TWI810318B - 無機氧化物微粒子分散液及其製造方法、樹脂組成物、以及硬化物 - Google Patents
無機氧化物微粒子分散液及其製造方法、樹脂組成物、以及硬化物 Download PDFInfo
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- TWI810318B TWI810318B TW108120510A TW108120510A TWI810318B TW I810318 B TWI810318 B TW I810318B TW 108120510 A TW108120510 A TW 108120510A TW 108120510 A TW108120510 A TW 108120510A TW I810318 B TWI810318 B TW I810318B
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- inorganic oxide
- weight
- dispersant
- fine particles
- parts
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- 229910052809 inorganic oxide Inorganic materials 0.000 title claims abstract description 102
- 239000006185 dispersion Substances 0.000 title claims abstract description 59
- 239000011859 microparticle Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000011342 resin composition Substances 0.000 title claims description 22
- 239000010419 fine particle Substances 0.000 claims abstract description 82
- 239000002270 dispersing agent Substances 0.000 claims abstract description 68
- 150000001875 compounds Chemical class 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000010298 pulverizing process Methods 0.000 claims abstract description 9
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims description 45
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- 239000011347 resin Substances 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- 229920001296 polysiloxane Polymers 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 14
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 9
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- 239000007787 solid Substances 0.000 claims description 6
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- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 11
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- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
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- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 5
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 4
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- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 235000019382 gum benzoic Nutrition 0.000 description 3
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
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- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 2
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- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
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- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- XYJRNCYWTVGEEG-UHFFFAOYSA-N trimethoxy(2-methylpropyl)silane Chemical compound CO[Si](OC)(OC)CC(C)C XYJRNCYWTVGEEG-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本發明之目的在於提供一種無機氧化物微粒子分散液之製造方法,其可簡便地使無機氧化物微粒子分散,且可減少分散劑之使用量。
本發明係一種無機氧化物微粒子分散液之製造方法,其包括:將下述(A)~(D)成分混合之步驟:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數(Hansen solubility parameter)之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑;及將該混合物濕式粉碎之步驟。
Description
本發明係關於一種無機氧化物微粒子分散液。
近年來,為了顯示器之反射防止或光學透鏡之聚光效率提高,正在研究摻合有氧化鈦、氧化鋯等顯示高折射率之無機氧化物微粒子之光學塗佈組成物,並將其實用化。
此種光學塗佈組成物可將無機氧化物微粒子之分散液一面維持分散狀態一面混合於硬化性樹脂而獲得。無機氧化物微粒子於表面具有羥基,顯示親水性,因此於欲將其混合於非水溶性之硬化性樹脂之情形時,亦有引起凝聚而發生白濁,或有時增黏而失去流動性之情況。因此,作為使無機氧化物微粒子之分散狀態穩定化之技術,提出有多種利用添加分散劑或藉由矽烷偶合劑之表面處理的無機微粒子分散液之製法。且說,若大量地摻合使微粒子分散穩定化而防止凝聚之分散劑,則有所獲得之薄膜或成形體之耐光性或耐熱性降低之情況。因此,要求減少分散劑之使用量且使無機氧化物微粒子分散,正在研究與藉由矽烷偶合劑之表面處理併用或以複雜之製程製備分散液。
專利文獻1中,使用分散劑、分散介質、矽烷偶合劑使氧化鋯奈米粒子分散。必須於向無機氧化物微粒子中添加分散劑之步驟之後,分批添加烷氧基矽烷。
專利文獻2中,於使無機氧化物微粒子於甲醇中分散後,將溶劑置換為非醇親油性有機溶劑。雖無機氧化物微粒子可分散,但需要溶劑置換步驟。
[先前技術文獻]
[專利文獻]
專利文獻1:日本特開2010-189506號公報
專利文獻2:日本特開2015-117157號公報
本發明之目的在於提供一種無機氧化物微粒子分散液之製造方法,其可簡便地使無機氧化物微粒子分散,且可減少分散劑之使用量。
本發明人等發現若使用特定之溶劑,則可簡便地使無機氧化物微粒子分散,且可減少分散劑之使用量,從而完成本發明。
即,本發明係關於一種無機氧化物微粒子分散液之製造方法,其包括:將下述(A)~(D)成分混合之步驟:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數(Hansen solubility parameter)之氫鍵項(dH)為11
以下且極性項(dP)為4以上之溶劑;及將該混合物濕式粉碎之步驟。
(B)分散劑與(C)烷氧基矽烷化合物之重量比較佳為20:80~5:95。
相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量較佳為5~40重量份。
又,本發明係關於一種無機氧化物微粒子分散液,其含有下述(A)~(D)成分:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑;且(B)分散劑與(C)烷氧基矽烷化合物之重量比為20:80~5:95。
相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量較佳為5~40重量份。
又,本發明係關於一種樹脂組成物,其含有上述無機氧化物微粒子分散液、及黏合劑樹脂。
固形物成分中之無機氧化物微粒子之含量較佳為30重量%以上。
又,本發明係關於一種硬化物,其係使上述樹脂組成物硬化而成。
本發明之無機氧化物微粒子分散液之製造方法可簡便地使無機氧化物微粒子分散,且可減少分散劑之使用量。又,使本發明之樹脂組成物硬
化而成之塗膜具有良好之光學特性及較高之可靠性。
<<無機氧化物微粒子分散液之製造方法>>
本發明係關於一種無機氧化物微粒子分散液之製造方法,其包括:將下述(A)~(D)成分混合之步驟:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑;及將上述混合物濕式粉碎之步驟。
<(A)無機氧化物微粒子>
本發明中,作為(A)無機氧化物微粒子,自獲取之容易性、折射率等光學特性之調整容易之觀點考慮,使用選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種。該等中較佳為氧化鋯。該等無機氧化物微粒子亦可為摻雜有異種之元素之化合物。作為於無機氧化物微粒子中摻雜有異種之元素之化合物,例如可列舉:摻雜有鉭之氧化鈦、或摻雜有鈮之氧化鈦等。該等無機氧化物微粒子可單獨地使用,亦可併用2種以上。又,無機氧化物微粒子之製法亦無特別限定。
無機氧化物微粒子之一次粒徑無特別限定,較佳為1~50nm,更佳為5~30nm。若未達1nm,則無機氧化物微粒子之比表面積較大,凝聚能量較高,因此有難以保持分散穩定性之情況。另一方面,若超過50nm,則有因薄膜或成形體中之無機氧化物微粒子而產生之光之散射變得激烈,無法將透明性維持得較高之情況。再者,一次粒徑可利用SEM、TEM等電子顯微鏡、或由比表面積之換算進行測定。
本發明之分散液中之無機氧化物微粒子之平均粒徑較佳為10~70nm,更佳為10~50nm。為了設為未達10nm,必須使用一次粒徑較小之粒子,因此有分散變得困難之情況。另一方面,若超過70nm,則於製成薄膜、成形體等硬化物時,有發生白濁之情況。二次粒徑可利用動態光散射法、雷射繞射法等裝置進行測定。
無機氧化物微粒子之摻合量於分散液中較佳為5~80重量%,更佳為10~70重量%,進而較佳為20~65重量%,最佳為30~65重量%。若為上述範圍內,則可充分地發揮光學特性,亦可維持製膜性。
<(B)分散劑>
分散劑只要可使無機氧化物微粒子於後述之溶劑中分散,則無特別限定,例如可列舉:聚丙烯酸系分散劑、多羧酸系分散劑、磷酸系分散劑、聚矽氧系分散劑。
作為聚丙烯酸系分散劑,例如可列舉聚丙烯酸鈉,作為市售品,可列舉:ARON系列(東亞合成股份有限公司製造)、SHALLOL系列(第一工業製藥股份有限公司製造)。
作為多羧酸系分散劑,例如可列舉未經陽離子中和之酸性類型之分散劑或多羧酸銨鹽,作為市售品,可列舉:AH-103P(第一工業製藥股份有限公司製造)、SN DISPERSANT 5020、SN DISPERSANT 5468(SAN NOPCO股份
有限公司製造)、POIZ 532A、POIZ 2100(花王股份有限公司製造)、MALIALIM AKM-0531、MALIALIM AKM-1511-60、MALIALIM HKM-50A、MALIALIM HKM-150A(日油股份有限公司製造)。
作為磷酸系分散劑,例如可列舉聚氧乙烯烷基醚磷酸酯。作為市售品,可列舉:Phosphanol RA-600、ML-220(東邦化學工業股份有限公司製造)、Disparlon PW-36(楠本化成股份有限公司製造)。
作為聚矽氧系分散劑,例如可列舉改質聚矽氧油等。作為市售品,可列舉ES-5612(東麗道康寧公司製造)。
分散劑之摻合量相對於無機氧化物微粒子100重量份,較佳為0.25~8重量份,更佳為0.5~7重量份,進而較佳為1~5重量份。若摻合量未達0.25重量份,則有無機氧化物微粒子無法充分地分散之情況,若超過8重量份,則有於加工成薄膜、成形體等時,使耐光性或耐熱性降低,或無法充分地獲得無機氧化物微粒子之特性之情況。
<(C)烷氧基矽烷化合物>
烷氧基矽烷化合物係以於使分散液與黏合劑樹脂混合時提高無機氧化物微粒子與黏合劑之親和性為目的而添加。若將本發明之分散液設為酸性條件或鹼性條件,則可使存在於無機氧化物微粒子之表面之羥基與烷氧基矽烷化合物反應,進行無機氧化物微粒子之表面處理。
作為烷氧基矽烷化合物,較佳為下述式(I)SiR4 (I)
(式中,R為氫、羥基、碳數1~4之烷氧基、可具有取代基之烷基、可具有取代基之苯基。其中,4個R中之至少1個為碳數1~4之烷氧基或羥基)
所表示之化合物。
作為烷氧基矽烷化合物之具體例,可列舉:3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、苯基三甲氧基矽烷、乙烯基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、對苯乙烯基三甲氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、3-脲基丙基三乙氧基矽烷、3-巰基丙基甲基二甲氧基矽烷、雙(三乙氧基矽基丙基)四硫化物、3-異氰酸基丙基三乙氧基矽烷等三烷氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、二甲基二甲氧基矽烷、二苯基二甲氧基矽烷等二烷氧基矽烷。該等可單獨地使用,亦可併用2種以上。該等中,較佳為三烷氧基矽烷,更佳為3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、苯基三甲氧基矽烷。
烷氧基矽烷化合物之摻合量相對於無機氧化物微粒子100重量份,較佳為4~50重量份,更佳為6~38重量份,進而較佳為8~20重量份。若摻合量未達4重量份,則有難以使無機氧化物微粒子均勻地分散之情況,若超過50重量份,則有無法使無機氧化物高填充而無法獲得目標之特性之情況。
又,分散液中之(B)分散劑與(C)烷氧基矽烷化合物之重量比較佳為20:80~5:95,更佳為18:82~7:93,進而較佳為18:82~9:91。若相對於分散劑20,烷氧基矽烷化合物之重量比低於80,則分散劑變得過量,有成為於加工成薄膜、成形體等時特性降低之原因之情況,若相對於分散劑5,烷氧基矽烷化合物之重量比超過95,則有難以製作均勻之分散液之情況。
本發明中,藉由使用特定之溶劑,可減少分散劑且簡便地使無機氧化物微粒子分散。相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量較佳為5~40重量份,更佳為7~35重量份,進而較佳為10~30重量份。若相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量低於5重量份,則有無機氧化物微粒子無法
充分地分散之情況,若超過40重量份,則有於利用分散體而獲得之光學塗佈塗膜、光學構件、成形體等中,使折射率、耐光性、耐熱性降低之情況。
<(D)溶劑>
本發明中,使用漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑。藉此,可減少分散劑之使用量且獲得穩定之無機氧化物微粒子之分散液。進而,於使無機氧化物微粒子分散於不滿足上述要件之溶劑中之情形時,必須首先向無機氧化物微粒子中添加分散劑,其後分批添加烷氧基矽烷,或者分散於醇性溶劑後,將溶劑置換為非醇性親油性有機溶劑。但是,本發明中之溶劑中,即便一次性添加無機氧化物微粒子、分散劑、烷氧基矽烷化合物,亦可使其微分散,亦無需分散後之溶劑置換,從而能夠簡化分散步驟。
漢森溶解度參數係將根據希德布朗(Hildebrand)之溶解度藉由分散項dD、極性項dP、氫鍵項dH之3個參數表現者。分散項dD、極性項dP、氫鍵項dH係物質固有之物性值,例如,揭示於「Hansen Solubility Parameters:A User's Handbook,HSPiP 3rd Edition ver.3.0.20」中。
本發明中,溶劑之漢森溶解度參數之氫鍵項(dH)為11以下。若超過11,則有變得難以獲得良好之分散狀態之分散液之情況。又,氫鍵項(dH)之下限無特別限定,通常為3以上。
溶劑之漢森溶解度參數之極性項(dP)為4以上,更佳為5以上。若低於4,則有變得難以獲得良好之分散狀態之分散液之情況。又,極性項(dP)之上限無特別限定,通常為13以下。
溶劑之漢森溶解度參數之分散項(dD)無特別限定,較佳為14~20。
作為漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑,可列舉:丙二醇單甲醚乙酸酯、甲基異丁基酮、環戊酮、甲基
乙基酮、四氫呋喃等。該等溶劑可單獨地使用,但只要混合後滿足上述漢森溶解度參數,則亦可混合2種以上使用。於製成混合溶劑之情形時,作為其成分,亦可使用單獨之情況下不滿足上述漢森溶解度參數之溶劑,只要藉由調整摻合比而使混合溶劑之漢森溶解度參數之氫鍵項(dH)成為11以下且使極性項(dP)成為4以上即可。作為單獨之情況下不滿足上述漢森溶解度參數但可作為混合溶劑之成分使用之溶劑,可列舉:丙二醇單甲醚、異丙醇、甲苯、甲醇、水等。
上述之溶劑中,作為單獨溶劑,較佳為丙二醇單甲醚乙酸酯、甲基異丁基酮、環戊酮。又,作為混合溶劑,較佳為將環戊酮與丙二醇單甲醚以50:50(重量基準)之比率混合之溶劑。
溶劑之摻合量相對於無機氧化物微粒子100重量份,較佳為30~900重量份,更佳為50~400重量份,進而較佳為60~400重量份。若摻合量未達30重量份,則有黏度變高而難以分散之情況,若超過900重量份,則有固形物成分濃度變低,無法使無機氧化物微粒子高填充,而無法獲得目標之特性之情況。
<任意成分>
無機氧化物微粒子分散液中,除上述之成分以外,亦可任意地含有其他成分。作為其他成分,例如可列舉:(A)無機氧化物微粒子以外之無機微粒子、丙烯酸酯單體、環氧樹脂等。
作為(A)無機氧化物微粒子以外之無機微粒子,例如可列舉:氧化矽(SiO2)、氧化鋁(Al2O3)、氧化鐵(Fe2O3、FeO、Fe3O4)、氧化銅(CuO、Cu2O)、氧化鋅(ZnO)、氧化釔(Y2O3)、氧化鈮(Nb2O5)、氧化鉬(MoO3)、氧化銦(In2O3、In2O)、氧化錫(SnO2)、氧化鉭(Ta2O5)、氧化鎢(WO3、W2O5)、氧化鉛(PbO、PbO2)、氧化鉍(Bi2O3)、氧化鈰(CeO2、Ce2O3)、氧化銻(Sb2O5、Sb2O5)、氧化鍺(GeO2、GeO)等金屬氧化物微粒子;鈦/矽複合氧化物、釔穩定化氧化鋯等由2種以上之金屬元素所構成之複合氧化物;及金、銀、銅、半導
體等非氧化物無機微粒子。複合氧化物不僅包含由多成分之元素所構成之化合物或固溶體,而且還包含:具有核殼結構者,該核殼結構係使成為核之金屬氧化物微粒子之周圍被覆有由其他金屬元素所構成之金屬氧化物;及具有多成分分散型之結構者,該多成分分散型之結構係如於1個金屬氧化物微粒子中分散有其他複數個金屬氧化物微粒子。於含有(A)無機氧化物微粒子以外之無機微粒子之情形時,其含量無特別限定,只要適當基於(A)無機氧化物微粒子之摻合量進行調整即可。
<混合步驟>
(A)無機氧化物微粒子、(B)分散劑、(C)烷氧基矽烷化合物、及(D)溶劑之混合順序無特別限定,可以任意之順序對溶劑添加無機氧化物微粒子、分散劑、烷氧基矽烷化合物。本發明中之溶劑容易使無機氧化物微粒子分散,因此亦可一次性添加全部成分。
<濕式粉碎步驟>
濕式粉碎步驟中,藉由濕式粉碎將混合步驟中所獲得之混合物粉碎。於漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑中進行濕式粉碎,藉此同時進行無機氧化物微粒子之粉碎與該粉碎物之分散。作為濕式粉碎步驟中所使用之濕式粉碎機,可列舉球磨機、珠磨機,亦可使用具有與該等研磨機不同之機構之裝置。於使用珠磨機作為濕式粉碎機之情形時,珠粒直徑較佳為30~100μm,旋轉速度較佳為6~12m/秒。
<<無機氧化物微粒子分散液>>
本發明之機氧化物微粒子分散液之特徵在於:含有下述(A)~(D)成分:(A)無機氧化物微粒子、(B)分散劑、
(C)烷氧基矽烷化合物、及(D)漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑;且(B)分散劑與(C)烷氧基矽烷化合物之重量比為20:80~5:95。關於無機氧化物微粒子分散液中所含之成分、含量、製造方法,如上文關於無機氧化物微粒子分散液之製造方法所述。
<<樹脂組成物>>
本發明之樹脂組成物含有上述無機氧化物微粒子分散液、及黏合劑樹脂。該樹脂組成物之固形物成分中,無機氧化物微粒子之含量較佳為30重量%以上,更佳為50重量%以上,進而較佳為70重量%以上。若為上述範圍內,則使該樹脂組成物硬化而成之硬化物可獲得所需之折射率。
作為黏合劑樹脂,無特別限定,例如可列舉:環氧樹脂、聚矽氧烷樹脂、聚酯樹脂、丙烯酸樹脂、胺酯(urethane)樹脂、聚烯烴樹脂、三聚氰胺等。該等可單獨地使用,亦可併用2種以上。
作為環氧樹脂,無特別限定,例如可列舉:雙酚A型、雙酚F型、酚系酚醛清漆型、作為具有多個苯環之多官能型之四(羥基苯基)乙烷型或三(羥基苯基)甲烷型、聯苯型、三苯酚甲烷型、萘型、鄰位酚醛清漆型、二環戊二烯型、胺基苯酚型、脂環式等之環氧樹脂、聚矽氧環氧樹脂等。該等可單獨地使用,亦可併用2種以上。
作為聚矽氧烷樹脂,例如可列舉為下述式(I)所表示之烷氧基矽烷之單體彼此縮合而成之烷氧基矽烷,且於1分子內具有1個以上之矽氧烷鍵(Si-O-Si)之低聚物等。
SiR1 4 (I)
(式中,R1為氫、羥基、碳數1~4之烷氧基、可具有取代基之烷基、可具
有取代基之苯基。其中,4個R1中之至少1個為碳數1~4之烷氧基或羥基)
聚矽氧烷樹脂較佳為式(I)所表示之烷氧基矽烷2分子以上縮合而成者。
聚矽氧烷樹脂之結構無特別限定,可為直鏈狀,亦可為支鏈狀。又,聚矽氧烷樹脂可單獨地使用式(I)所表示之化合物,亦可併用2種以上。
作為上述聚矽氧烷樹脂,可列舉:烷醇矽(silicon alkoxide)丙烯酸系樹脂、烷醇矽環氧系樹脂、烷醇矽乙烯基系樹脂、烷醇矽甲基丙烯酸系樹脂、烷醇矽硫醇系樹脂、烷醇矽胺基系樹脂、烷醇矽異氰酸酯系樹脂、烷醇矽烷基系樹脂、及不具有烷醇矽基以外之官能基之烷醇矽系樹脂等烷醇矽系樹脂。
作為上述聚矽氧烷樹脂之具體之構成成分,可列舉:2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二乙氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、3-巰基丙基甲基二甲氧基矽烷、3-巰基丙基三甲氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-三乙氧基矽基-N-(1,3-二甲基-亞丁基)丙基胺、N-苯基-3-胺基丙基三甲氧基矽烷、3-異氰酸基丙基三乙氧基矽烷、甲基三甲氧基矽烷、二甲基二甲氧基矽烷、三甲基甲氧基矽烷、甲基三乙氧基矽烷、甲基苯氧基矽烷、正丙基三甲氧基矽烷、二異丙基二甲氧基矽烷、異丁基三甲氧基矽烷、二異丁基二甲氧基矽烷、異丁基三乙氧基矽烷、正己基三甲氧基矽烷、正己基三乙氧基矽烷、環己基甲基二甲氧基矽烷、正辛基三乙氧基矽烷、正癸基三甲氧基矽烷、四甲氧基矽烷、四乙氧基
矽烷、四丙氧基矽烷、四丁氧基矽烷等四烷氧基矽烷或四苯氧基矽烷、矽酸甲酯低聚物、矽酸乙酯低聚物等烷氧基矽酸酯低聚物等。該等中,較佳為四烷氧基矽烷、四苯氧基矽烷、烷氧基矽酸酯低聚物。
聚矽氧烷樹脂之重量平均分子量無特別限定,較佳為大於1000且5000以下,更佳為大於1300且3700以下,進而較佳為1500~3500。
作為聚酯樹脂,只要為使於分子內具有2個以上之羧基之化合物與具有2個以上之羥基之化合物縮聚而獲得之高分子化合物,則無特別限定,例如可列舉:聚對苯二甲酸乙二酯、聚對苯二甲酸丙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸乙二酯、聚萘二甲酸丁二酯等。該等可單獨地使用,亦可併用2種以上。
作為丙烯酸樹脂,無特別限定,例如可列舉:(甲基)丙烯酸系樹脂、乙烯酯系樹脂等。作為該等丙烯酸樹脂,例如只要為含有具有羧基、酸酐基、磺酸基、磷酸基等酸基之聚合性單體作為構成單體之聚合物即可,例如可列舉:具有酸基之聚合性單體之均聚物或共聚物、具有酸基之聚合性單體與共聚性單體之共聚物等。該等可單獨地使用,亦可併用2種以上。
(甲基)丙烯酸系樹脂只要含有(甲基)丙烯酸系單體作為主要構成單體(例如50莫耳%以上),則亦可與共聚性單體聚合,於該情形時,只要(甲基)丙烯酸系單體及共聚性單體中之至少一者具有酸基即可。
作為(甲基)丙烯酸系樹脂,例如可列舉:具有酸基之(甲基)丙烯酸系單體[(甲基)丙烯酸、(甲基)丙烯酸磺烷基酯、含有磺酸基之(甲基)丙烯醯胺等]或其共聚物、可具有酸基之(甲基)丙烯酸系單體與具有酸基之其他聚合性單體[其他聚合性羧酸、聚合性多元羧酸或酸酐、乙烯基芳香族磺酸等]及/或共聚性單體[例如,(甲基)丙烯酸烷基酯、(甲基)丙烯酸環氧丙酯、(甲基)丙烯腈、芳香族乙烯基單體等]之共聚物、具有酸基之其他聚合物單體與(甲基)丙烯酸系共
聚性單體[例如,(甲基)丙烯酸烷基酯、(甲基)丙烯酸羥基烷基酯、(甲基)丙烯酸環氧丙酯、(甲基)丙烯腈等]之共聚物、不具有酸基之(甲基)丙烯酸系單體[(甲基)丙烯酸烷基酯、(甲基)丙烯酸芳基酯、茀系(甲基)丙烯酸酯等]或其共聚物、松香改質胺酯丙烯酸酯、特殊改質丙烯酸樹脂、胺酯丙烯酸酯、環氧丙烯酸酯、胺酯丙烯酸酯乳液等。
該等(甲基)丙烯酸系樹脂中,較佳為(甲基)丙烯酸-(甲基)丙烯酸酯聚合物(丙烯酸-甲基丙烯酸甲酯共聚物等)、(甲基)丙烯酸-(甲基)丙烯酸酯-苯乙烯共聚物(丙烯酸-甲基丙烯酸甲酯-苯乙烯共聚物等)等。
作為聚胺酯(polyurethane),只要為使具有異氰酸基之化合物與具有羥基之化合物共聚而獲得之高分子化合物,則無特別限定,例如可列舉:酯-醚系聚胺酯、醚系聚胺酯、聚酯系聚胺酯、碳酸酯系聚胺酯、丙烯酸系聚胺酯等。該等可單獨地使用,亦可併用2種以上。
作為聚烯烴樹脂,無特別限定,例如可列舉:聚乙烯、聚丙烯、氯化聚丙烯、順丁烯二酸酐改質聚丙烯、順丁烯二酸酐改質氯化聚丙烯等。該等可單獨地使用,亦可併用2種以上。
以上所列舉之黏合劑樹脂中,以獲得光學用途之硬化物為目的,為了容易調整光學特性,較佳為熱硬化性之黏合劑樹脂,更佳為熱硬化性之環氧樹脂、聚矽氧烷樹脂。黏合劑樹脂可單獨地使用,亦可併用2種以上。
黏合劑樹脂之含量無特別限定,相對於無機氧化物微粒子100重量份,較佳為5~100重量份,更佳為10~80重量份,進而較佳為10~50重量份。若為上述範圍內,則於製膜時不產生裂痕,可形成均勻之膜,並且光學特性優異。
<任意成分>
樹脂組成物中,除上述之成分以外,亦可任意地含有其他成分。作為其他
成分,例如可列舉:聚合起始劑、光敏劑、溶劑、調平劑、界面活性劑、消泡劑、中和劑、抗氧化劑、脫模劑、紫外線吸收劑等。
作為聚合起始劑,可列舉:光聚合起始劑、自由基起始劑。
作為光聚合起始劑,例如可列舉:苯乙酮、2,2-二乙氧基苯乙酮、對二甲基苯乙酮、對二甲胺基苯丙酮、二氯苯乙酮、三氯苯乙酮、對三級丁基苯乙酮等苯乙酮類;二苯甲酮、2-氯二苯甲酮、對,對'-雙二甲胺基二苯甲酮等二苯甲酮類;二苯乙二酮、安息香、安息香甲醚、安息香異丙醚、安息香異丁醚等安息香醚類;二苯乙二酮二甲基縮酮、硫、2-氯硫、2,4-二乙基硫 、2-甲基硫、2-異丙基硫等硫化合物;2-乙基蒽醌、八甲基蒽醌、1,2-苯并蒽醌、2,3-二苯基蒽醌等蒽醌類;偶氮二異丁腈、過氧化苯甲醯、過氧化異丙苯等有機過氧化物;及2-巰基苯并咪唑、2-巰基苯并唑、2-巰基苯并噻唑等硫醇化合物。該等化合物可單獨使用其1種,又,亦可組合2種以上使用。光聚合起始劑之摻合量相對於黏合劑樹脂100重量份,較佳為0.05~5.0重量份,更佳為0.1~3.0重量份。
作為自由基起始劑,例如可列舉:作為過氧化酮系化合物、過氧化雙乙醯基系化合物、過氧化氫系化合物、過氧化二烷基系化合物、過氧縮酮系化合物、烷基過氧酸酯系化合物、過碳酸酯系化合物、偶氮雙系化合物等之自由基起始劑。該等化合物可單獨地使用其1種,又,亦可組合2種以上使用。自由基起始劑之摻合量相對於黏合劑樹脂100重量份,較佳為0.05~10.0重量份,更佳為0.1~5.0重量份。
溶劑可較佳地使用水系或有機溶劑系之任一種,例如可列舉:甲苯、乙基苯、三甲基苯、二甲苯等芳香族烴系溶劑;戊烷、己烷、環己烷等脂肪族烴系溶劑;丙酮、甲基乙基酮、甲基異丁基酮、環己酮等酮系溶劑;甲醇、乙醇、異丙醇、乙二醇、二乙二醇、三乙二醇、丙二醇等醇系溶劑;甲基賽路
蘇、乙基賽路蘇、丁基賽路蘇、二乙二醇甲醚(methyl diglycol)、二乙二醇***、二乙二醇丁醚、丙二醇單甲醚等二醇醚系溶劑;乙酸乙酯、乙酸丁酯、丙二醇單甲醚乙酸酯等酯系溶劑;水等。又,作為可用作芳香族烴系溶劑之市售品,可列舉:Solvesso 100、Solvesso 150、Solvesso 200等。該等可單獨地使用,亦可併用2種以上。
溶劑之含量只要根據塗佈方法、所需之塗膜之膜厚而選擇即可,無特別限定,相對於樹脂組成物之固形物成分100重量份,較佳為10~5000重量份,更佳為20~2000重量份。若未達10重量份,則有黏度變高,無法均勻地塗佈之情況,若超過5000重量份,則有無法獲得充分之膜厚之塗膜之情況,此外,就經濟性或揮發性有機化合物之過量使用之觀點而言欠佳。
<<硬化物>>
本發明之硬化物之特徵在於:其係使上述樹脂組成物硬化而成。作為此種硬化物之例,可列舉將上述樹脂組成物塗佈於基材表面,使其硬化而獲得之塗膜。本發明之樹脂組成物可減少其中所含之無機氧化物微粒子分散液中之分散劑之含量,且使無機氧化物微粒子充分地分散。因此,使該樹脂組成物硬化而獲得之塗膜具有良好之光學特性及較高之可靠性。
塗膜之形成方法無特別限定,可列舉於將樹脂組成物塗佈於基材之至少一表面後,進行加熱而使其硬化之方法等。作為將樹脂組成物塗佈於基材表面之方法,例如可列舉:棒式塗佈法、旋轉塗佈法、噴霧塗佈法、浸漬塗佈法、噴嘴塗佈法、凹版塗佈法、逆輥塗佈法、模嘴塗佈法、氣刀塗佈法、刮刀塗佈法、桿式塗佈法、淋幕式塗佈法、刀式塗佈法、傳送輥塗佈法、擠壓式塗佈法、含浸塗佈法、接觸塗佈法、壓延塗佈法、擠出塗佈法等。
所塗佈之樹脂組成物之硬化條件無特別限定,加熱溫度較佳為80~300℃,更佳為90~120℃。又,加熱時間較佳為5~300秒,更佳為20~120秒。
若加熱時間未達5秒,則有造成硬化不良之情況,若超過300秒,則根據基材之材質而有基材之形狀受損之情況,又,步驟所需之時間變長,因此就生產性之觀點而言亦欠佳。
硬化後之塗膜之厚度無特別限定,較佳為0.1~30μm,更佳為0.3~20μm。若厚度未達0.1μm,則有塗膜之平滑性變得不充分之情況,若超過30μm,則有因內部應力之增加而對於基材之密接性變得不充分之情況。
<基材>
基材之材質無特別限定,可列舉:樹脂、無機材料、紙、聚矽氧等半導體製作基板。
作為樹脂,可列舉:聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯等聚酯、聚乙烯、聚丙烯、聚甲基戊烯等聚烯烴、環烯烴、聚苯乙烯、聚四氟乙烯、PMMA、尼龍6、尼龍66等聚醯胺、聚碳酸酯、聚乙酸乙烯酯、聚醯亞胺、ABS樹脂等。該等中,就經濟性、加工容易性之觀點而言,較佳為聚酯。作為無機材料,可列舉:玻璃、石英、陶瓷、Ni、Cu、Cr、Fe等金屬基板、ITO等導電基材等。
上述硬化物可以光學塗佈塗膜、光學構件或成形體之形式較佳地用於光學裝置。作為光學裝置之具體例,例如可列舉:有機EL照明、有機EL顯示器、觸控面板、液晶顯示器、CMOS影像感測器等。
[實施例]
以下,舉出實施例對本發明進行說明,但本發明不限定於以下之實施例。以下,只要無特別說明,則「部」或「%」分別表示「重量份」或「重量%」。
(1)使用材料
(1-1)無機氧化物微粒子
氧化鋯(第一稀元素化學工業股份有限公司製造,UEP-50,平均一次粒徑20nm)
氧化鋯(第一稀元素化學工業股份有限公司製造,UEP-100,平均一次粒徑10nm)
氧化鈦(日本Aerosil公司製造,P90,平均一次粒徑13nm)
(1-2)分散劑
聚醚磷酸酯系分散劑(楠本化成股份有限公司製造,Disparlon PW-36,有效成分50%)
(1-3)烷氧基矽烷化合物
3-甲基丙烯醯氧基丙基三甲氧基矽烷(信越化學工業股份有限公司製造,KBM-503)
3-環氧丙氧基丙基三甲氧基矽烷(信越化學工業股份有限公司製造,KBM-403)
苯基三甲氧基矽烷(信越化學工業股份有限公司製造:KBM-103)
(1-4)溶劑
丙二醇單甲醚乙酸酯(大賽璐股份有限公司製造,PGMEA)
甲基異丁基酮(昭和化學公司製造,MIBK)
環戊酮(日本瑞翁公司製造,CPN)
丙二醇單甲醚(日本乳化劑股份有限公司製造,PGME)
(1-5)黏合劑樹脂
茀系丙烯酸酯(Osaka Gas Chemicals公司製造,OGSOL EA-0250P)
聚矽氧烷1(合成例1中製造)
(1-6)聚合起始劑
Omnirad127(IGM Resins B.V.公司製造)
(1-7)調平劑
BYK-301(BYK Chemie公司製造)
將各溶劑之漢森溶解度參數示於表1。
再者,CPN/PGME表示將環戊酮與丙二醇單甲醚以50:50(重量基準)之比率混合而成之溶劑。
(2)實施例1~11、比較例1~3
以表2所示之摻合量將無機氧化物微粒子、分散劑、烷氧基矽烷化合物、及溶劑混合。繼而,使用介質型分散機(珠磨機)使該混合物分散,獲得無機氧化物微粒子分散液。珠磨機之處理條件係設為混合物之添加總重量350g、珠粒直徑50μm、旋轉速度10m/秒、分散時間180分鐘。
利用後述之方法,測定所獲得之分散液中之無機氧化物微粒子之平均粒徑及保存穩定性。將結果示於表2。再者,表2中,分散劑、烷氧基矽烷化合物、及溶劑之摻合量表示相對於無機氧化物微粒子100重量份之重量份。
(3)微粒子分散液之評價方法
(3-1)平均粒徑
對於實施例及比較例之分散液,使用Malvern公司製造之Zetasizer Nano ZS,基於利用動態光散射法測定之散射強度分佈,算出Z-平均粒徑。
(3-2)保存穩定性
對於實施例及比較例之分散液,藉由目視確認製造後靜置1天後之流動性,將具有與剛製造後相同之流動性者評價為「○」。再者,由於比較例1~3中產生
沈澱,故而無法評價保存穩定性。
如表2所示,實施例1~11之分散液中,無機氧化物微粒子之平均粒徑為40nm以下,獲得充分之分散性,保存穩定性亦良好。不含有分散劑之比較例1、不含有烷氧基矽烷化合物之比較例2、不滿足溶劑之要件之比較例3中,無法使無機氧化物微粒子充分地分散,平均粒徑較大。比較例1~3中產生沈澱。
(4)合成例1(黏合劑樹脂之合成)
將3-甲基丙烯醯氧基丙基三甲氧基矽烷(信越化學工業股份有限公司製造,KBM-503)與苯基三甲氧基矽烷(信越化學工業股份有限公司製造,KBM-103)以莫耳比為90:10之方式混合,利用MIBK稀釋至50重量%,添加烷氧基矽烷合計量之3當量之水。滴加烷氧基矽烷合計量之0.05當量之20重量%之氫氧化鈉水溶液,於60℃加熱3小時。向反應後之溶液添加水,進行3次之去除分液步驟,添加硫酸鈉使其脫水。其後,利用蒸發器使其濃縮,獲得聚矽氧烷1。藉由GPC測定所獲得之聚矽氧烷1之分子量,結果重量平均分子量為3300。
(5)製造例1(無機氧化物微粒子分散液之製造)
將作為無機氧化物微粒子之UEP50 100重量份、作為分散劑之PW-36 10重量
份、作為烷氧基矽烷化合物之KBM-503 10重量份、作為溶劑之PGME 120重量份混合。繼而,使用介質型分散機(珠磨機)使該混合物分散,獲得無機氧化物微粒子分散液。珠磨機之處理條件係設為混合物之添加總重量350g、珠粒直徑50μm、旋轉速度10m/秒、分散時間180分鐘。所獲得之無機氧化物微粒子分散液之平均粒徑為40nm,製造後靜置1天後亦具有與剛製造後相同之流動性。
(6)實施例12~18、比較例4~5
將下述表3所示之各成分混合,獲得塗佈用樹脂組成物。表3之摻合量表示重量比,溶劑以外係固形物成分之數值。使用棒式塗佈機(No.8)將所獲得之塗佈用樹脂組成物塗佈於玻璃基材上,於熱風乾燥機內以110℃加熱40秒而使其硬化,形成膜厚8μm之塗膜,獲得構件。將構件冷卻至室溫,使用冷卻至室溫之構件作為試片,利用後述之方法對塗膜外觀、折射率、全光線透過率、霧度值、及可靠性試驗後之塗膜外觀進行評價。將評價結果示於表3。
(7)塗膜之評價方法
(7-1)塗膜外觀
對上述所製作之試片之塗膜之狀態進行目視觀察,基於以下之基準進行評價。
良好:無凝聚物或不均而為均勻之塗膜
變白:局部地發生微粒子凝聚而產生變白。
(7-2)折射率
對於上述所製作之試片之折射率,使用橢圓光譜偏光儀(J.A.Woollam Japan股份有限公司製造,M-2000C),測定550nm時之折射率。
(7-3)全光線透過率、霧度值
對於上述所製作之試片之全光線透過率、霧度值,依據JIS K7150,使用霧度計(Suga Test Instruments公司製造,HGM-2B)測定。
(7-4)可靠性試驗後之塗膜外觀之評價
使上述所製作之試片暴露於溫度85℃、相對濕度85%之濕熱烘箱中,觀察500小時後之塗膜外觀,確認有無裂痕。
如表3所示,實施例12~18中,可於基材上形成良好之塗膜,塗膜之耐久性較高,折射率、全光線透過率、霧度值亦良好。比較例4中所使用之微粒子分散液中不含有烷氧基矽烷化合物,無法使無機氧化物微粒子充分地分散,因此塗膜變白,光學特性亦變差。比較例5中,雖可形成塗膜,但由於所使用之製造例1之微粒子分散液中含有較多之分散劑,故而塗膜之可靠性較低。
Claims (6)
- 一種無機氧化物微粒子分散液之製造方法,其包括:將下述(A)~(D)成分混合成混合物之步驟:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)選自由聚丙烯酸系分散劑、多羧酸系分散劑、磷酸系分散劑、及聚矽氧系分散劑所組成之群中之至少1種分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數(Hansen solubility parameter)之氫鍵項(dH)為11以下且極性項(dP)為4以上之溶劑;及將該混合物濕式粉碎之步驟;相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量為5~40重量份;相對於(A)無機氧化物微粒子100重量份,(B)分散劑之摻合量為0.25~8重量份。
- 如請求項1所述之無機氧化物微粒子分散液之製造方法,其中,(B)分散劑與(C)烷氧基矽烷化合物之重量比為20:80~5:95。
- 一種無機氧化物微粒子分散液,其含有下述(A)~(D)成分:(A)選自由氧化鋯(ZrO2)、氧化鈦(TiO2)、及鈦酸鋇(BaTiO3)所組成之群中之至少1種無機氧化物微粒子、(B)選自由聚丙烯酸系分散劑、多羧酸系分散劑、磷酸系分散劑、及聚矽氧系分散劑所組成之群中之至少1種分散劑、(C)烷氧基矽烷化合物、及(D)漢森溶解度參數之氫鍵項(dH)為11以下且極性項(dP)為4以上之 溶劑;且(B)分散劑與(C)烷氧基矽烷化合物之重量比為20:80~5:95;相對於(A)無機氧化物微粒子100重量份,(B)分散劑與(C)烷氧基矽烷化合物之總量為5~40重量份;相對於(A)無機氧化物微粒子100重量份,(B)分散劑之摻合量為0.25~8重量份。
- 一種樹脂組成物,其含有請求項3所述之無機氧化物微粒子分散液、及黏合劑樹脂。
- 如請求項4所述之樹脂組成物,其中,固形物成分中之無機氧化物微粒子之含量為30重量%以上。
- 一種硬化物,其係使請求項4或5所述之樹脂組成物硬化而成。
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