CN108883946A - 氧化锆纳米粒子 - Google Patents
氧化锆纳米粒子 Download PDFInfo
- Publication number
- CN108883946A CN108883946A CN201780019378.8A CN201780019378A CN108883946A CN 108883946 A CN108883946 A CN 108883946A CN 201780019378 A CN201780019378 A CN 201780019378A CN 108883946 A CN108883946 A CN 108883946A
- Authority
- CN
- China
- Prior art keywords
- zirconium oxide
- particle
- oxide nano
- acid
- atom
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 144
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 141
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 42
- 150000001875 compounds Chemical class 0.000 claims abstract description 42
- 239000006185 dispersion Substances 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 20
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005253 cladding Methods 0.000 claims abstract description 17
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 14
- 125000004429 atom Chemical group 0.000 claims abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 8
- 125000005843 halogen group Chemical group 0.000 claims abstract description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract 8
- 239000013078 crystal Substances 0.000 claims description 59
- 229920005989 resin Polymers 0.000 claims description 42
- 239000011347 resin Substances 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 41
- 229910052726 zirconium Inorganic materials 0.000 claims description 37
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 235000019441 ethanol Nutrition 0.000 claims description 25
- 239000002904 solvent Substances 0.000 claims description 22
- 239000000178 monomer Substances 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 12
- 229910010293 ceramic material Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims 1
- 239000002798 polar solvent Substances 0.000 abstract description 12
- 230000002349 favourable effect Effects 0.000 abstract description 9
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 70
- -1 sulphur Alcohol radical Chemical class 0.000 description 40
- 239000002245 particle Substances 0.000 description 31
- 150000001721 carbon Chemical group 0.000 description 30
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 28
- 239000002253 acid Substances 0.000 description 25
- 238000001027 hydrothermal synthesis Methods 0.000 description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 229910052761 rare earth metal Inorganic materials 0.000 description 19
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000002585 base Substances 0.000 description 15
- 239000003960 organic solvent Substances 0.000 description 15
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 14
- 150000003839 salts Chemical class 0.000 description 13
- 239000004615 ingredient Substances 0.000 description 12
- 229910052809 inorganic oxide Inorganic materials 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000010408 film Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 10
- 150000007942 carboxylates Chemical class 0.000 description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 150000002148 esters Chemical class 0.000 description 9
- YZGQDNOIGFBYKF-UHFFFAOYSA-N Ethoxyacetic acid Chemical compound CCOCC(O)=O YZGQDNOIGFBYKF-UHFFFAOYSA-N 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 150000004706 metal oxides Chemical class 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- RMIODHQZRUFFFF-UHFFFAOYSA-N methoxyacetic acid Chemical compound COCC(O)=O RMIODHQZRUFFFF-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 150000001298 alcohols Chemical class 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- GTCAXTIRRLKXRU-UHFFFAOYSA-N methyl carbamate Chemical compound COC(N)=O GTCAXTIRRLKXRU-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 235000019198 oils Nutrition 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 6
- 229910052727 yttrium Inorganic materials 0.000 description 6
- HBHXRPHNNKAWQL-UHFFFAOYSA-N 2-ethylhexanoic acid;zirconium Chemical compound [Zr].CCCCC(CC)C(O)=O HBHXRPHNNKAWQL-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000011164 primary particle Substances 0.000 description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- IAQRGUVFOMOMEM-UHFFFAOYSA-N but-2-ene Chemical group CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 4
- 229940068984 polyvinyl alcohol Drugs 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 3
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- 229910021529 ammonia Inorganic materials 0.000 description 3
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- 238000004364 calculation method Methods 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 3
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- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000012454 non-polar solvent Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 3
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 3
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- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- OVBFMEVBMNZIBR-UHFFFAOYSA-N 2-methylvaleric acid Chemical compound CCCC(C)C(O)=O OVBFMEVBMNZIBR-UHFFFAOYSA-N 0.000 description 2
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- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
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- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/64—Burning or sintering processes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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Abstract
本发明的目的是提供对极性溶剂的分散性良好,并且可以提高分散液中的核浓度的氧化锆纳米粒子。本发明涉及的氧化锆纳米粒子,其特征在于,用选自R1‑COOH、(R1O)3‑n‑P(O)‑(OH)n、(R1)3‑n‑P(O)‑(OH)n、(R1O)‑S(O)(O)‑(OH)、R1‑S(O)(O)‑(OH)、(R1)4‑m‑Si(R4)m中的1种以上的化合物包覆。式中,R1表示含有选自氧原子、氮原子和硫原子中的1种以上的元素和碳原子,R1中的碳原子、氧原子、氮原子和硫原子的总原子数为8以下的基团;R4为卤原子或‑OR2,R2表示氢原子或烷基;n表示1或2,m表示1‑3的整数。
Description
技术领域
本发明涉及氧化锆纳米粒子。
背景技术
近年,金属氧化物的纳米粒子具有在光学材料、电子零件材料等中发挥各种功能的可能性,在各种功能材料领域引起关注。然而,由于单独的金属氧化物对有机介质的分散性不充分,因此在许多情况下发生凝聚,导致透明度降低和机械强度降低等的问题。为了赋予对有机介质良好的分散性,提出了将有机基团化学键合到金属氧化物上的方法。
例如,专利文献1中记载了通过2种以上的包覆剂包覆的氧化锆纳米粒子,该包覆剂中的至少1种为式R-COOH(R为碳原子数6以上的烃基)表示的包覆剤,这样的氧化锆纳米粒子,对于非极性溶剂等能够改善分散性。
另一方面,由于氧化锆纳米粒子分散液的使用例范围广,作为树脂基板使用聚碳酸酯时,甲基乙基酮等具有侵蚀性的非极性溶剂是不优选的,而要求使用水、乙醇等极性溶剂作为分散介质的分散液。另外,伴随着光学材料、电子零件材料等要求的物性的变化,使用比以往极性更高的光学材料的单体,并且要求氧化锆纳米粒子本身分散在极性溶剂中。特别是形成层压膜时,为了根据溶剂的极性而调控均匀的层压膜,强烈期望氧化锆纳米粒子的分散性调控。然而,在专利文献1中没有使用代表性的极性溶剂甲醇的实施例,并且对水、乙醇等更具极性的溶剂氧化锆纳米粒子的分散性不充分。进而,这些氧化锆纳米粒子即使能够分散在非极性溶剂中,分散液中的金属氧化物浓度(核浓度;通过式(A)算出的浓度)也存在上限,期望可以更高浓度分散的氧化锆纳米粒子。
现有技术文献
专利文献
专利文献1:日本特开2008-44835号公报
发明内容
本发明的目的是提供对极性溶剂的分散性良好,并且可以提高分散液中的核浓度的氧化锆纳米粒子。
解決上述课题的本发明具有以下要点。
[1]一种氧化锆纳米粒子,其特征在于,用选自R1-COOH、(R1O)3-n-P(O)-(OH)n、(R1)3-n-P(O)-(OH)n、(R1O)-S(O)(O)-(OH)、R1-S(O)(O)-(OH)、(R1)4-m-Si(R4)m中的1种以上的化合物包覆。
〔式中,
R1表示含有选自氧原子、氮原子和硫原子中的1种以上的元素和碳原子,R1中的碳原子、氧原子、氮原子和硫原子的总原子数为8以下的基团。
R4为卤原子或-OR2,R2表示氢原子或烷基。
n表示1或2,m表示1-3的整数。〕
[2]根据[1]所述的氧化锆纳米粒子,其中,R1中,相对于碳原子数的氧原子、氮原子和硫原子的和的比(氧原子、氮原子和硫原子的和/碳原子数)为1/7以上且1/1以下。
[3]根据[1]或[2]所述的氧化锆纳米粒子,其中,所述化合物中,相对于碳原子数的氧原子数的比(氧原子数/碳原子数)为大于1/6且1/0.2以下。
[4]根据[1]-[3]中任意一项所述的氧化锆纳米粒子,其中,正方晶和立方晶的合计为晶体结构总体的60%以上。
[5]根据[1]-[4]中任意一项所述的氧化锆纳米粒子,其中,所述氧化锆纳米粒子的平均粒径为1-100nm。
[6]根据[1]-[5]中任意一项所述的氧化锆纳米粒子,其中,对于乙醇的R1的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且20(MPa)1/2以下。
[7]根据[1]-[5]中任意一项所述的氧化锆纳米粒子,其中,对于水的R1的汉森溶解度参数(HSP)距离为20(MPa)1/2以上且41(MPa)1/2以下。
[8]一种分散液,其含有[1]-[7]中任意一项所述的氧化锆纳米粒子。
[9]根据[8]所述的分散液,其中,该分散液含有对于水的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且40(MPa)1/2以下的溶剂。
[10]一种树脂组合物,其含有[1]-[7]中任意一项所述的氧化锆纳米粒子。
[11]根据[10]所述的树脂组合物,其中,所述树脂组合物含有选自单体、低聚物以及聚合物中的至少1种以上的树脂成分。
[12]根据[10]或[11]所述的树脂组合物,其中,该树脂组合物含有对于水的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且40(MPa)1/2以下的溶剂。
[13]一种成型材料,其含有[1]-[7]中任意一项所述的氧化锆纳米粒子。
[14]一种陶瓷材料,其由[1]-[7]中任意一项所述的氧化锆纳米粒子得到。
[15]一种陶瓷材料的制备方法,其特征在于,将[1]-[7]中任意一项所述的氧化锆纳米粒子在500℃以上进行焙烧。
[16]一种陶瓷材料的制备方法,其特征在于,将含有[1]-[7]中任意一项所述的氧化锆纳米粒子的组合物在500℃以上进行焙烧。
根据本发明,由于氧化锆纳米粒子用特定的基团R1包覆,从而能够得到对水、醇等的极性溶剂的分散性良好,并且可以提高分散液中的核浓度的氧化锆纳米粒子。
具体实施方式
本发明的氧化锆纳米粒子,由于用选自具有基团R1的R1-COOH、(R1O)3-n-P(O)-(OH)n、(R1)3-n-P(O)-(OH)n、(R1O)-S(O)(O)-(OH)、R1-S(O)(O)-(OH)、(R1)4-m-Si(R4)m的化合物(以下,有单以“化合物(1)”统称的情况)包覆,对水、醇等的极性溶剂的分散性提高,制备层压膜时,可以根据溶剂的极性形成膜。另外,可以提高分散液中的核浓度,可以扩大膜形成中使用的溶剂的选择范围。
因此本发明中,通过使R1中含有的碳原子、氧原子、氮原子和硫原子的总原子数为8以下,可以使化合物(1)的分子量变小,从而能够相对提高在氧化锆纳米粒子中氧化锆成分所占的比例(质量%)。由此,可以更强力地发挥氧化锆纳米粒子的性能,例如,由含有本发明的氧化锆纳米粒子的树脂组合物,能够制备更高折射率的涂膜。R1中含有的碳原子、氧原子、氮原子和硫原子的总原子数的下限为2以上,更优选为7以下,进一步优选为5以下,更进一步优选为4以下,特别优选为3以下。为了提高氧化锆纳米粒子的金属氧化物浓度,优选R1中含有的碳原子、氧原子、氮原子和硫原子的总原子数越少越好。
R1的特性,可以利用汉森溶解度参数(HSP)进行评价。汉森溶解度参数(HSP)是用于物质的溶解度预测的值。HSP由分子间的分散力引起的能量(D)、分子间的偶极相互作用引起的能量(P)、以及分子间氢键引起的能量(H)这三个参数组成。这三个参数可以视为三维空间中的坐标。因此将两种物质(物质1和物质2)的HSP置于三维空间中时,距离越近,表明二者越容易相互溶解。HSP间的距离R3由以下式子给出。
(R3)2=4*(D1-D2)2+(P1-P2)2+(H1-H2)2
〔式中,D1、P1、H1为物质1的HSP参数,D2、P2、H2为物质2的HSP参数。〕
对于乙醇的R1的HSP距离,优选为0(MPa)1/2以上,更优选为5(MPa)1/2以上,进一步优选为10(MPa)1/2以上,优选为20(MPa)1/2以下,更优选为18(MPa)1/2以下,进一步优选为17(MPa)1/2以下。通过将HSP距离调整至所述范围内,可以提高氧化锆纳米粒子对醇类等的极性溶剂的分散性。
对于水的R1的HSP距离,优选为20(MPa)1/2以上,更优选为25(MPa)1/2以上,进一步优选为30(MPa)1/2以上,优选为41(MPa)1/2以下,更优选为39(MPa)1/2以下,进一步优选为38(MPa)1/2以下。通过将对于水的R1的HSP距离调整在所述范围内,可以提高氧化锆纳米粒子对水等的极性溶剂的分散性。
为了提高氧化锆纳米粒子的分散性,R1中,相对于碳原子数的氧原子、氮原子和硫原子的和的比(氧原子、氮原子和硫原子的和/碳原子数),优选为1/7以上,更优选为1/5以上,进一步优选为1/3以上,优选为1/1以下,更优选为1/1.3以下,进一步优选为1/1.6以下。
另外,R1中,相对于碳原子数的氧原子数的原子数的比(氧原子数/碳原子数)优选为1/7以上,更优选为1/5以上,进一步优选为1/3以上,优选为1/1以下,更优选为1/1.3以下,进一步优选为1/1.6以下。为了提高R1的亲水性,相对于R1中的碳原子存在一定比率以上的氧原子,有助于提高氧化锆纳米粒子对极性溶剂的分散性。
R1例如为烃基,优选为构成烃基的一部分元素被选自氧原子、氮原子和硫原子中的1种以上的元素取代的基团。作为所述烃基包含的元素的取代基,例如,可举出:醚键、羰基、硫酮基、硫醚键、亚砜基、氨基甲酰基、>NH基、>N-基等的取代碳原子的基团;羟基、硫醇基、-NH2基、羧基、氰基、脲基、异氰酸酯基等的取代氢原子的基团等,优选为醚键、羟基或-NH2基,更优选为醚键。
作为R1的烃基,可举出链式烃基、环式烃基,优选为链式烃基。
链式烃基优选为饱和或不饱和的任意一种,更优选为饱和。另外,链式烃基优选为直链状或支链状的任意一种,更优选为直链状。链式烃基优选为饱和链式烃基,更优选为直链状的饱和链式烃基。
环式烃基优选为饱和或不饱和的任意一种。
R1优选含有氧原子,更优选为由氢原子、碳原子以及氧原子构成的基团。
所述化合物(1)具有R1-C,R1-O,R1-P,R1-S以及R1-Si中任意一种的部分结构,该R1-部中的R1的键末端,优选为碳原子。R1的键末端的碳原子,优选为式(A-1)~式(A-4)(式中,单键相当于所述R1-部的键),更优选为式(A-1)。此外,式(A-4)中,一个单键和双键可以是作为共振结构的一个实施方式的键。因而,式(A-4)中的一个单键和双键也可以包含成为芳香环的一部分的情况。
【化1】
所述化合物(1)中,相对于碳原子数的氧原子数的比(氧原子数/碳原子数)优选为大于1/6,更优选为1/2以上,进一步优选为1/1.4以上,优选为1/0.2以下,更优选为1/0.8以下,进一步优选为1/0.9以下。相对于化合物(1)中的碳原子存在一定比率以上的氧原子,有助于提高在极性溶剂中的氧化锆纳米粒子的含量。
作为R1-COOH,可举出甲氧基乙酸、乙氧基乙酸、3-乙氧基丙酸,2-甲氧基乙氧基乙酸等的含醚键的羧酸;乙醛酸、丙酮酸、乙酰丙酸、2-氧代戊酸、天冬酰胺、谷氨酰胺、β-甲基乙酰丙酸、α-甲基乙酰丙酸等的含有羰基的羧酸;甲硫氨酸等的含硫醚键的羧酸;乙醇酸、DL-乳酸、2-羟基异丁酸、二羟甲基丙酸、羟基新戊酸、3-羟基丙酸、DL-2-羟基丁酸、DL-3-羟基丁酸、2-羟基-2-甲基丁酸、β-羟基异戊酸、2,2-双(羟甲基)丁酸、丝氨酸、苏氨酸、4-羟基环己烷羧酸、(o-、m-、p-)羟基安息香酸等的含羟基羧酸;巯基乙酸、硫代乳酸、半胱氨酸等的含巯基羧酸;甘氨酸、丙氨酸、2-甲基丙氨酸、半胱氨酸、丝氨酸、苏氨酸、缬氨酸、亮氨酸、异亮氨酸、甲硫氨酸、赖氨酸等的含-NH2基羧酸;天冬酰胺、谷氨酰胺等的含氨基甲酰基羧酸;天冬氨酸、谷氨酸等的二羧酸;氰基乙酸等的含氰基羧酸;脯氨酸等的羧基取代杂环式化合物等。
作为(R1O)3-n-P(O)-(OH)n或(R1)3-n-P(O)-(OH)n,可例示出磷酸甲氧基甲酯、磷酸二(甲氧基甲基酯)、DL-甘油醛-3-磷酸、磷酸甘油酯等。
作为(R1O)-S(O)(O)-(OH)或R1-S(O)(O)-(OH),可例示出硫酸甲氧基甲酯、L-丝氨酸-O-硫酸钾盐等。
(R1)4-m-Si(R4)m中,R4为卤原子时,R4优选为氯原子,可例示出甲氧基甲基三氯硅烷、甲氧基乙基三氯硅烷、(3-氨基丙基)三氯硅烷、(3-巯基丙基)三氯硅烷、2-氰基乙基三氯硅烷、[3-(N,N-二甲基氨基)丙基]三氯硅烷、3-(甲基氨基)丙基三氯硅烷、3-氰基丙基三氯硅烷、(3-脲基丙基)三氯硅烷、(3-异氰酸基丙基)三氯硅烷、3-(2-氨基乙基氨基)丙基三氯硅烷、[3-(三氯硅烷基)丙基]氨基甲酸甲酯等。
(R1)4-m-Si(R4)m中,R4为OR2时,R2为氢原子或烷基,R2优选为氢原子或碳原子数1-6(特别是1-4)的烷基,R2更优选为碳原子数1-4的烷基(特别是甲基或乙基)。R2为烷基时,作为(R1)4-m-Si(OR2)m,可例示出甲氧基甲基三甲氧基硅烷、甲氧基乙基三乙氧基硅烷、(3-氨基丙基)三甲氧基硅烷、(3-巯基丙基)三甲氧基硅烷、2-氨基乙基三乙氧基硅烷、[3-(N,N-二甲基氨基)丙基]三甲氧基硅烷、3-(甲基氨基)丙基三甲氧基硅烷、3-氰基丙基三甲氧基硅烷、(3-脲基丙基)三甲氧基硅烷、(3-异氰酸基丙基)三乙氧基硅烷、3-(2-氨基乙基氨基)丙基三甲氧基硅烷、[3-(三甲氧基硅烷)丙基]氨基甲酸甲酯等。
m优选为2或3,更优选为3。R2为氢原子时,作为(R1)4-m-Si(OR2)m,可例示出甲氧基甲基三羟基硅烷、甲氧基乙基三羟基硅烷、(3-氨基丙基)三羟基硅烷、(3-巯基丙基)三羟基硅烷、2-氨基乙基三羟基硅烷、[3-(N,N-二甲基氨基)丙基]三羟基硅烷、3-(甲基氨基)丙基三羟基硅烷、3-氰基丙基三羟基硅烷、(3-脲基丙基)三羟基硅烷、(3-异氰酸基丙基)三羟基硅烷、3-(2-氨基乙基巯基)丙基三羟基硅烷、[3-(三羟基硅烷)丙基]氨基甲酸甲酯等。
(R1)4-m-Si(R4)m所示的化合物优选不为四乙氧基硅烷,更优选不为四烷氧基硅烷。
作为包覆氧化锆纳米粒子的化合物,优选为R1-COOH,更优选为含醚键的羧酸,进一步优选为甲氧基乙酸、乙氧基乙酸、3-乙氧基丙酸或2-甲氧基乙氧基乙酸,特别优选为甲氧基乙酸或乙氧基乙酸。
在氧化锆纳米粒子中,化合物(1)的量为5-35质量%(优选为8质量%以上,更优选为10质量%以上,优选为33质量%以下,更优选为30质量%以下)。
此外,氧化锆纳米粒子用化合物(1)包覆,是指包括化合物(1)与氧化锆纳米粒子键合的状态和物理结合的状态中的任意一种,化合物(1)为羧酸时,例如,是指用化合物(1)和/或来自化合物(1)的羧酸酯包覆。
氧化锆纳米粒子可以用化合物(1)以外的第二化合物包覆。作为第二化合物,例如,可举出混入化合物(1)的原料的羧酸(但是,化合物(1)除外;以下也称为“羧酸(2)”)。在不阻碍化合物(1)的包覆效果的程度下,第二化合物也可以包含于氧化锆粒子中,氧化锆纳米粒子中,第二化合物的量优选为30质量%以下,更优选为10质量%以下,进一步优选为5质量%以下。
羧酸(2)优选为碳原子数3-22(优选为4-20)的羧酸,羧酸(2)可以含有伯羧酸、仲羧酸和叔羧酸中的任意一种。
作为伯羧酸,优选为碳原子数4-20的直链状伯羧酸、碳原子数4-20的支链状伯羧酸(即,α位以外的碳原子为分支的羧酸)。直链状羧酸优选为直链状饱和脂肪族羧酸,具体包括丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、月桂酸、十四烷酸、硬脂酸、油酸、蓖麻油酸等。作为支链状伯羧酸,可举出异戊酸、3,3-二甲基丁酸、3-甲基戊酸、异壬酸、4-甲基戊酸、4-甲基正辛酸、环烷酸等。
作为仲羧酸,优选为碳原子数4-20的仲羧酸,具体可举出异丁酸、2-甲基丁酸、2-乙基丁酸、2-乙基己酸、2-甲基戊酸、2-甲基己酸、2-甲基庚酸、2-丙基丁酸、2-己基戊酸、2-己基癸酸、2-庚基十一烷酸、2-甲基十六烷酸、4-甲基环己烷羧酸等,优选为2-乙基己酸、2-己基癸酸的1种以上,特别优选为2-乙基己酸。
作为叔羧酸,优选为碳原子数5-20的叔羧酸,具体可举出新戊酸、2,2-二甲基丁酸、2,2-二甲基戊酸、2,2-二甲基己酸、2,2-二甲基庚酸、新癸酸等。
氧化锆纳米粒子主要由锆构成,为了稳定氧化锆晶体中的晶体结构,还可以包含选自Al和稀土类元素中的至少1种以上。含有这些金属的氧化锆纳米粒子,粒子中的正方晶和/或立方晶的比例变高的同时,能够抑制焙烧氧化锆纳米粒子时的正方晶的减少,提高焙烧后的正方晶的比例。稀土类元素包括Sc(钪)、Y(钇)、原子序数57(La)~原子序数71(Lu)的镧系元素。
在Al和稀土类元素中,优选为选自Al、Y、La、Yb、Sc、Ce和Er中的至少一种以上,更优选为选自Al、Y、Sc和Er中的至少一种以上。
含有Al和稀土类元素的情况下,在氧化锆的锆、Al以及稀土类元素的合计100质量%中,优选含有0-20质量%,更优选含有3-20质量%,进一步优选含有5-20质量%。
此外,氧化锆纳米粒子中,可以含有锆、Al和稀土类元素以外的金属元素,在氧化锆纳米粒子所含的总金属元素中,本发明的纳米粒子所含的锆的含有率优选为60质量%以上,更优选为70质量%以上,进一步优选为80质量%以上。另外,除此以外的金属元素的含有率越少越优选,在纳米粒子所含的总金属元素中,除锆、Al、稀土类元素以及作为锆的杂质通常含有的铪以外的金属元素的含有率,优选为3质量%以下,更优选为1质量%以下,也可以为0质量%。
氧化锆纳米粒子的晶体结构为立方晶、正方晶、单斜晶,正方晶和立方晶的合计优选为晶体结构总体的60%以上。正方晶和立方晶的合计比例优选为70%以上,更优选为80%以上。特别是,氧化锆纳米粒子含有Al或稀土类元素时,由于正方晶和/或立方晶稳定,纳米粒子中的正方晶和/或立方晶的比例也容易提高。另外,氧化锆纳米粒子含有Al或稀土类元素时,焙烧后也容易维持正方晶和/或立方晶。
作为氧化锆纳米粒子的形状,可举出球状、粒状、椭圆球状、立方体状、长方体状、锥状、针状、柱状、棒状、筒状、鳞片状、板状、薄片状等。考虑到对溶剂等的分散性,作为所述形状,优选为球状、粒状、柱状等。
通过X射线衍射分析算出的氧化锆纳米粒子的正方晶和/或立方晶的晶粒直径优选为30nm以下,更优选为20nm以下。通过这样,能够提高含有氧化锆纳米粒子的组合物的透明率。该晶粒直径更优选为20nm以下,进一步优选为15nm以下。该晶粒直径的下限通常为1nm左右。
氧化锆纳米粒子的粒径能够通过处理各种电子显微镜得到的图像而得到的平均粒径进行评价,该平均粒径(平均一次粒径)优选为100nm以下,更优选为50nm以下,进一步优选为30nm以下,下限没有特别的限定,通常为1nm。通过将平均粒径调整至所述范围内,能够提高含有氧化锆纳米粒子的组合物的透明性。
所述平均粒径可以通过用透射型电子显微镜(TEM)、场发射型透射电子显微镜(FE-TEM)、场发射型扫描电子显微镜(FE-SEM)等将氧化锆纳米粒子放大,任意选取100个粒子测定其长轴方向的长度,并求出其算术平均而确定。
氧化锆纳米粒子通过将含氧化锆的粒子与化合物(1)接触而制备。接触温度优选为0-120℃,更优选为10-100℃,进一步优选为20-80℃。另外,与化合物(1)接触时,含氧化锆的粒子可以分散或溶解在有机溶剂中,作为所述有机溶剂,可例示出后述的水热反应中使用的溶剂。
含氧化锆的粒子通过将锆成分、羧酸(2)、根据需要使用的Al或稀土类元素成分进行水热反应而制备。作为所述锆成分,可以使用由羧酸(2)与锆或含锆的化合物构成(优选为结合体)的锆原料物质。另外,合成含有Al或稀土类元素成分的纳米粒子时,可以使用由羧酸(2)和选自Al、稀土类元素、含Al的化合物以及含稀土类元素的化合物中的至少1种构成(优选为结合体)的Al或稀土类元素原料物质。
作为锆原料物质,具体可举出选自(i)羧酸(2)和氧化锆前驱体的盐、(ii)羧酸(2)的锆盐、以及(iii)羧酸(2)和氧化锆前驱体,中的至少1种以上。
作为所述的氧化锆前驱体,例如包含锆的氢氧化物、氯化物,氯氧化物、醋酸盐、氧乙酸盐、氧硝酸盐、硫酸盐、碳酸盐、烷氧化物等。即为氢氧化锆、氯化锆、氯氧化锆、醋酸锆、氧乙酸锆、硝酸氧锆、硫酸锆、碳酸锆和四丁氧基锆等的锆烷氧化物等。
以下,针对(i)的情况进行详述。此外,盐不仅指羧酸(2)和氧化锆前驱体以化学计量比构成的单种类的化合物,也可以为复合盐、存在有未反应的羧酸(2)或氧化锆前驱体的组合物。
所述(i)中,羧酸(2)和氧化锆前驱体的盐,优选为通过来自将中和度调整为0.1-0.8(更优选为0.2-0.7)的范围内的羧酸(2)的含羧酸盐组合物,与氧化锆前驱体反应而得到的羧酸(2)和锆的盐。所述中和度不满0.1时,由于羧酸(2)化合物的溶解性低,可能不能充分形成所述盐,而超过0.8时,生成推测是锆的氢氧化物的大量白色沉淀,包覆型氧化锆粒子的收率可能降低。中和度优选通过碱金属和/或碱土类金属进行调整,优选为形成高水溶性的盐的碱金属,特别是钠以及钾。
所述含羧酸盐组合物与所述氧化锆前驱体的比例,相对于氧化锆前驱体1摩尔,羧基优选为1摩尔~20摩尔,更优选为1.2-18摩尔,进一步优选为1.5-15摩尔。
将所述含羧酸盐组合物与所述氧化锆前驱体反应时,优选将水溶液之间或水溶液与有机溶剂混合。反应温度只要是水溶液能够保持的温度即可,优选为室温至100℃,更优选为40℃-80℃。
将所述含羧酸盐组合物与所述氧化锆前驱体反应得到的所述盐,虽然可以直接供给水热反应,但优选通过过滤、分液等将不溶性副产物除去。
接下来,针对(ii)的情况进行详细说明。
(ii)的实施方式中,使用预先调制的羧酸(2)的锆盐。其优点是可以不需经过上述各种烦杂的工序,而供给水热反应。但是,由于能够容易获得的化合物有限,可能不能得到作为目标的的有机基团包覆的氧化锆粒子。
作为用(ii)的实施方式得到的锆盐,可以例示出辛酸锆、2-乙基己酸锆、硬脂酸锆、月桂酸锆、环烷酸锆、油酸锆、蓖麻油酸锆等。锆盐的纯度低时,可以纯化后再使用,也可以将市售品或预先制备的盐直接供给水热反应。
可用于所述(iii)中的所述氧化锆前驱体,与上述的氧化锆前驱体相同。(iii)的情况中,氧化锆前驱体优选为碳酸锆。羧酸(2)与所述氧化锆前驱体的比例,相对于氧化锆前驱体1摩尔,羧酸(2)优选为0.5摩尔~10摩尔,更优选为1摩尔~8摩尔,进一步优选为1.2摩尔~5摩尔。羧酸(2)和所述氧化锆前驱体,可以直接供给水热反应,也可以在水热反应前使之进行预反应。水热反应前使之反应时,优选将羧酸(2)和氧化锆前驱体在有机溶剂中以浆料形式进行反应。此时,从提高反应速度和收率的角度,优选一边进行反应一边将反应时生成的水除去。为了在进行反应的同时除去反应时的水,作为反应溶剂优选使用沸点比水高的溶剂,更优选为后述的水热反应中使用的溶剂。另外,反应温度优选为70℃以上,更优选为80℃以上,以便可以除去水。反应温度上限为180℃以下,更优选为150℃以下。温度过高时,进行副反应而有可能导致羧酸的分解。反应时无法顺利进行除去水时,可以降低反应压力从而降低水的沸点使其反应。
作为Al或稀土类元素原料物质,具体地,可举出选自(i)羧酸(2)和氧化稀土类元素等的前驱体的盐、(ii)羧酸(2)的稀土类元素等的盐、以及(iii)羧酸(2)以及氧化稀土类元素等的前驱体,中的至少1种以上。(i)-(iii)的优选方式,与锆原料物质中的(i)-(iii)的优选方式相同。
关于锆成分的所述(i)-(iii)中的至少1种,并入Al或稀土类元素成分的情况,优选与所述(i)-(iii)中的至少1种在水存在下进行混合。此时,通过在加热或减压下进行,能够将氨或醋酸等的所述氧化锆前驱体中含有的低沸点的化合物逼出体系外,抑制下一工序的水热反应中的压力上升从而优选。此外,也可以在添加了后述的有机溶剂的溶液中进行所述反应。
接下来,针对水热反应进行说明。
关于锆成分的所述(i)-(iii)中的至少1种,并入Al或稀土类元素成分的情况,通过将其与所述(i)-(iii)中的至少1种供给水热反应得到氧化锆纳米粒子组合物。仅有所述(i)-(iii)无法有效地进行粘度高的水热反应时,可以添加对该(i)-(iii)示出良好溶解性的有机溶剂。为了得到氧化锆纳米粒子,特别优选使用羧酸(2)的锆盐、羧酸(2)的稀土类元素等的盐,分别作为锆成分、Al或稀土类元素成分。
作为所述有机溶剂,可以使用烃、酮、醚、醇等。水热反应时气化的溶剂有可能不能充分进行反应,优选为常压下的沸点为120℃以上的有机溶剂,更优选为140℃以上,进一步优选为150℃以上。具体地,可以例示出癸烷、十二烷、十四烷、均三甲苯、偏三甲苯、矿油、辛醇、癸醇、环己醇、萜品醇、乙二醇、二乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、2,3-丁二醇、己二醇、甘油、甲烷三甲醇、甲苯、二甲苯、三甲基苯、二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)等,优选为矿油、十二烷、十四烷、三甲基苯。
由于添加所述有机溶剂后分离为2层的情况,虽然可以通过添加表面活性剂等使之为均匀相状态或悬浊乳化状态,但通常可以在2层状态下供给水热反应。虽然也有所述组合物含有来自原料的充分量的水的情况,但原料中无水分或水分少的情况下,供给水热反应前需要添加水分。
水热反应的体系内存在的水分量,相对于体系内存在的氧化锆前驱体或含锆的盐(以下,氧化锆前驱体等)的摩尔数的水的摩尔数(水的摩尔数/氧化锆前驱体等的摩尔数)优选为4/1~100/1,更优选为8/1~50/1。不满4/1时,水热反应需要长时间,得到的所述氧化锆粒子的粒径变大。另一方面,超过100/1超时,由于体系内存在的氧化锆前驱体等少,除了产率降低以外没有特别的问题。
水热反应优选在2MPaG(表压)以下的压力下进行。超过2MPaG时,虽然反应也能进行,但是反应装置价格高而在工业上不优选。另一方面,压力过低时,由于反应进行缓慢,并且长时间的反应导致所述纳米粒子的粒径变大,氧化锆具有多种结晶系,因此优选在0.1MPaG以上的压力下进行,更优选在0.2MPaG以上进行。水热反应的时间例如为2-24小时左右。
由于氧化锆纳米粒子对各种介质的分散性良好,可以添加至多种的溶剂、单体(单官能单体和/或交联性单体)、低聚物、聚合物等,或它们的组合中。本发明也包含含有氧化锆纳米粒子的组合物。组合物包含,含有氧化锆纳米粒子以及溶剂的分散液,以及,含有选自氧化锆纳米粒子,选自单体、低聚物和聚合物中的至少1种以上的树脂成分的树脂组合物。
此外,树脂组合物包含,含有聚合物(聚合体等)和氧化锆纳米粒子的组合物;含有二羧酸和二胺的混合物,丙烯酸或甲基丙烯酸等的不饱和羧酸或其酯化合物等的具有聚合性的单体,以及氧化锆纳米粒子的组合物;含有所述聚合物、所述具有聚合性的单体、以及氧化锆纳米粒子的组合物等。所述树脂成分可以为用于光学薄膜等的成型材料中使用的成型用树脂。所述树脂组合物还可以为含有溶剂的组合物(涂层材料)。
氧化锆纳米粒子,特别是对高极性的溶剂可发挥良好的分散性。因而,组合物(例如,分散液或树脂组合物)中使用的溶剂,对于水的HSP距离优选为40(MPa)1/2以下,更优选为35(MPa)1/2以下,进一步优选为30(MPa)1/2以下,下限虽然没有特别的限定,但通常为0(MPa)1/2以上。
作为可分散氧化锆纳米粒子的有机溶剂,例如,可举出:甲醇、乙醇、正丙醇、异丙醇、乙二醇等的醇类;甲基乙基酮、甲基异丁基酮、环己酮等的酮类;乙酸乙酯、乙酸丙酯等的酯类;乙二醇单甲醚、二乙二醇单丁醚等的醚类;丙二醇单甲醚乙酸酯等的改性醚类;苯、甲苯、二甲苯、乙苯、己烷、环己烷、甲基环己烷、乙基环己烷、矿物油精等的烃类;二氯甲烷、氯仿等的卤代烃类;二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮等的酰胺类;水;矿物油、植物油、蜡油、硅油等的油类。它们可以使用1种,也可以将2种以上组合使用。
氧化锆纳米粒子,由于特别是对极性溶剂的分散性良好,优选的有机溶剂为水、醇类、酯类或酰胺类,更优选为水、醇类或酯类,进一步优选为水或醇类,特别优选为水、甲醇或乙醇。
本发明的氧化锆纳米粒子,由于对有机溶剂的分散性良好,可以制备高核浓度的分散液。分散液中,本发明的纳米粒子所含的金属元素(锆、铝、过渡金属等)的氧化物的总量(核浓度),在分散液100质量中,优选为45质量%以上,更优选为50质量%以上,进一步优选为53质量%以上,上限没有特别的限定,例如为80质量%以下,更优选为70质量%以下。通过提高分散液中含有的金属成分的比例,金属成分的性质更容易显现,能够简便地制备具有高折射率的制品。
此外,在分散液中,本发明的纳米粒子所含的金属元素(锆、铝、过渡金属等)的氧化物的总量(核浓度)基于式(A)计算。
核浓度=分散液中的本发明的纳米粒子所含的金属氧化物的总重量/分散液重量…(A)
单官能单体,只要是仅具有一个可聚合的碳-碳双键的化合物即可,可举出(甲基)丙烯酸酸酯;苯乙烯、对叔丁基苯乙烯、α-甲基苯乙烯、间甲基苯乙烯、对甲基苯乙烯、对氯苯乙烯、对氯甲基苯乙烯等的苯乙烯类单体;(甲基)丙烯酸等的含羧基单体;(甲基)丙烯酸羟乙酯等的含羟基单体等。作为上述的(甲基)丙烯酸酯,具体地,例如可举出(甲基)丙烯酸甲酯,(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯等的(甲基)丙烯酸烷基酯;(甲基)丙烯酸环己酯、(甲基)丙烯酸异冰片酯等的(甲基)丙烯酸环烷基酯;(甲基)丙烯酸苯甲酯等的(甲基)丙烯酸芳烷基酯;(甲基)丙烯酸缩水甘油酯等的具有缩水甘油基的(甲基)丙烯酸酯等。上述例示的单官能单体可以单独使用,也可以适当混合两种以上使用。
交联性单体,只要是含有可与单体具有的碳-碳双键共聚的多个碳-碳双键的化合物即可。作为该交联性单体,具体地,例如可举出:二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸二乙二醇酯、二(甲基)丙烯酸丙二醇酯、二(甲基)丙烯酸二丙二醇酯等的多(甲基)丙烯酸亚烷基二醇酯;二(甲基)丙烯酸新戊二醇酯、二(甲基)丙烯酸二新戊二醇酯等的多(甲基)丙烯酸新戊二醇酯;三羟甲基丙烷三(甲基)丙烯酸酯、二(三羟甲基丙烷)四(甲基)丙烯酸酯等的三羟甲基丙烷多(甲基)丙烯酸酯;季戊四醇三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯等的季戊四醇多(甲基)丙烯酸酯等的多官能(甲基)丙烯酸酯;二乙烯基苯等的多官能苯乙烯类单体;邻苯二甲酸二烯丙酯、间苯二甲酸二烯丙酯、三聚氰酸三烯丙酯、异三聚氰酸三烯丙酯等的多官能烯丙基酯类单体等。
含有上述单体的组合物,属于固化性组合物。该固化性组合物在固化后构成树脂组合物,这样的固化性组合物也包含在本发明的树脂组合物中。另外,本发明的组合物可以为含有上述含聚合物(树脂)的树脂组合物。构成树脂组合物时,可举出:作为介质的聚合物例如6-尼龙、66-尼龙、12-尼龙等的聚酰胺类;聚酰亚胺类;聚氨酯类;聚乙烯、聚丙烯等的聚烯烃类;PET、PBT、PEN等的聚酯类;聚氯乙烯类;聚偏氯乙烯类;聚乙酸乙烯类;聚乙烯醇类;聚苯乙烯类;(甲基)丙烯酸树脂类聚合物;ABS树脂;氟树脂;苯酚-甲醛树脂、甲酚-甲醛树脂等的酚树脂;环氧树脂;尿素树脂、三聚氰胺树脂、胍胺树脂等的氨基树脂;聚乙烯醇缩丁醛类树脂、聚氨酯类树脂、乙烯-乙酸乙烯酯共聚物类树脂、乙烯-(甲基)丙烯酸酸酯共聚物类树脂等的软质树脂或硬质树脂等。上述中,更优选为聚酰亚胺类、聚氨酯类、聚酯类、聚乙烯醇类、(甲基)丙烯酸树脂类聚合物、酚树脂、氨基树脂、环氧树脂,进一步优选为聚乙烯醇类或(甲基)丙烯酸树脂类聚合物。它们可以单独使用,也可以2种以上混合使用。
上述组合物中所占有的氧化锆纳米粒子的浓度,可以根据用途适当设定,该组合物未固化时或含有聚合物(树脂)时,相对于该组合物的所有成分(氧化锆纳米粒子、溶剂、单体、低聚物、聚合物以及后述的聚合物前驱体等中使用的全部合计)100质量%,通常为90质量%以下。超过90质量%时,难以均匀分散未固化组合物可能产生白浊。另一方面,下限值没有特别的限定,考虑到溶剂成本,例如为1质量%以上。更优选为5质量%以上且85质量%以下,进一步优选为10质量%以上且80质量%以下。
另外,由于氧化锆纳米粒子的分散性非常好,即使是高浓度的组合物(分散体),组合物也具有良好的透明性。氧化锆纳米粒子以高浓度分散的组合物,例如有利于折射率的提高,可以根据各种用途进行折射率的调整。作为高浓度的氧化锆纳米粒子组合物使用时,该组合物中的氧化锆纳米粒子的量优选为25质量%以上,更优选为30质量%以上,进一步优选为60质量%以上。上限没有特别的限定,该组合物中的氧化锆纳米粒子的量可以为90质量%以下。
树脂组合物(含有固化后的固化性组合物)中,可以掺合氧化锆纳米粒子和树脂之外其他的添加成分。作为相关的添加成分,例如可举出固化剂、固化促进剂、着色剂、脱模剂、反应性稀释剂、增塑剂、稳定剂、阻燃助剂、交联剂等。
树脂组合物(含有固化后的固化性组合物)的形状没有特别的限定,例如可以为板、片材、薄膜、纤维等的成型材料。
氧化锆纳米粒子,由于分散性良好,除了适用于防反射膜、硬涂膜、增亮膜、棱镜膜、双凸透镜片、微透镜片等光学膜(片),光学用折射率调节剂、光学用粘合剂、光波导、透镜、催化剂、CMP研磨用组合物、电极、电容器、喷墨记录方法、压电元件、LED·OLED·有机EL等取光提升剂、抗菌剂、牙科用粘合剂、用于太阳能电池面板的聚光结构体之外,由于良好的分散性以外,焙烧前后晶体结构的变化受到抑制,还适用于假牙材料、SOFC(固体氧化物燃料电池)材料、坩埚等的陶瓷材料用途。
氧化锆纳米粒子,由于用具有基团R1的化合物(1)包覆,对溶剂(特别是高极性的溶剂)的分散性良好,将含有氧化锆纳米粒子的组合物焙烧得到的陶瓷材料,透光性、韧性、强度等的陶瓷特性良好。
由氧化锆纳米粒子得到的陶瓷材料,能够通过将氧化锆纳米粒子单独焙烧而得到。另外,也可以将在氧化锆纳米粒子,包含氧化铝、尖晶石、YAG、莫来石、硼酸铝化合物等的添加剂的组合物焙烧而得到。进而,能够通过将由氧化锆纳米粒子和粘合剂构成的组合物进行焙烧而得到。此时的焙烧温度为500-1600℃左右即可。焙烧能够采用公知的方法进行。焙烧时为了促进烧结,可以进行加压。另外,可以在空气中或氧气气氛中、氧和空气的混合气氛中进行焙烧,也可以在氮气中、氩气中等的惰性气氛中进行焙烧。可以根据焙烧后的用途分别进行适当选择。
本申请主张2016年3月25日申请的日本专利申请第2016-061941号以及2016年7月19日申请的日本专利申请第2016-141696号为基础的优先权的利益。2016年3月25日申请的日本专利申请第2016-061941号以及2016年7月19日申请的日本专利申请第2016-141696号的说明书的全部内容,引入到本发明中作为参考。
实施例
以下,通过举出实施例对本发明进行更具体的说明,本发明并不受下述实施例的限制,在符合前后文的主旨的范围内可以进行适当地变更实施,它们均包含在本发明的技术范围内。
实施例中公开的物性和特性通过以下的方法测定。
(1)晶体结构的解析
氧化锆纳米粒子的晶体结构使用X射线衍射装置(理学社制,RINT-TTRIII)解析。测定条件如下。
X射线源:CuKα(0.154nm)
X射线输出设定:50kV,300mA
采样宽度:0.0200°
扫描速度:10.0000°/min
测定范围:10-75°
测定温度:25℃
(2)正方晶、单斜晶的比例的定量
基于使用X射线衍射装置(理学社制,RINT-TTRIII)算出的值,使用计算软件(理学社制,PDXL)通过参考强度比法(RIP法)进行定量(峰的归属也根据计算软件的指定)。
(3)通过X射线衍射分析算出晶粒直径
氧化锆纳米粒子的晶粒直径,是基于通过X射线衍射装置(理学社制,RINT-TTRIII)解析并算出的30°的峰的半峰宽,使用计算软件(理学社制,PDXL)算出。
此外,X射线衍射测定中难以区分氧化锆纳米粒子的立方晶和正方晶,立方晶存在的情况下,其比例被记为正方晶的比例。
(4)重量(质量)减少率的测定
通过TG-DTA(热重-差热分析)装置,在空气气氛下,将氧化锆纳米粒子以10℃/分钟的速率从室温升温至800℃,测定该粒子的重量(质量)减少率。通过该重量(质量)减少率,可以知道包覆氧化锆纳米粒子的包覆剂的比例。
(5)通过电子显微镜的平均一次粒径的测定
包覆型氧化锆粒子的平均一次粒径,通过超高分辨率场发射型扫描电子显微镜(日立High Technologies社制,S-4800)观察而测定。在倍率15万倍下观察包覆型氧化锆粒子,针对任意的100个粒子,测定各粒子的长轴方向的长度,将其平均值作为平均一次粒径。
(6)核浓度的计算
核浓度基于式(A)算出。此外,实施例中,将“分散液中的纳米粒子所含的金属氧化物的总重量”作为“(掺合的纳米粒子重量×(1-(4)中测定的重量减少率))”进行计算。
核浓度=分散液中的纳米粒子所含的金属氧化物的总重量/分散液重量…(A)
<比较例1:2-乙基己酸(对于乙醇的R1的汉森溶解度参数(HSP)距离为21(MPa)1/2)和/或来自2-乙基己酸的羧酸酯包覆的氧化锆纳米粒子的制备>
在2-乙基己酸锆矿物油精溶液(90.4g,2-乙基己酸锆含有率44质量%,第一稀元素化学工业社制)中混合纯水(15.5g),进料至200mL的水热合成容器中。将该容器加热至190℃,在该温度下保持16小时进行反应。水热合成时的压力为1.3MPaG(表压)。反应后,从水热合成反应溶液分液除去水。
确认将除去水后的水热合成反应液上层在180℃下加热除去有机溶剂得到的氧化锆纳米粒子的晶体结构时,检出属于正方晶和单斜晶的衍射线,从衍射线的强度可知,正方晶与单斜晶的比例为74/26,其粒径(正方晶和/或立方晶的晶粒直径)为5nm。通过电子显微镜测定平均一次粒径的结果为11nm。另外,氧化锆纳米粒子的重量(质量)减少率为14质量%。从而可知,包覆的2-乙基己酸和/或来自2-乙基己酸的羧酸酯为氧化锆纳米粒子总体的14质量%。
在该除去有机溶剂得到的粒子(1g)中添加乙醇(0.5g,对于水的汉森溶解度参数(HSP)距离为24(MPa)1/2),产生白浊且无法使粒子分散。
<实施例1:用甲氧基乙酸包覆的氧化锆纳米粒子的制备>
比较例1的除去水后的水热合成反应液上层50g与甲氧基乙酸(对于乙醇的R1的汉森溶解度参数(HSP)距离为14(MPa)1/2)5g在60℃下搅拌混合30分钟。接下来,添加正己烷之后通过过滤分离凝聚粒子。然后,将分离的凝聚粒子添加至正己烷中,搅拌10分钟后,通过过滤分离凝聚粒子,将得到的粒子在室温下真空干燥,得到用甲氧基乙酸包覆的氧化锆纳米粒子。
确认该粒子的晶体结构时,检出属于正方晶和单斜晶的衍射线,从衍射线的强度可知,正方晶和单斜晶的比例为74/26,其粒径(正方晶和/或立方晶的晶粒直径)为5nm。另外,氧化锆纳米粒子的重量(质量)减少率为11质量%。从而可知,包覆的2-乙基己酸、来自2-乙基己酸的羧酸酯以及甲氧基乙酸的质量为氧化锆纳米粒子总体的11质量%。
<实施例2:含无机氧化物微粒子的溶液1的制备>
将实施例1中得到的氧化锆纳米粒子(1g)与乙醇(0.5g)掺合,搅拌至均匀,得到含无机氧化物微粒子的溶液1。此外,分散液中,得到的纳米粒子所含的金属氧化物的浓度(核浓度)为59%(=(1g×(1-0.11))/(1g+0.5g))。
<比较例2:用2-乙基己酸和/或来自2-乙基己酸的羧酸酯包覆的氧化钇稳定氧化锆纳米粒子的制备>
除了将实施例1的2-乙基己酸锆矿物油精溶液(2-乙基己酸锆含有率44质量%,第一稀元素化学工业社制)变为86.7g,NIKKA OCTHIX钇(钇含量6.2%,日本化学产业社制)变为10.1g以外,与实施例1同样进行合成。
确认得到的氧化钇稳定氧化锆纳米粒子的晶体结构时,检出属于正方晶和单斜晶的衍射线,从衍射线的强度可知,正方晶和单斜晶的比例为97/3,其粒径(正方晶和/或立方晶的晶粒直径)为4nm。通过电子显微镜测定平均一次粒径的结果为6nm。另外,氧化钇稳定氧化锆纳米粒子的重量(质量)减少率为25质量%。从而可知,包覆的2-乙基己酸和/或来自2-乙基己酸的羧酸酯为氧化钇稳定氧化锆纳米粒子总体的25质量%。将除去有机溶剂得到的氧化钇稳定氧化锆纳米粒子(1g)以及乙醇(0.5g)混合搅拌,白色粉体无法分散。
<实施例3:用甲氧基乙酸包覆的包覆型氧化钇稳定氧化锆纳米粒子的制备>
除了将除去使用的水后的水热合成反应液上层变为比较例2中合成的反应液上层以外,与实施例1同样进行合成。氧化钇稳定氧化锆纳米粒子的重量(质量)减少率为15质量%。从而可知,包覆的2-乙基己酸、来自2-乙基己酸的羧酸酯以及甲氧基乙酸的质量为氧化钇稳定氧化锆纳米粒子总体的15质量%。
<实施例4:含无机氧化物微粒子的溶液2的制备>
将实施例3得到的氧化钇稳定氧化锆纳米粒子(1g)与乙醇(0.5g)掺合,搅拌至均匀,得到含有无机氧化物微粒子的溶液2。此外,分散液中,得到的纳米粒子所含的金属氧化物的浓度(核浓度)为57%(=(1g×(1-0.15))/(1g+0.5g))。
<实施例5:含有无机氧化物微粒子的树脂组合物1的制备>
将实施例1得到的氧化锆纳米粒子1g、丙烯酸2-羟乙酯(日本触媒制)1g以及甲醇4g掺合,在室温下搅拌1小时,得到均匀的含有无机氧化物微粒子的树脂组合物1。
<实施例6:含有无机氧化物微粒子的树脂组合物2的制备>
将实施例1得到的氧化锆纳米粒子1g、季戊四醇三丙烯酸酯(SARTOMER社制“SR444NS”)1g以及甲醇4g掺合,在室温下搅拌1小时,得到均匀的含有无机氧化物微粒子的树脂组合物2。
<实施例7:含有无机氧化物微粒子的树脂组合物3的制备>
将实施例1得到的氧化锆纳米粒子1g、二季戊四醇六丙烯酸酯(日本化药制“KAYARAD DPHA”)1g以及甲醇4g掺合,在80℃下加热搅拌1小时,得到均匀的含有无机氧化物微粒子的树脂组合物3。
<实施例8:含有无机氧化物微粒子的树脂组合物4的制备>
将实施例1得到的氧化锆纳米粒子1g、聚乙烯醇(Kuraray制“CP-1210”)1g以及离子交换水4g掺合,在80℃下加热搅拌1小时,得到均匀的含有无机氧化物微粒子的树脂组合物4。
工业可利用性
本发明的氧化锆纳米粒子,对醇等极性溶剂的分散性良好,并且可以提高分散液中的核浓度,能够广泛用作光学材料、电子零件材料等而有用。
Claims (16)
1.一种氧化锆纳米粒子,其特征在于,用选自R1-COOH、(R1O)3-n-P(O)-(OH)n、(R1)3-n-P(O)-(OH)n、(R1O)-S(O)(O)-(OH)、R1-S(O)(O)-(OH)、(R1)4-m-Si(R4)m中的1种以上的化合物包覆,
式中,R1表示含有选自氧原子、氮原子和硫原子中的1种以上的元素和碳原子,R1中的碳原子、氧原子、氮原子和硫原子的总原子数为8以下的基团;
R4为卤原子或-OR2,R2表示氢原子或烷基;
n表示1或2,m表示1-3的整数。
2.根据权利要求1所述的氧化锆纳米粒子,其中,R1中,相对于碳原子数的氧原子、氮原子和硫原子的和的比(氧原子、氮原子和硫原子的和/碳原子数)为1/7以上且1/1以下。
3.根据权利要求1或2所述的氧化锆纳米粒子,其中,所述化合物中,相对于碳原子数的氧原子数的比(氧原子数/碳原子数)为大于1/6且1/0.2以下。
4.根据权利要求1-3中任意一项所述的氧化锆纳米粒子,其中,正方晶和立方晶的合计为晶体结构总体的60%以上。
5.根据权利要求1-4中任意一项所述的氧化锆纳米粒子,其中,所述氧化锆纳米粒子的平均粒径为1-100nm。
6.根据权利要求1-5中任意一项所述的氧化锆纳米粒子,其中,对于乙醇的R1的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且20(MPa)1/2以下。
7.根据权利要求1-5中任意一项所述的氧化锆纳米粒子,其中,对于水的R1的汉森溶解度参数(HSP)距离为20(MPa)1/2以上且41(MPa)1/2以下。
8.一种分散液,其含有权利要求1-7中任意一项所述的氧化锆纳米粒子。
9.根据权利要求8所述的分散液,其中,该分散液含有对于水的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且40(MPa)1/2以下的溶剂。
10.一种树脂组合物,其含有权利要求1-7中任意一项所述的氧化锆纳米粒子。
11.根据权利要求10所述的树脂组合物,其中,所述树脂组合物含有选自单体、低聚物以及聚合物中的至少1种以上的树脂成分。
12.根据权利要求10或11所述的树脂组合物,其中,所述树脂组合物含有对于水的汉森溶解度参数(HSP)距离为0(MPa)1/2以上且40(MPa)1/2以下的溶剂。
13.一种成型材料,其含有权利要求1-7中任意一项所述的氧化锆纳米粒子。
14.一种陶瓷材料,其由权利要求1-7中任意一项所述的氧化锆纳米粒子得到。
15.一种陶瓷材料的制备方法,其特征在于,将权利要求1-7中任意一项所述的氧化锆纳米粒子在500℃以上进行焙烧。
16.一种陶瓷材料的制备方法,其特征在于,将含有权利要求1-7中任意一项所述的氧化锆纳米粒子的组合物在500℃以上进行焙烧。
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CN112585219A (zh) * | 2018-12-21 | 2021-03-30 | 第一稀元素化学工业株式会社 | 含锆的醇溶液 |
CN113692392A (zh) * | 2019-04-15 | 2021-11-23 | 马自达汽车株式会社 | 隔热材料、包括隔热材料的发动机、纳米粒子分散液以及隔热材料等的制造方法 |
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TW201741244A (zh) | 2017-12-01 |
JP2017178763A (ja) | 2017-10-05 |
KR20180122390A (ko) | 2018-11-12 |
KR102575562B1 (ko) | 2023-09-05 |
EP3434648A4 (en) | 2019-12-18 |
CN108883946B (zh) | 2024-05-10 |
TWI668190B (zh) | 2019-08-11 |
JP6851740B2 (ja) | 2021-03-31 |
EP3434648A1 (en) | 2019-01-30 |
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