles of the present disclosure prepared according to Example 1 are shown in FIGS. 2 and 3. 3 is an inverted color of FIG. 2. That is, FIG. 2 shows the dark field of the TEM, and FIG. 3 shows the bright field of the TEM.
- the dark field TEM image of the present specification when the electron bunches of the TEM touch the hollow metal nanoparticles, the diffraction occurs at a large mass of the shell, thereby showing a bright image.
- the hollow areas of the nanoparticles show slightly darker images because the electron bunches of the TEM have less diffraction.
- the area with the cavity of the shell part is transmitted through the electron bunches of the TEM as it is, resulting in a black image.
- Ni (NO 3 ) 2 as the first metal salt, K 2 PtCl 4 as the second metal salt, ammonium lauryl sulfate (ALS) as the first surfactant, sodium 1-heptanesulfonate as the second surfactant 1-heptanesulfonate (SHS), trisodium citrate as a stabilizer was added to distilled water to form a solution, and stirred for 30 minutes.
- the molar ratio of K 2 PtCl 4 to Ni (NO 3 ) 2 was 1: 3
- ALS was twice the critical micelle concentration (CMC) for water
- SHS was 1/30 mol of ALS. It was.
- NaBH 4 as a reducing agent and polyvinylpyrrolidone (PVP) as a nonionic surfactant were added and reacted for 30 minutes.
- the supernatant of the upper layer was discarded by centrifugation at 10,000 rpm for 10 minutes, and the remaining precipitate was redispersed in distilled water, followed by repeated centrifugation to prepare hollow metal nanoparticles including the cavity of the present specification.
- the manufacturing process of the metal nanoparticles was carried out in an atmosphere of 14 °C.
- FIGS. 4 and 5 Transmission electron microscope (TEM) images of the hollow metal nanoparticles of the present disclosure prepared according to Example 2 are shown in FIGS. 4 and 5. 5 is an inverted color of FIG. That is, FIG. 4 shows the dark field of the TEM, and FIG. 5 shows the bright field of the TEM.
- Trisodium citrate was added to distilled water as a stabilizer to form a solution and stirred for 30 minutes.
- the molar ratio of K 2 PtCl 4 and Ni (NO 3 ) 2 was 1: 3
- ALS was twice the critical micelle concentration (CMC) to water
- sodium hexanesulfonate was 1 / A of ALS. 30 moles.
- NaBH 4 as a reducing agent and polyvinylpyrrolidone (PVP) as a nonionic surfactant were added and reacted for 30 minutes.
- the supernatant of the upper layer was discarded by centrifugation at 10,000 rpm for 10 minutes, and the remaining precipitate was redispersed in distilled water, followed by repeated centrifugation to prepare hollow metal nanoparticles including the cavity of the present specification.
- the manufacturing process of the metal nanoparticles was carried out in an atmosphere of 14 °C.
- FIG. 6 and 7 show transmission electron microscope (TEM) images of hollow metal nanoparticles of the present disclosure prepared according to Example 3.
- FIG. 7 is an inverted color of FIG. 6. That is, FIG. 6 shows the dark field of the TEM, and FIG. 7 shows the bright field of the TEM.
- K 2 PtCl 4 as the second metal salt
- sodium dodecyl sulfate (SDS) as the first surfactant
- N-dodecyl-N, N as the second surfactant -Dimethyl-3-ammonio-1-propanesulfonate
- DDAPS dimethyl-3-ammonio-1-propane sulfonate
- trisodium citrate as a stabilizer added to distilled water
- the solution was formed and stirred for 30 minutes.
- the molar ratio of K 2 PtCl 4 to Ni (NO 3 ) 2 was 1: 3
- ALS was twice the critical micelle concentration (CMC) for water
- DDAPS was 1/30 mol of SDS. It was.
- NaBH 4 as a reducing agent and polyvinylpyrrolidone (PVP) as a nonionic surfactant were added and reacted for 30 minutes.
- the supernatant of the upper layer was discarded by centrifugation at 10,000 rpm for 10 minutes, and the remaining precipitate was redispersed in distilled water, followed by repeated centrifugation to prepare hollow metal nanoparticles including the cavity of the present specification.
- the manufacturing process of the metal nanoparticles was carried out in an atmosphere of 14 °C.
- FIGS. 8 and 9 Transmission electron microscope (TEM) images of the hollow metal nanoparticles of the present specification prepared according to Example 4 are shown in FIGS. 8 and 9.
- FIG. 9 is an inverted color of FIG. 8. That is, FIG. 8 shows the dark field of the TEM, and FIG. 9 shows the bright field of the TEM.
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Abstract
Description
Claims (20)
- 중공 코어(core)부;제1 금속 및 제2 금속을 포함하는 쉘(shell)부; 및상기 쉘부의 1 또는 2 이상의 영역에 쉘부 외면으로부터 상기 중공 코어에 이르는 공동(cavity)을 포함하는 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자는 상기 공동을 1개 포함하는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자의 입경은 1 ㎚ 이상 30 ㎚ 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자의 입경은 1 ㎚ 이상 20 ㎚ 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자의 입경은 1 ㎚ 이상 12 ㎚ 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자의 입경은 1 ㎚ 이상 6 ㎚ 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자는 구 형상인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 공동의 직경은 상기 중공 금속 나노입자 입경의 5 % 이상 30 % 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 쉘부의 두께는 0 ㎚ 초과 5 ㎚ 이하인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 금속 나노입자의 입경은 중공 금속 나노입자들의 평균 입경의 80% 내지 120% 범위 이내인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공 코어는 상기 중공 금속 나노입자의 50 부피% 이상인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 중공은 계면활성제가 포함되어 있는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 쉘부의 제1 금속과 제2 금속의 원자 백분율 비는 1:5 내지 10:1인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 쉘부는 상기 제1 금속을 포함하는 제1 쉘; 및 상기 제2 금속을 포함하는 제2 쉘을 포함하는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 쉘부는 상기 제 1 금속의 함량이 상기 제2 금속의 함량보다 높은 제1 쉘; 및 상기 제2 금속의 함량이 상기 제1 금속의 함량보다 높은 제2 쉘을 포함하는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 제1 금속 및 상기 제2 금속은 각각 독립적으로,주기율표상 3 ~ 15족에 속하는 금속, 준금속(metalloid), 란타늄족 금속 및 악티늄족 금속으로 이루어진 군에서 선택되는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 제1 금속 및 상기 제2 금속은 각각 독립적으로,백금(Pt); 루테늄(Ru); 로듐(Rh); 몰리브덴(Mo); 오스뮴(Os); 이리듐(Ir); 레늄(Re); 팔라듐(Pd); 바나듐(V); 텅스텐(W); 코발트(Co); 철(Fe); 셀레늄(Se); 니켈(Ni); 비스무트(Bi); 주석(Sn); 크롬(Cr); 타이타늄(Ti); 금(Au); 세륨(Ce); 은(Ag); 및 구리(Cu)로 이루어진 군에서 선택되는 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 제1 금속 또는 상기 제2 금속은 서로 상이하며, 상기 제1 금속 또는 상기 제2 금속은 니켈인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 제1 금속 또는 상기 제2 금속은 서로 상이하며, 상기 제1 금속 또는 상기 제2 금속은 백금인 것인 중공 금속 나노입자.
- 청구항 1에 있어서,상기 제1 금속은 니켈이고, 상기 제2 금속은 백금인 것인 중공 금속 나노입자.
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CN201480032619.9A CN105307799B (zh) | 2013-06-07 | 2014-06-03 | 中空金属纳米粒子 |
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KR102432090B1 (ko) * | 2018-06-08 | 2022-08-12 | 한국과학기술연구원 | 비정질 나노구조체를 이용하여 제조된 초소형 나노구조체 및 이의 제조방법 |
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Also Published As
Publication number | Publication date |
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KR101858304B1 (ko) | 2018-05-16 |
EP2990138A4 (en) | 2017-01-11 |
US20160107147A1 (en) | 2016-04-21 |
US9776173B2 (en) | 2017-10-03 |
CN105307799A (zh) | 2016-02-03 |
CN105307799B (zh) | 2018-02-02 |
KR20140143713A (ko) | 2014-12-17 |
JP2016526108A (ja) | 2016-09-01 |
EP2990138A1 (en) | 2016-03-02 |
EP2990138B1 (en) | 2021-03-03 |
JP6191764B2 (ja) | 2017-09-06 |
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