TWI543987B - A fluorine-based surface treatment agent for vapor deposition, and an article to be vapor-treated with the surface treatment agent - Google Patents

A fluorine-based surface treatment agent for vapor deposition, and an article to be vapor-treated with the surface treatment agent Download PDF

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TWI543987B
TWI543987B TW101143978A TW101143978A TWI543987B TW I543987 B TWI543987 B TW I543987B TW 101143978 A TW101143978 A TW 101143978A TW 101143978 A TW101143978 A TW 101143978A TW I543987 B TWI543987 B TW I543987B
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Taiwan
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group
integer
surface treatment
treatment agent
fluorine
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TW101143978A
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TW201335167A (zh
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Yuji Yamane
Noriyuki Koike
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Shinetsu Chemical Co
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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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    • C09K3/00—Materials not provided for elsewhere
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
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    • B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
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    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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    • C03C17/23—Oxides
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    • C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/32—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with synthetic or natural resins
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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    • C08G2650/48—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing halogen containing fluorine, e.g. perfluropolyethers
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Description

蒸鍍用氟系表面處理劑及以該表面處理劑蒸鍍處理之物品
本發明係關於包含含有氟氧伸烷基之聚合物改質矽烷之表面處理劑，詳言之，係關於可形成撥水撥油性、低動摩擦性優異之被膜之以特定比例包含含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物、及重量平均分子量比其大之含有氟氧伸烷基之聚合物之表面處理劑，以及以該表面處理劑處理之物品。
近年來，以行動電話之顯示器為代表，已加速畫面之觸控面板化。然而，觸控面板之畫面大部分為外露者，以手指或臉頰等直接接觸之機會較多，而容易附著皮脂等髒污成為問題。因此，為了使外觀或辨識性良好故對於顯示器之表面不易附著指紋之技術、或使髒污容易脫落之技術之要求逐年增高。以往之撥水撥油劑雖然撥水撥油性高，可形成髒污擦拭性優異之膜，但具有每次製膜耐久性能大為不同之缺點，又，由於處理劑彼此會凝聚，故難以獲得平滑之膜。為此，期待開發出可形成安定且高性能之膜之處理劑或處理方法。
一般而言，含有氟氧伸烷基之化合物由於其表面自由能極小，故具有撥水撥油性、耐藥品性、潤滑性、脫模性、防污性等。利用該性質，工業上已廣泛利用於紙、纖維等之撥水撥油防污劑、磁性儲存介質之滑劑、精密設備之 防油劑、脫模劑、化妝料、保護膜等。然而，此性質同時意味著對其他基材為非黏著性、非密著性，即使塗佈於基材表面，仍難以使其被膜密著於基材上。
另一方面，作為使玻璃或布等之基材表面與有機化合物結合者，矽烷偶合劑為被充分悉知者，且廣泛利用作為各種基材表面之塗覆劑。矽烷偶合劑於一分子中具有有機官能基與反應性矽烷基(一般為烷氧基矽烷基)。烷氧基矽烷基係藉由空氣中之水分等引起自我縮合而形成被膜。該被膜藉由烷氧基矽烷基與玻璃或金屬等之表面化學性．物理性結合而成為具有耐久性之強固被膜。
至於具有該等者，於專利文獻1(日本特開2003-238577號公報)中提案含有以下述式表示之直鏈狀全氟氧伸烷基之含有全氟氧伸烷基之聚合物改質矽烷。以該含有全氟氧伸烷基之聚合物改質矽烷處理之玻璃或抗反射膜亦可獲得滑動性、脫模性及耐磨耗性優異之材料，但難以形成安定且高性能之膜。由於非氟基存在於末端基上，故在塗佈步驟中，或塗佈後有非氟基彼此凝聚之情況，對於耐久性造成影響。
(式中，Rf為二價直鏈型全氟氧伸烷基，R為碳數1~4之烷基或苯基，X為水解性基，n為0~2，m為1~5之整數，a為2或3)。
[先前技術文獻] [專利文獻]
[專利文獻1]日本特開2003-238577號公報
本發明係鑑於上述情況而完成者，其目的係提供一種可形成安定且高性能之撥水撥油膜之蒸鍍用氟系表面處理劑及以該表面處理劑予以表面處理之物品。
氟系表面處理劑具有水解性基時，於基板上設置SiO2層作為底塗，於其上塗佈該氟系表面處理劑。塗佈方法已知以真空蒸鍍法蒸鍍氟系表面處理劑者，比將基板浸漬於處理劑中之浸漬塗佈，可形成耐久性更優異之被膜。
本發明人等如先前之上述，提案兩末端具有水解性基之含有全氟伸烷基之聚合物改質矽烷(日本特開2003-238577號公報：專利文獻1)，但由以該聚合物改質之矽烷作為主成分之表面處理劑形成之膜，處理劑彼此容易凝聚，若未控制處理條件則無法獲得高性能之膜。
主鏈上具有氟氧伸烷基構造，且分子鏈之兩末端含有水解性基之聚合物，烷氧基矽烷基彼此會相互作用，且聚合物會彼此凝聚。以原子力顯微鏡觀察蒸鍍後之表面時，會有觀測到單分子膜(10nm)以上之凹凸之情況。即使 使用單末端官能性處理劑亦引起同樣現象。
因此，本發明人等為解決上述問題而積極檢討之結果，發現將無官能基聚合物添加於含有末端具有水解性基且主鏈上具有氟氧伸烷基構造之聚合物之氟系表面處理劑中，可解決凝聚之問題，因而完成本發明。
據此，本發明提供下述蒸鍍用氟系表面處理劑及以該表面處理劑進行表面處理之物品。
[1]
一種蒸鍍用氟系表面處理劑，其包含含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物，及重量平均分子量比該含有氟氧伸烷基之聚合物改質之矽烷及/或其部分水解縮合物大之含有氟氧伸烷基之聚合物，且含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物與含有氟氧伸烷基之聚合物之混合質量比為6：4~9：1。
[2]
如[1]項所記載之蒸鍍用氟系表面處理劑，其中含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物與含有氟氧伸烷基之聚合物之重量平均分子量之比為1：1.5~1：5。
[3]
如[1]或[2]項所記載之蒸鍍用氟系表面處理劑，其中含有氟氧伸烷基之聚合物改質矽烷之含有氟氧伸烷基之聚合物殘基包含3~151個之以下述通式(1)表示之重複單位，
(式中，g在每單位中獨立為1~6之整數)，含有氟氧伸烷基之聚合物含有5~755個之以上述通式(1)表示之重複單位。
[4]
如[1]~[3]項所記載之蒸鍍用氟系表面處理劑，其中含有氟氧伸烷基之聚合物改質矽烷係以下述通式(2)表示，
(式中，Rf為一價氟氧伸烷基或二價氟氧伸烷基，Q為連結Rf基與X基之二價有機基，X為具有複數個水解性基之一價有機基，a為1或2)。
[5]
如[4]項所記載之蒸鍍用氟系表面處理劑，其中前述式(2)之a為1，Rf基係選自由下述通式(3)、(4)及(5)表示之基，
(式中，Y獨立為F或CF3基，m為3~150之整數，d’為1~3之整數)，【化5】C3F7O(CF2CF2CF2O)mCd'F2d'- (4)
(式中，m為3~150之整數，d’為1~3之整數)，
(式中，Y獨立為F或CF3基，Z為H或F基，p、q各為0~150之整數，p+q為3~150之整數，各重複單位可無規鍵結，且d為1~3之整數)。
[6]
如[4]項所記載之蒸鍍用氟系表面處理劑，其中前述式(2)之a為2，Rf基係選自由下述通式(6)、(7)及(8)表示之基，
(式中，Y各獨立為F或CF3基，d’獨立為1~3之整數，e為2~6之整數，r、t各為0~150之整數，s為0~6之整數，r+t+s為3~150，各重複單位可無規地鍵結)，【化8】-CdF2dO(CF2CF2CF2O)m'CdF2d- (7)
(式中，m’為3~150之整數，d為1~3之整數)，
(式中，Y獨立為F或CF3基，d為1~3之整數，p’、q’各為0~150之整數，p’+q’為3~150，各重複單位可無規地鍵結)。
[7]
一種物品，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
[8]
一種光學物品，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
[9]
一種觸控面板，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
[10]
一種抗反射膜，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
[11]
一種SiO2處理玻璃，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
[12]
一種強化玻璃，其係以如[1]~[6]項中任一項所記載之表面處理劑進行蒸鍍處理者。
將本發明之含有含氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物、及重量平均分子量比該含有氟氧伸烷基之聚合物改質之矽烷及/或其部分水解縮合物大之含有氟氧伸烷基之聚合物之表面處理劑於基材上進行蒸鍍處理而形成之被膜，成為平滑之撥水撥油性表面。藉由蒸鍍 處理含有本發明之含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物、及重量平均分子量比含有氟氧伸烷基之聚合物改質之矽烷及/或其部分水解縮合物大之含有氟氧伸烷基之聚合物之表面處理劑，可對各種物品賦予優異之防污性能，保護基材免於藥品等之侵入，可長期保持防污性。
本發明之蒸鍍用氟系表面處理劑包含含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)，及重量平均分子量比該含有氟氧伸烷基之聚合物改質之矽烷及/或其部分水解縮合物(A)大之含有氟氧伸烷基之聚合物(B)，且含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)與含有氟氧伸烷基之聚合物(B)之混合質量比為6：4~9：1之組成物。
本發明之蒸鍍用氟系表面處理劑為包含含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)，及含有氟氧伸烷基之聚合物(B)，將本發明之表面處理劑真空蒸鍍於SiO2處理玻璃(預先蒸鍍或濺鍍SiO2之玻璃)之防污處理玻璃，相較於僅真空蒸鍍含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)之防污處理玻璃，在可形成安定且表面平滑之撥水撥油膜之方面較為優異。
(A)成分之含有氟氧伸烷基之聚合物改質矽烷較好 使用以下述通式(2)表示者。
(式中，Rf為一價氟氧伸烷基或二價氟氧伸烷基，Q為連結Rf基與X基之二價有機基，X為具有複數個水解性基之一價有機基，a為1或2)。
上述式(2)中，Rf為一價氟氧伸烷基或二價氟氧伸烷基，該Rf含有較好3~151個，更好6~101個，又更好25~81個以下述通式(1)表示之重複單位，【化11】-CgF2gO- (1)
(式中，g在每單位中獨立為1~6之整數)。又，各重複單位g值可互為不同，較好g為1~4之整數。
以上述通式表示之重複單位列舉為例如下述之單位等。又，上述Rf基可以該等重複單位之單一種構成，亦可為兩種以上之組合。
-CF2O-
-CF2CF2O-
-CF2CF2CF2O-
-CF(CF3)CF2O-
-CF2CF2CF2CF2O-
-CF2CF2CF2CF2CF2CF2O-
-C(CF3)2O-
上述式(2)中，a為1時，含上述重複單位之Rf較好為由以下述通式(3)、(4)及(5)表示之基選出之 一價氟氧伸烷基。
(式中，Y獨立為F或CF3基，m為3~150之整數，較好為10~100之整數，d’為1~3之整數，較好為2)，【化13】C3F7O(CF2CF2CF2O)mCd'F2d'- (4)
(式中，m為3~150之整數，較好為10~100之整數，d’為1~3之整數，較好為2)， (式中，Y獨立為F或CF3基，Z為H或F基，p、q各為0~150之整數，較好為10~40之整數，p+q為3~150，較好為20~80，各重複單位可無規鍵結，且d為1~3之整數，較好為1)。
上述式(2)中，a為2時，含上述重複單位之Rf較好為由以下述通式(6)、(7)及(8)表示之基選出之二價氟氧伸烷基。
(式中，Y各獨立為F或CF3基，d’獨立為1~3之整數，較好為2，e為2~6之整數，較好為2~4之整數，r、t各為0~150之整數，較好為20~40之整數，s為0~6之 整數，較好為1~3之整數，r+t+s為3~150，較好為20~80，各重複單位可無規地鍵結)，【化16】-CdF2dO(CF2CF2CF2O)m'CdF2d- (7)
(式中，m’為3~150之整數，較好為20~80之整數，d為1~3之整數，較好為1)，
(式中，Y獨立為F或CF3基，d為1~3之整數，較好為1，p’、q’各為0~150之整數，較好為20~40之整數，p’+q’為3~150，較好為20~80，各重複單位可無規地鍵結)。
上述式(2)中，Q為二價有機基，為Rf基與X基之連結基。較好為可含有由醯胺鍵、醚鍵、酯鍵、乙烯鍵、或二甲基亞矽烷基等二有機亞矽烷基所組成群組選出之一種或兩種以上之構造之未取代或經取代之碳數2~12之二價有機基，較好為可含前述構造之未取代或經取代之碳數2~12之二價烴基。
此處，未取代或經取代之碳數2~12之二價烴基列舉為亞甲基、伸乙基、伸丙基(三亞甲基、甲基伸乙基)、伸丁基(四亞甲基、甲基伸丙基)、六亞甲基、八亞甲基等伸烷基、伸苯基等伸芳基，或該等基之兩種以上之組合(伸烷基．伸芳基等)，以及該等基之氫原子之一部分或全部經氟等之鹵原子取代者等，其中以未取代或經取代之 碳數2~4之烷基、苯基較佳。
該Q列舉為例如下述之基。
(式中，b為2~4之整數，Me為甲基)。
上述式(2)中，X為具有複數個，較好為2~18個，更好為2~9個水解性基之一價有機基。此處，水解性基列舉為甲氧基、乙氧基、丙氧基、丁氧基等碳數1~10之烷氧基，甲氧基甲氧基、甲氧基乙氧基等碳數2~10之烷氧基烷氧基，乙醯氧基等碳數1~10之醯氧基、異丙醯氧基等碳數2~10之烯氧基、氯基、溴基、碘基等鹵基等。其中，以甲氧基、乙氧基、異丙氧基、氯基較佳。
上述水解性基較好鍵結於矽原子上，至於X之構造較好為水解性矽烷基，或具有該水解性矽烷基或水解性矽烷基伸烷基之直鏈狀、分支狀或環狀之矽烷氧基或矽烷基。
至於導入複數個水解性基之有機基X列舉為下述所示者。
(式中，c為2~6之整數)。
上述例示之構造中，雖例示甲氧基作為水解性基，但可為甲氧基以外者，且水解性基亦可彼此不同。
至於以上述式(2)表示之含有氟氧伸烷基之聚合物改質矽烷，連結基Q為下式，
水解性基X為下式者係例示如下述，
該等Q、X之組合並不限於該等，藉由僅變更Q與X，可獲得數種含有氟氧伸烷基之聚合物改質矽烷。任一種處理劑均可發揮本發明之效果。
又，組合上述Q、X以外之Q與X之以上述式(2)表示之含有氟氧伸烷基之聚合物改質矽烷進而列舉為下述構造者。
【化28】HF2C(OC2F4)p(OCF2)q-OCF2CH2OC3H6Si(OCH3)3(p/q=0.9、p+q≒45)
【化29】F3C(OC2F4)p(OCF2)q-OCF2CH2OC3H6Si(OCH3)3(p/q=0.9、p+q≒45)
【化30】(CH3O)3SiC3H6OCH2-CF2(OC2F4)p'(OCF2)q'OCF2-CH2OC3H6Si(OCH3)3(p’/q’=0.9、p’+q’≒45)
【化31】(CH3O)3SiC3H6OCH2-CF2(OC2F4)p'(OCF2)q'OCF2-CH2OC3H6Si(OCH3)3(p’/q’=0.9、p’+q’≒23)
本發明之蒸鍍用氟系表面處理劑亦可含有預先以習知方法使上述含有氟氧伸烷基之聚合物改質矽烷之末端水解性基部分水解，且經縮合獲得之部分水解縮合物作為(A)成分。
又，本發明之蒸鍍用氟系表面處理劑含有含氟氧伸烷基之聚合物(B)。本發明之蒸鍍用氟系表面處理劑中所含有之聚合物由於必須為與含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)相溶性良好之聚合物，故使用含有氟氧伸烷基之聚合物(B)。
含有氟氧伸烷基之聚合物(B)在真空蒸鍍時，可減輕含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)之突沸，故可安定地蒸鍍含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)。又，蒸鍍處理後，可有效地防止含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)彼此之凝聚，可有效地完全被覆表面。該含有氟氧伸烷基之聚合物(B)使用不含矽原子者亦可有效地使用。
另一方面，含有氟氧伸烷基之聚合物(B)由於末端不具有官能基，故不與基材反應，在真空蒸鍍時，會比含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)更先蒸鍍，亦成為耐久性惡化之原因。
此處，藉由使含有氟氧伸烷基之聚合物(B)之重量平均分子量比含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)之重量平均分子量大，尤其為1.5倍以上，在真空蒸鍍時，可使含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)先蒸鍍，含有氟氧伸烷基之聚合物(B)後蒸鍍。
含有氟氧伸烷基之聚合物(B)含有較好5~755個，更好5~300個，又更好10~115個以下述通式(1)表示之重複單位，【化34】-CgF2gO- (1)
(式中，g在每單位中獨立為1~6之整數)。又，各重覆單位之g之值可互為不同，較好g為1~4之整數。
至於以上述通式表示之重複單位列舉為例如下述之單位等。又，該聚合物可單獨以該等重覆單位之一種構成，亦可為兩種以上之組合。
-CF2O-
-CF2CF2O-
-CF2CF2CF2O-
-CF(CF3)CF2O-
-CF2CF2CF2CF2O-
-CF2CF2CF2CF2CF2CF2O-
-C(CF3)2O-
又，含有氟氧伸烷基之聚合物(B)由於可使用市售品，例如以FOMBLIN、DEMNUM、KRYTOX之商標名銷售，故可容易地取得。
此等聚合物舉例為例如下述構造者。
FOMBLIN Y(Solvay Solexis公司製造之商品名，FOMBLIN Y25(重量平均分子量：3,200)、FOMBLIN Y45(重量平均分子量：4,100))
(式中，x、y、z1為滿足上述重量平均分子量之數)。
FOMBLIN Z(Solvay Solexis公司製造之商品名，FOMBLIN Z03(重量平均分子量：4,000)、FOMBLIN Z15(重量平均分子量：8,000)、FOMBLIN Z25(重量平 均分子量：9,500))
(式中，v、w、z2為滿足上述重量平均分子量之數)。
DEMNUM(Daikin工業公司製造之商品名，DEMNUM S20(重量平均分子量：2,700)、DEMNUM S65(重量平均分子量：4,500)、DEMNUM S100(重量平均分子量：5,600)
(式中，z3為滿足上述重量平均分子量之數)。
KRYTOX(DuPont公司製造之商品名，KRYTOX 143AB(重量平均分子量：3,500)、KRYTOX 143AX(重量平均分子量：4,700)、KRYTOX 143AC(重量平均分子量：5,500)、KRYTOX 143AD(重量平均分子量：7,000))
(式中，z4為滿足上述重量平均分子量之數)。
藉由使含有氟氧伸烷基之聚合物(B)之重量平均分子量比含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)之重量平均分子量大，較好為1.5倍以上，雖為可真空蒸鍍之大小即可，但就含有氟氧伸烷基之聚 合物改質矽烷及/或其部分水解縮合物(A)與含有氟氧伸烷基之聚合物(B)之混合性而言，較好為1.5倍以上且5倍以下。再者，就製膜時液體之處理容易而言，較好為1.5倍且以上4倍以下。
此處，含有氟氧伸烷基之聚合物(B)之以AK225(旭硝子公司製造)作為展開溶劑，以凝膠滲透層析儀(GPC)測定之聚苯乙烯換算之重量平均分子量，只要在上述範圍內即無特別限制，但較好為1,500~20,000，最好為2,000~10,000。
本發明之蒸鍍用氟系表面處理劑係上述含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)與含有氟氧伸烷基之聚合物(B)之混合質量比為6：4~9：1，較好為8：2~9：1。含有氟氧伸烷基之聚合物改質矽烷及/或其部分水解縮合物(A)過多時，矽烷彼此容易凝聚，含有氟氧伸烷基之聚合物(B)過多時硬化性惡化。
本發明之蒸鍍用氟系表面處理劑宜含有適當溶劑。該溶劑只要可均勻地溶解上述含有氟氧伸烷基之聚合物改質矽烷及其部分水解縮合物(A)與含有氟氧伸烷基之聚合物(B)者即無特別限制，但可例示為氟改質之脂肪族烴系溶劑(全氟庚烷、全氟辛烷等)、氟改質之芳香族烴系溶劑(1,3-三氟甲基苯等)、氟改質之醚系溶劑(甲基全氟丁基醚、乙基全氟丁基醚、全氟(2-丁基四氫呋喃)等)，氟改質之烷基胺系溶劑(全氟三丁基胺、全氟三戊基胺等)、烴系溶劑(石油揮發油(benzine)、甲苯、二 甲苯等)，酮系溶劑(丙酮、甲基乙基酮、甲基異丁基酮等)。該等中，就溶解性、潤濕性方面而言，宜為氟改質之溶劑，最好為氟改質之醚系溶劑、氟改質之芳香族烴系溶劑。
上述溶劑可單獨使用一種，亦可混合兩種以上使用。
又，本發明之蒸鍍用氟系表面處理劑中，可視需要，在不損及本發明之範圍內調配其他添加劑。具體而言，列舉為水解縮合觸媒，例如有機錫化合物(二丁基錫二甲氧化物、二月桂酸二丁基錫等)、有機鈦化合物(鈦酸四正丁酯等)、有機酸(氟系羧酸、乙酸、甲烷磺酸等)、無機酸(鹽酸、硫酸等)等。該等中，尤其以氟系羧酸、乙酸、鈦酸四正丁酯、二月桂酸二丁基錫較佳。添加量為觸媒量，通常相對於上述(A)成分100質量份，為0.01~5質量份，最好為0.1~1質量份。
本發明之蒸鍍用氟系表面處理劑可藉由均勻混合上述各成分之特定量而調製。
本發明之氟系表面處理劑可藉由習知蒸鍍處理對基材施與。蒸鍍處理時之加熱方法可為電阻加熱方式，亦可為電子束加熱方式，並無特別限制。又，蒸鍍後之硬化溫度隨硬化方法而不同，但宜為室溫至200℃之範圍。硬化濕度就促進反應而言宜在加濕下進行。另外，硬化被膜之膜厚係依基材之種類適當選定，但通常為0.1~30nm，最好為5~20 nm。
以本發明之蒸鍍用氟系表面處理劑處理之基材並無特 別限制，可為紙、布、金屬及其氧化物、玻璃、塑膠、陶瓷、石英等各種材質。本發明之蒸鍍用氟系表面處理劑可對前述基板賦予撥水撥油性。尤其，可適當地使用作為經SiO2處理之玻璃或薄膜之表面處理劑。
以本發明之蒸鍍用氟系表面處理劑處理之物品列舉為汽車導航、平板個人電腦、智慧型手機、行動電話、數位相機、數位錄影機、PDA、可攜式影音播放器、汽車音響、遊戲機、眼鏡鏡片、相機鏡片、鏡片濾波器、太陽眼鏡、照胃鏡等醫療用設備、影印機、PC、液晶顯示器、有機EL顯示器、電漿顯示器、觸控面板顯示器、保護膜、抗反射膜等光學物品。本發明之蒸鍍用氟系表面處理劑由於可防止指紋及皮脂附著於前述物品，且進而賦予刮傷防止性，故作為觸控面板顯示器、抗反射膜等撥水撥油層尤其有用。
[實施例]
以下列示實施例及比較例，更詳細說明本發明，但本發明並不由下述實施例所限制。
[實施利1~11、比較例1~9]
準備下述化合物作為含有氟氧伸烷基之聚合物改質矽烷。
化合物1
化合物2
【化40】HF2C(OC2F4)p(OCF2)q-OCF2CH2OC3H6Si(OCH3)3 (p/q=0.9，p+q≒45，重量平均分子量：4,400)
化合物3
【化41】F3C(OC2F4)p(OCF2)q-OCF2CH2OC3H6Si(OCH3)3(p/q=0.9，p+q≒45，重量平均分子量：4,400)
化合物4
【化42】(CH3O)3SiC3H6OCH2-CF2(OC2F4)p'(OCF2)q'OCF2-CH2OC3H6Si(OCH3)3(p’/q’=0.9，p’+q’≒45，重量平均分子量：4,600)
化合物5
【化43】(CH3O)3SiC3H6OCH2-CF2(OC2F4)p'(OCF2)q'OCF2-CH2OC3H6Si(OCH3)3(p’/q’=0.9，p’+q’≒23，重量平均分子量：2,600)
含有氟氧伸烷基之聚合物係使用下列者。
FOMBLIN Z03(Solvay Solexis公司製造)重複單位：約45，重量平均分子量：4,000
FOMBLIN Z15(Solvay Solexis公司製造)重複單位：約90，重量平均分子量：8,000
FOMBLIN Z25(Solvay Solexis公司製造)重複單位：約100，重量平均分子量：9,500
表面處理劑之調製及硬化被膜之形成
以濃度成為20質量%之方式將表1所示之含有氟氧伸烷基之聚合物改質矽烷與含有氟氧伸烷基之聚合物之9：1(質量比)混合物溶解於Novec 7200(3M公司製造)中，調製表面處理劑。於最表面經15nm SiO2處理之玻璃(CORNING公司製造Gorilla)上，真空蒸鍍各表面處理劑5μL(處理條件為壓力：2.0×10-2Pa、加熱溫度：700℃)，在25℃、濕度50%之環境下硬化24小時，形成硬化被膜(膜厚：約10nm)，製作試驗體。
以下述方法評價所得硬化被膜。結果一併列於表1。
[撥水撥油性之評價]
使用上述製作之試驗體，使用接觸角計DropMaster(協和界面科學公司製造)，測定硬化被膜對水之接觸角(撥水性)及對油酸之接觸角(撥油性)。
[表面粗糙度Ra之評價]
以下述所示之原子間力顯微鏡觀察上述製作之試驗體之塗佈表面的粗糙度Ra。
裝置名稱：SPA-400(SII科技公司製造)
測定模式：DFM(輕敲式(Tapping Mode))
懸臂(cantilever)：SI-DF20(無鋁塗層)
測定範圍：5μm×5μm
[不良率]
使用下述所示之裝置，進行上述製作之試驗體之鹽水噴霧試驗，以與上述撥水撥油性之評價相同之方法測定鹽水噴霧試驗後之水接觸角，接觸角低於100度之樣品記為不良。又，試驗係對每一處理劑進行10次，以(不良樣品數)/10×100作為不良率。
裝置名稱：鹽水噴霧試驗機SQ-800-ST(板橋理化工業公司製造)
鹽水條件：35℃ 5質量% NaCl水溶液噴霧
試驗時間：72小時
由上述結果可知，比較例1~5之含有氟氧伸烷基之聚合物改質矽烷單獨之表面處理劑，聚合物彼此凝聚，表面粗糙度超過10nm，但在含有氟氧伸烷基之聚合物改質矽烷與含有氟氧伸烷基之聚合物之合計中混合10質量%之含有氟氧伸烷基之聚合物之實施例1~11之表面處理劑，可抑制聚合物彼此之凝聚，可安定地形成表面平滑之撥水撥油表面。又，如於比較例6~9之表面處理劑所見，含有氟氧伸烷基之聚合物之重量平均分子量與含有氟氧伸烷基之聚合物改質矽烷之重量平均分子量相等以下之情況下，無法獲得該效果。
表面平滑之實施例1~11之硬化被膜之鹽水噴霧試驗前後之表面特性幾乎沒有改變，但表面凹凸之比較例1~9之硬化被膜經鹽水噴霧試驗後，水接觸角大幅降低。比較例1~9中，即使設置平均10nm之硬化被膜層，仍有膜較厚部分與較薄部分，隨著部位而無法完全被覆基材，會因鹽水等之浸入而入侵底塗層之SiO2層。為了完全被覆SiO2層，雖亦考慮增加處理劑之塗佈量，但會有使玻璃之反射率下降，透射率降低之情況故較不佳。
[產業上之可能利用性]
本發明之包含含有氟氧伸烷基之聚合物改質矽烷及其部分水解縮合物及含有氟氧伸烷基之聚合物之表面處理劑可獲得撥水撥油性優異、平滑之硬化被膜。因此，本發明之表面處理劑尤其於觸控面板顯示器、抗反射膜等推定會附著油脂且辨識性重要之用途中極為有效。

Claims (12)

  1. 一種蒸鍍用氟系表面處理劑，其包含(A)經含有氟氧伸烷基之聚合物改質的含水解性基之矽烷及/或其部分水解縮合物，及(B)重量平均分子量比前述成分(A)大之含有氟氧伸烷基之聚合物，前述成分(A)與成分(B)之混合質量比為6：4~9：1，前述成分(A)與成分(B)之重量平均分子量之比為1：1.5~1：5，且前述成分(A)之矽烷係以下述通式(2)表示， 式中，a為1或2；a為1時，Rf基係選自由下述通式(3)、(4)及(5)表示之基； 式中，Y獨立為F或CF3基，m為3~150之整數，d’為1~3之整數；C3F7O(CF2CF2CF2O)mCd'F2d'- (4)式中，m為3~150之整數，d’為1~3之整數； 式中，Y獨立為F或CF3基，Z為H或F基，p、q各為0~150之整數，p+q為3~150之整數，各重複單位可無規鍵結，且d為1~3之整數；或者 a為2時，Rf基係選自由下述通式(6)、(7)及(8)表示之基； 式中，Y各獨立為F或CF3基，d’獨立為1~3之整數，e為2~6之整數，r、t各為0~150之整數，s為0~6之整數，r+t+s為3~150，各重複單位可無規地鍵結；-CdF2dO(CF2CF2CF2O)m'CdF2d- (7)式中，m’為3~150之整數，d為1~3之整數； 式中，Y獨立為F或CF3基，d獨立地為1~3之整數，p’、q’各為0~150之整數，p’+q’為3~150，各重複單位可無規地鍵結；Q為含有選自由醯胺鍵、醚鍵、酯鍵、乙烯鍵、及二有機亞矽烷基所組成群組之一種或兩種以上之構造的未取代或經取代之碳數2~12之二價烴基，X為一價有機基，其具有含水解性基之矽烷及複數個水解性基；前述成分(B)之含有氟氧伸烷基之聚合物，係含有選自由以下重複單位所組成群組之一種或兩種以上之組合的重複單位，且末端不具有水解性基： -CF2O-、-CF2CF2O-、-CF2CF2CF2O-、-CF(CF3)CF2O-、-CF2CF2CF2CF2O-、-CF2CF2CF2CF2CF2CF2O-、及-C(CF3)2O-，且該重複單位之數目為5~755個。
  2. 如申請專利範圍第1項之氟系表面處理劑，其中Q係選自由下述所組成之群組： -CH2OCH2CH2- -CH2OCH2CH2CH2- -CF2OCH2CH2CH2- 式中，Me為甲基。
  3. 如申請專利範圍第1項之氟系表面處理劑，其中X為水解性矽烷基，或具有水解性矽烷基或水解性矽烷基伸烷基之直鏈狀、分支狀或環狀之矽烷氧基或矽烷基。
  4. 如申請專利範圍第1項之氟系表面處理劑，其中X為以下述式之任一者表示之具有鍵結於烷氧基之矽烷基之基：-Si(OR)3 式中，c為2~6之整數，OR為碳數1~10之烷氧基、 碳數2~10之烷氧基烷氧基、碳數2~10之烯氧基、或碳數1~10之醯氧基。
  5. 如申請專利範圍第1項之氟系表面處理劑，其中前述成分(B)之含有氟氧伸烷基之聚合物，係選自由具有式(9)之聚合物及具有式(10)之聚合物所組成群組： 式中，x、y及z係滿足使前述含有氟氧伸烷基之聚合物的重量平均分子量成為1,500~20,000之值。
  6. 如申請專利範圍第1項之氟系表面處理劑，其係進一步含有氟改質之醚溶劑或氟改質之芳香族烴溶劑。
  7. 一種物品，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
  8. 一種光學物品，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
  9. 一種觸控面板，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
  10. 一種抗反射膜，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
  11. 一種SiO2處理玻璃，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
  12. 一種強化玻璃，其係以如申請專利範圍第1~6項中任一項之表面處理劑進行蒸鍍處理者。
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JP2016094669A (ja) 2016-05-26
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CN103146305A (zh) 2013-06-12
CN103146305B (zh) 2017-03-01
TW201335167A (zh) 2013-09-01
JP6044701B2 (ja) 2016-12-14
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US20130136928A1 (en) 2013-05-30
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