TWI676653B - 形成透明導電膜用保護膜之組成物 - Google Patents
形成透明導電膜用保護膜之組成物 Download PDFInfo
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- TWI676653B TWI676653B TW103144081A TW103144081A TWI676653B TW I676653 B TWI676653 B TW I676653B TW 103144081 A TW103144081 A TW 103144081A TW 103144081 A TW103144081 A TW 103144081A TW I676653 B TWI676653 B TW I676653B
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- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
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- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
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- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
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- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/103—Esters of polyhydric alcohols or polyhydric phenols of trialcohols, e.g. trimethylolpropane tri(meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/104—Esters of polyhydric alcohols or polyhydric phenols of tetraalcohols, e.g. pentaerythritol tetra(meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0638—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with at least three nitrogen atoms in the ring
- C08G73/0644—Poly(1,3,5)triazines
-
- C—CHEMISTRY; METALLURGY
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Abstract
Description
本發明係關於形成透明導電膜用保護膜之組成物。
目前,作為透明導電膜材料係主要使用有銦錫氧化物(ITO)、銦鋅氧化物(IZO)等,此等係成為顯示良好的光學透明性及導電性之標準材料。但,為了得到此等之無機氧化物膜,係需要濺鍍、高真空下、高溫退火等之複雜的製程。因而需要特殊的機器,而有花費成本的問題。
電子裝置,係正在進行以塑膠基板等的使用所致之可撓性化、輕量化,而需要對於彎曲等之物理性應力的耐久性。雖對於可撓性基板之ITO或IZO的製膜技術亦正在探討,但無機氧化物之脆弱性且容易損傷的性質仍未獲得改善。
近年來,伴隨著可撓性化的進行,而開發出一種具有導電性奈米結構(金屬奈米粒子或金屬奈米線之滲流結構(percolation structure)、金屬網目結構等)的透明
導電膜。若使用金屬奈米粒子或金屬奈米線分散液,則可藉由濕式製程而製作透明導電膜(專利文獻1~3)。
具有導電性奈米結構的透明導電膜之電阻,係能夠無須複雜的製程地僅以增加所含有之金屬量而降低。但,因金屬量的增加,而有引起藉由光的漫射所導致之白濁化而喪失光學透明性,又由於是金屬因此會因表面的劣化或結構體的破壞而喪失導電性之問題。
[專利文獻1]日本特開2009-505358號公報
[專利文獻2]日本特開2013-77234號公報
[專利文獻3]日本特開2010-108877號公報
[專利文獻4]國際公開第2010/128661號
本發明係鑑於上述情事而完成者,其目的為提供一種賦予可改善具有導電性奈米結構的透明導電膜之視認性,進而具有透明導電膜之劣化抑制效果的透明導電膜用保護膜之組成物。
本發明者們為了達成上述目的屢經努力探討
的結果發現:包含特定的含三嗪環之超枝化聚合物及分子量1,000以上之交聯劑的組成物,係賦予可改善透明導電膜之視認性,該膜係由於具有高溫高濕耐性,因此適合作為透明導電膜用保護膜,而完成本發明。
亦即,本發明係提供下述形成透明導電膜用保護膜之組成物。
[式中,R1~R92係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基,R93及R94係表示氫原子或碳數1~10之烷基,W1及W2係各自獨立表示單鍵、-C(R95)(R96)-(R95及R96係各自獨立表示氫原子或碳數1~10之烷基,於R95及R96皆為烷基時,此等係可相互鍵結而與鍵結此等之碳原子一起形成環)、-C(O)-、-O-、-S-、-S(O)-、-S(O)2-或-N(R97)-(R97係表示氫原子或碳數1~10之烷基),X1及X2係各自獨立表示單鍵、碳數1~10之伸烷基或以式(14)所表示之基;
(式中,R98~R101係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基,Y1及Y2係各自獨立表示單鍵或碳數1~10之伸烷基)]}。
2.如1之組成物,其中,交聯劑A為多官能(甲基)丙烯酸化合物。
3.如1或2之組成物,其中,相對於前述含三嗪環之超枝化聚合物100質量份而言,包含0.1~30質量份之交聯劑A。
4.如1~3中任一項之組成物,其中,進一步含有分子量未達1,000之交聯劑B。
5.如4之組成物,其中,交聯劑B為多官能(甲基)丙烯酸化合物。
6.如4或5之組成物,其中,相對於交聯劑A 100質量份而言,包含0.5~400質量份之交聯劑B。
7.如1~6中任一項之組成物,其中,進一步包含溶劑。
8.一種透明導電膜用保護膜,其係使如1~7中任一項之組成物硬化而得。
9.如8之保護膜,其中,透明導電膜係具有導電性奈米結構的透明導電膜。
10.如9之保護膜,其中,導電性奈米結構為銀奈米線。
11.一種透明電極,其係具備透明導電膜與形成於該透明導電膜上之如8之保護膜。
12.一種電子裝置,其係具備透明導電膜與形成於該透明導電膜上之如8之保護膜。
13.如12之電子裝置,其係有機電致發光顯示器。
使用本發明之形成透明導電膜用保護膜之組成物所形成的保護膜,係由於透明性高,折射率亦高,因此可改善透明導電膜之視認性,進而,由於耐熱性、高溫高濕耐性亦高,因此可抑制透明導電膜之劣化。亦即,使用本發明之組成物所製作的保護膜,係可適合利用作為透明導電膜用保護膜。
[第1圖]係合成例1所得到的HB-TmDA40之1H-NMR光譜。
[第2圖]係顯示合成例1所得到的HB-TmDA40之TG-DTA測定結果之圖表。
本發明之形成透明導電膜用保護膜之組成物,係含有包含以下述式(1)所表示的重複單元之含三嗪環之超枝化聚合物。
式中,R及R’係各自獨立表示氫原子、烷基、烷氧基、芳基或芳烷基。
上述烷基之碳數雖無特別限定,但較佳為1~20,若考慮更提高聚合物之耐熱性,則更佳為1~10,再更佳為1~3。此外,該結構係可為直鏈狀、分支狀、環狀之任一者。
烷基之具體例係可列舉:甲基、乙基、n-丙基、異丙基、環丙基、n-丁基、異丁基、s-丁基、t-丁基、環丁基、1-甲基-環丙基、2-甲基-環丙基、n-戊基、1-甲基-n-丁基、2-甲基-n-丁基、3-甲基-n-丁基、1,1-二甲基-n-丙基、1,2-二甲基-n-丙基、2,2-二甲基-n-丙基、1-乙基-n-丙基、環戊基、1-甲基-環丁基、2-甲基-環丁基、3-甲基-環丁基、1,2-二甲基-環丙基、2,3-二甲基-環丙基、1-乙基-環丙基、2-乙基-環丙基、n-己基、1-甲基-n-戊基、2-甲基-n-戊基、3-甲基-n-戊基、4-甲基-n-戊基、1,1-
二甲基-n-丁基、1,2-二甲基-n-丁基、1,3-二甲基-n-丁基、2,2-二甲基-n-丁基、2,3-二甲基-n-丁基、3,3-二甲基-n-丁基、1-乙基-n-丁基、2-乙基-n-丁基、1,1,2-三甲基-n-丙基、1,2,2-三甲基-n-丙基、1-乙基-1-甲基-n-丙基、1-乙基-2-甲基-n-丙基、環己基、1-甲基-環戊基、2-甲基-環戊基、3-甲基-環戊基、1-乙基-環丁基、2-乙基-環丁基、3-乙基-環丁基、1,2-二甲基-環丁基、1,3-二甲基-環丁基、2,2-二甲基-環丁基、2,3-二甲基-環丁基、2,4-二甲基-環丁基、3,3-二甲基-環丁基、1-n-丙基-環丙基、2-n-丙基-環丙基、1-異丙基-環丙基、2-異丙基-環丙基、1,2,2-三甲基-環丙基、1,2,3-三甲基-環丙基、2,2,3-三甲基-環丙基、1-乙基-2-甲基-環丙基、2-乙基-1-甲基-環丙基、2-乙基-2-甲基-環丙基、2-乙基-3-甲基-環丙基等。
上述烷氧基之碳數雖無特別限定,但較佳為1~20,若考慮更提高聚合物之耐熱性,則更佳為1~10,再更佳為1~3。此外,該烷基部分的結構係可為直鏈狀、分支狀、環狀之任一者。
烷氧基之具體例係可列舉:甲氧基、乙氧基、n-丙氧基、異丙氧基、n-丁氧基、異丁氧基、s-丁氧基、t-丁氧基、n-戊氧基、1-甲基-n-丁氧基、2-甲基-n-丁氧基、3-甲基-n-丁氧基、1,1-二甲基-n-丙氧基、1,2-二甲基-n-丙氧基、2,2-二甲基-n-丙氧基、1-乙基-n-丙氧基、n-己氧基、1-甲基-n-戊氧基、2-甲基-n-戊氧基、3-甲基-n-戊氧基、4-甲基-n-戊氧基、1,1-二甲基-n-丁氧基、1,2-二
甲基-n-丁氧基、1,3-二甲基-n-丁氧基、2,2-二甲基-n-丁氧基、2,3-二甲基-n-丁氧基、3,3-二甲基-n-丁氧基、1-乙基-n-丁氧基、2-乙基-n-丁氧基、1,1,2-三甲基-n-丙氧基、1,2,2-三甲基-n-丙氧基、1-乙基-1-甲基-n-丙氧基、1-乙基-2-甲基-n-丙氧基等。
上述芳基之碳數雖無特別限定,但較佳為6~40,若考慮更提高聚合物之耐熱性,則更佳為6~16,再更佳為6~13。芳基之具體例係可列舉:苯基、α-萘基、β-萘基、1-蒽基、2-蒽基、9-蒽基、1-菲基、2-菲基、3-菲基、4-菲基、9-菲基等。
此外,上述芳基之氫原子的一部分或全部係可以氟、氯、溴、碘等之鹵素原子、碳數1~10之烷基、碳數1~10之烷氧基、硝基、氰基、苯基等取代。取代芳基之具體例係可列舉:o-氯苯基、m-氯苯基、p-氯苯基、o-氟苯基、p-氟苯基、o-甲氧苯基、p-甲氧苯基、p-硝苯基、p-氰苯基、o-聯苯基、m-聯苯基、p-聯苯基等。
芳烷基之碳數雖無特別限定,但較佳為7~20,更佳為7~17,再更佳為7~14。該伸烷基部分係可為直鏈狀、分支狀、環狀之任一者。芳烷基之具體例係可列舉:苄基、苯乙基、1-萘甲基等。
此外,上述芳烷基之氫原子的一部分或全部係可以氟、氯、溴、碘等之鹵素原子、碳數1~10之烷基、碳數1~10之烷氧基、硝基、氰基、苯基等取代。取代芳烷基之具體例係可列舉:p-甲基苯甲基、m-甲基苯甲
基、o-乙基苯甲基、m-乙基苯甲基、p-乙基苯甲基、2-丙基苯甲基、4-異丙基苯甲基、4-異丁基苯甲基等。
式中,Ar係表示由以式(2)~(13)所表示之基所成之群中選出的至少1種之基。
式中,R1~R92係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基。
R93及R94係表示氫原子或碳數1~10之烷基。
W1及W2係各自獨立表示單鍵、-C(R95)(R96)-(R95及R96係各自獨立表示氫原子或碳數1~10之烷基,於R95及R96皆為烷基時,此等係可相互鍵結而與鍵結此等之碳原子一起形成環)、-C(O)-、-O-、-S-、-S(O)-、-S(O)2-或-N(R97)-(R97係表示氫原子或碳數1~10之烷基)。
X1及X2係各自獨立表示單鍵、碳數1~10之伸烷基或以式(14)所表示之基。
式中,R98~R101係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基。Y1及Y2係各自獨立表示單鍵或碳數1~10之伸烷基。
R1~R101所表示的鹵素原子係可列舉:氟原子、氯原子、溴原子、碘原子。此外,以R1~R101所表示的烷基、烷氧基方面雖可列舉與作為R及R’所例示者相同者,但尤以直鏈狀或分支狀者為佳。
碳數1~10之伸烷基係可列舉從作為R及R’所例示者之烷基排除1個氫原子之基,尤以直鏈狀或分支
狀者為佳,具體而言係可列舉:亞甲基、伸乙基、伸丙基、三亞甲基、四亞甲基、五亞甲基等。
尤其,Ar較佳為以式(2)、(5)~(13)所表示之基,更佳為以式(2)、(5)、(7)、(8)、(11)~(13)所表示之基。以式(2)~(13)所表示之基的具體例雖可列舉以下述式所表示者,但並不限定於此等。
此等當中,就可得到更高折射率之聚合物的
觀點而言,更佳為以下述式所表示之基。
本發明所使用之超枝化聚合物,尤其,若考慮對於有機溶劑等之溶解性,則較佳為包含以式(15)所表示的重複單元。
(式中,R、R’及R1~R4係與上述相同)。
就如此之觀點而言,特別適合之重複單元結構係可列舉以下述式(16)所表示者,以下述式(17)所表示之超枝化聚合物最為適合。
(式中,R及R’係與上述相同)。
本發明所使用之超枝化聚合物的重量平均分子量(Mw)雖無特別限定,但較佳為500~500,000,更佳為1,000~100,000。就更提昇耐熱性,並且降低收縮率的觀點而言,Mw的下限較佳為2,000,就更提高溶解性而使所得到的溶液之黏度降低的觀點而言,其上限較佳為50,000,更佳為30,000,再更佳為10,000。另外,於本發明中,Mw係以凝膠滲透層析法(GPC)分析所致之標準苯乙烯換算值。
本發明所使用之含三嗪環之超枝化聚合物,係可藉由專利文獻4所揭示的手法進行製造。
例如,如下述流程1所示般,超枝化聚合物(20),係可使鹵化氰尿醯(cyanuric halide)(18)及m-伸苯基二胺化合物(19)在適當的有機溶劑中進行反應而得到。
(式中,R及R’係與上述相同;X係各自獨立表示鹵素原子)。
如下述流程2所示般,超枝化聚合物(20),亦可由使使用等量之鹵化氰尿醯(18)及m-伸苯基二胺化合物(19)在適當的有機溶劑中進行反應所得到的化合物(20’)進行合成。
(式中,R、R’及X係與上述相同)。
於流程1及2之方法的情況中,各原料之裝入量,雖只要可得到作為目的之聚合物則為任意,但較佳為相對於三嗪化合物(18)1當量而言,二胺化合物(19)0.01~10當量。但,於流程1之方法的情況中,較佳為相對於鹵化氰尿醯(18)2當量而言,避免使用3當量之二胺化合物(19)。藉由錯開官能基之當量而可防止凝膠化物的生成。
為了得到較多具有各種之分子量的三嗪環末端之超枝化聚合物,較佳為相對於鹵化氰尿醯(18)2當量而言,使用未達3當量之二胺化合物(19)。例如,於製作薄膜的情況中,就具有優異的透明性或耐光性的觀點而言,以具有較多三嗪環末端之超枝化聚合物為佳。
為了得到較多具有各種之分子量的三嗪環末
端之超枝化聚合物,較佳為相對於二胺化合物(19)3當量而言,使用未達2當量之鹵化氰尿醯(18)。
如此一來,藉由適當調節二胺化合物(19)或鹵化氰尿醯(18)之量,而可容易地調節所得到的超枝化聚合物之分子量。
上述有機溶劑方面係可使用於該種反應中通常使用的各種溶劑,可列舉例如:四氫呋喃、二噁烷、二甲基亞碸;N,N-二甲基甲醯胺、N-甲基-2-吡咯啶酮、四甲基脲、六甲基磷醯胺、N,N-二甲基乙醯胺、N-甲基-2-哌啶酮、N,N-二甲基乙烯脲、N,N,N’,N’-四甲基丙二酸醯胺、N-甲基己內醯胺、N-乙醯吡咯啶、N,N-二乙基乙醯胺、N-乙基-2-吡咯啶酮、N,N-二甲基丙酸醯胺、N,N-二甲基異丁基醯胺、N-甲基甲醯胺、N,N’-二甲基丙烯脲等之醯胺系溶劑、及此等之混合溶劑。
此等當中,較佳為N,N-二甲基甲醯胺、二甲基亞碸、N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺及此等之混合溶劑,尤以N,N-二甲基乙醯胺、N-甲基-2-吡咯啶酮為佳。
於流程1及流程2之第2階段的反應中,反應溫度雖只要在從所使用之溶劑的熔點至沸點之範圍內適當設定即可,但較佳為0~150℃左右,更佳為60~100℃。尤其,於流程1的反應中,就抑制退火性,提高分支度的觀點而言,反應溫度較佳為60~150℃,更佳為80~150℃,再更佳為80~120℃。
於流程2之第1階段的方法中,反應溫度雖只要在從所使用之溶劑的熔點至溶劑的沸點之範圍內適當設定即可,但較佳為-50~50℃左右,更佳為-20~50℃左右,再更佳為-10~50℃左右,又再更佳為-10~10℃。尤其,於流程2的方法中,較佳為採用由在-50~50℃進行反應之第1步驟、與繼此步驟後在60~150℃進行反應之第2步驟所構成的2階段步驟。
於上述各反應中,各成分之摻合順序雖為任意,但於流程1的反應中,最理想為將鹵化氰尿醯(18)或二胺化合物(19)及包含有機溶劑之溶液加熱至60~150℃,較佳為80~150℃,並在此溫度下,於該溶液中添加二胺化合物(19)或鹵化氰尿醯(18)的方法。
於此情況中,預先溶於溶劑中的成分及之後添加的成分雖哪者皆可,但較佳為於二胺化合物(19)之加熱溶液中添加鹵化氰尿醯(18)的手法。
此外,於流程2的反應中,預先溶於溶劑中的成分及之後添加的成分雖哪者皆可,但較佳為於鹵化氰尿醯(18)之冷卻溶液中添加二胺化合物(19)的手法。之後添加的成分係可純添加,亦可以如上述般之溶於有機溶劑的溶液添加,但若考慮操作的容易度或反應之控制的容易度等,則以後者之手法較為理想。此外,之後添加的成分,係可藉由滴下等緩緩地添加,亦可全量一併添加。
於流程1中,以加熱的狀態將兩化合物進行混合之後,即使於以(無須使溫度階段性地上昇)一階段進
行反應的情況中,亦可不進行凝膠化而得到作為目的之含三嗪環之超枝化聚合物。
此外,於上述流程1及流程2之第2階段的反應中,亦可在聚合時或聚合後添加通常使用的各種之鹼。該鹼之具體例係可列舉:碳酸鉀、氫氧化鉀、碳酸鈉、氫氧化鈉、碳酸氫鈉、乙氧化鈉、乙酸鈉、碳酸鋰、氫氧化鋰、氧化鋰、乙酸鉀、氧化鎂、氧化鈣、氫氧化鋇、磷酸三鋰、磷酸三鈉、磷酸三鉀、氟化銫、氧化鋁、氨、三甲基胺、三乙基胺、二異丙基胺、二異丙基乙基胺、N-甲基哌啶、2,2,6,6-四甲基-N-甲基哌啶、吡啶、4-二甲基胺基吡啶、N-甲基嗎啉等。
鹼之添加量,較佳為相對於鹵化氰尿醯(18)1當量而言,為1~100當量,更佳為1~10當量。另外,此等之鹼亦可製成水溶液而使用。
於任一流程的方法中,於反應結束後,生成物皆可藉由再沉澱法等而容易地純化。
另外,於本發明中,亦可將至少1個末端三嗪環的鹵素原子之一部分以烷基、芳烷基、芳基、烷基胺基、含烷氧矽烷基之烷基胺基、芳烷基胺基、芳基胺基、烷氧基、芳烷基氧基、芳基氧基、酯基等覆蓋(cap)。
此等當中,較佳為烷基胺基、含烷氧矽烷基之烷基胺基、芳烷基胺基、芳基胺基,更佳為烷基胺基、芳基胺基,再更佳為芳基胺基。
上述烷基、烷氧基、芳基及芳烷基方面,係
可列舉與作為R及R’所例示者相同者。
酯基之具體例係可列舉:甲氧基羰基、乙氧基羰基等。
烷基胺基之具體例係可列舉:甲基胺基、乙基胺基、n-丙基胺基、異丙基胺基、n-丁基胺基、異丁基胺基、s-丁基胺基、t-丁基胺基、n-戊基胺基、1-甲基-n-丁基胺基、2-甲基-n-丁基胺基、3-甲基-n-丁基胺基、1,1-二甲基-n-丙基胺基、1,2-二甲基-n-丙基胺基、2,2-二甲基-n-丙基胺基、1-乙基-n-丙基胺基、n-己基胺基、1-甲基-n-戊基胺基、2-甲基-n-戊基胺基、3-甲基-n-戊基胺基、4-甲基-n-戊基胺基、1,1-二甲基-n-丁基胺基、1,2-二甲基-n-丁基胺基、1,3-二甲基-n-丁基胺基、2,2-二甲基-n-丁基胺基、2,3-二甲基-n-丁基胺基、3,3-二甲基-n-丁基胺基、1-乙基-n-丁基胺基、2-乙基-n-丁基胺基、1,1,2-三甲基-n-丙基胺基、1,2,2-三甲基-n-丙基胺基、1-乙基-1-甲基-n-丙基胺基、1-乙基-2-甲基-n-丙基胺基等。
芳烷基胺基之具體例係可列舉:苄基胺基、甲氧基羰基苯甲基胺基、乙氧基羰基苯甲基胺基、p-甲基苯甲基胺基、m-甲基苯甲基胺基、o-乙基苯甲基胺基、m-乙基苯甲基胺基、p-乙基苯甲基胺基、2-丙基苯甲基胺基、4-異丙基苯甲基胺基、4-異丁基苯甲基胺基、萘甲基胺基、甲氧基羰基萘甲基胺基、乙氧基羰基萘甲基胺基等。
芳基胺基之具體例係可列舉:苯基胺基、甲
氧基羰基苯基胺基、乙氧基羰基苯基胺基、萘基胺基、甲氧基羰基萘基胺基、乙氧基羰基萘基胺基、蒽基胺基、芘基胺基、聯苯胺基、聯三苯胺基、茀基胺基等。
含烷氧矽烷基之烷基胺基,係可為含單烷氧矽烷基之烷基胺基、含二烷氧矽烷基之烷基胺基、含三烷氧矽烷之烷基胺基中任一者,其具體例係可列舉:3-三甲氧基矽烷基丙基胺基、3-三乙氧基矽烷基丙基胺基、3-二甲基乙氧基矽烷基丙基胺基、3-甲基二乙氧基矽烷基丙基胺基、N-(2-胺基乙基)-3-二甲基甲氧基矽烷基丙基胺基、N-(2-胺基乙基)-3-甲基二甲氧基矽烷基丙基胺基、N-(2-胺基乙基)-3-三甲氧基矽烷基丙基胺基等。
芳氧基之具體例係可列舉:苯氧基、萘氧基、蒽基氧基、芘基氧基、聯苯氧基、聯三苯氧基、茀基氧基等。
芳烷氧基之具體例係可列舉:苄氧基、p-甲基苯甲基氧基、m-甲基苯甲基氧基、o-乙基苯甲基氧基、m-乙基苯甲基氧基、p-乙基苯甲基氧基、2-丙基苯甲基氧基、4-異丙基苯甲基氧基、4-異丁基苯甲基氧基、α-萘甲基氧基等。
此等之基,係可藉由以賦予對應三嗪環上之鹵素原子的取代基之化合物進行取代而容易地導入,例如,如下述流程3所示般,藉由添加苯胺衍生物使其反應,而可得到於至少1個末端具有苯基胺基之超枝化聚合物(21)。
(式中,R、R’及X係與上述相同)。
此時,進行有機單胺之同時裝入。亦即,在有機單胺的存在下,藉由使鹵化氰尿醯化合物與二胺基芳基化合物進行反應,而可得到超枝化聚合物之剛直性獲得緩和之分支度低之柔軟的超枝化聚合物。藉由該手法所得到的超枝化聚合物,係由於成為對溶劑之溶解性(凝聚抑制)或與交聯劑之交聯性優異者,而特別有利於作為與後述之交聯劑組合的組成物而使用。
在此,有機單胺方面亦可使用烷基單胺、芳烷基單胺、芳基單胺中任一者。
烷基單胺係可列舉:甲基胺、乙基胺、n-丙基胺、異丙基胺、n-丁基胺、異丁基胺、s-丁基胺、t-丁基胺、n-戊基胺、1-甲基-n-丁基胺、2-甲基-n-丁基胺、3-甲基-n-丁基胺、1,1-二甲基-n-丙基胺、1,2-二甲基-n-丙基
胺、2,2-二甲基-n-丙基胺、1-乙基-n-丙基胺、n-己基胺、1-甲基-n-戊基胺、2-甲基-n-戊基胺、3-甲基-n-戊基胺、4-甲基-n-戊基胺、1,1-二甲基-n-丁基胺、1,2-二甲基-n-丁基胺、1,3-二甲基-n-丁基胺、2,2-二甲基-n-丁基胺、2,3-二甲基-n-丁基胺、3,3-二甲基-n-丁基胺、1-乙基-n-丁基胺、2-乙基-n-丁基胺、1,1,2-三甲基-n-丙基胺、1,2,2-三甲基-n-丙基胺、1-乙基-1-甲基-n-丙基胺、1-乙基-2-甲基-n-丙基胺、2-乙基己基胺等。
芳烷基單胺之具體例係可列舉:苄基胺、p-甲氧基羰基苄基胺、p-乙氧基羰基苯基苄基、p-甲基苄基胺、m-甲基苄基胺、o-甲氧基苄基胺等。
芳基單胺之具體例係可列舉:苯胺、p-甲氧基羰基苯胺、p-乙氧基羰基苯胺、p-甲氧基苯胺、1-萘基胺、2-萘基胺、蒽基胺、1-胺基芘、4-聯苯基胺、o-苯基苯胺、4-胺基-p-聯三苯、2-胺基茀等。
於此情況中,有機單胺之使用量,係較佳為相對於鹵化氰尿醯化合物而言,為0.05~500當量,更佳為0.05~120當量,再更佳為0.05~50當量。
於此情況中之反應溫度,就抑制退火性,提高分支度的觀點而言,反應溫度亦較佳為60~150℃,更佳為80~150℃,再更佳為80~120℃。但,有機單胺、鹵化氰尿醯化合物及二胺芳基化合物之3成分的混合,亦可在低溫下進行,於此情況中之溫度,係較佳為-50~50℃左右,更佳為-20~50℃左右,再更佳為-20~10℃。
低溫裝入後,較佳為一氣呵成地(以一階段)昇溫至使其聚合的溫度而進行反應。
此外,亦可在低溫下進行鹵化氰尿醯化合物及二胺芳基化合物之2成分的混合,於此情況中之溫度,係較佳為-50~50℃左右,更佳為-20~50℃左右,再更佳為-20~10℃。低溫裝入後,較佳為添加有機單胺,並一氣呵成地(以一階段)昇溫至使其聚合的溫度而進行反應。此外,在如此之有機單胺的存在下,使鹵化氰尿醯化合物及二胺芳基化合物進行反應的反應,係可使用與上述相同的有機溶劑來進行。
本發明之組成物係含有分子量1,000以上之交聯劑A。藉此,可提高保護膜之膜密度,使高溫高濕耐性提昇。
此外,本發明之組成物,係較佳為進一步含有分子量未達1,000之交聯劑B。藉由添加交聯劑B,而可進一步提高保護膜之膜密度,使高溫高濕耐性更加提昇。交聯劑B,係更佳為分子量900以下者,再更佳為800以下者。
交聯劑A及B係可列舉:作為交聯形成基而具有羥甲基、甲氧基甲基等之交聯形成基的三聚氰胺系化合物、取代脲系化合物、含有環氧基或氧雜環丁烷基等之交聯形成基的化合物、含有封端化異氰酸酯的化合物、具
有酸酐的化合物、具有(甲基)丙烯醯基的化合物、胺基塑料(aminoplast)化合物、酚醛塑料(phenoplast)化合物等。此等當中,就耐熱性或保存安定性的觀點而言,較佳為含有環氧基、封端化異氰酸酯基、(甲基)丙烯基之化合物、尤以具有封端化異氰酸酯基之化合物、或賦予不使用起始劑亦可光硬化的組成物之多官能環氧化合物及/或多官能(甲基)丙烯酸化合物為佳。
另外,此等之多官能化合物雖需要具有至少2個交聯形成基,但較佳為具有3個以上之交聯形成基。
多官能環氧化合物,係只要1分子中具有2個以上環氧基者則無特別限定。該具體例係可列舉:參(2,3-環氧丙基)異氰脲酸酯、1,4-丁二醇二環氧丙基醚、1,2-環氧-4-(環氧乙基)環己烷、甘油三環氧丙基醚、二乙二醇二環氧丙基醚、2,6-二環氧丙基苯基環氧丙基醚、1,1,3-參[p-(2,3-環氧丙氧基)苯基]丙烷、1,2-環己烷二羧酸二環氧丙基酯、4,4’-亞甲基雙(N,N-二環氧丙基苯胺)、3,4-環氧環己基甲基-3,4-環氧環己烷羧酸酯、三羥甲基乙烷三環氧丙基醚、雙酚-A-二環氧丙基醚、季戊四醇聚環氧丙基醚等。
此外,市售品方面亦可使用:至少具有2個之環氧基的環氧樹脂之YH-434、YH-434L(新日鐵住金化學(股)製);具有環氧環己烷結構的環氧樹脂之Epolead GT-401、GT-403、GT-301、GT-302、CELLOXIDE 2021、3000(Daicel(股)製);雙酚A型環氧樹脂之jER(註冊商
標)1001、1002、1003、1004、1007、1009、1010、828(三菱化學(股)製);雙酚F型環氧樹脂之jER(註冊商標)807(三菱化學(股)製);酚酚醛清漆型環氧樹脂之jER(註冊商標)152、154(三菱化學(股)製)、EPPN201、202(以上、日本化藥(股)製);甲酚酚醛清漆型環氧樹脂之EOCN-102、EOCN-103S、EOCN-104S、EOCN-1020、EOCN-1025、EOCN-1027(日本化藥(股)製)、jER(註冊商標)180S75(三菱化學(股)製);脂環式環氧樹脂之Denacol EX-252(Nagase chemteX(股)製)、ARALDITE(註冊商標)CY175、CY177、CY179、CY-182、CY-192、CY-184(Huntsman Advanced Materials公司製)、EPICLON 200、400(DIC(股)製)、jER(註冊商標)871、872(三菱化學(股)製)、ED-5661、ED-5662(Celanese Coatings(股)製);脂肪族聚環氧丙基醚之Denacol EX-611、EX-612、EX-614、EX-622、EX-411、EX-512、EX-522、EX-421、EX-313、EX-314、EX-321(Nagase chemteX(股)製)等。
多官能(甲基)丙烯酸化合物,係只要1分子中具有2個以上(甲基)丙烯基者則無特別限定。該具體例係可列舉:乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、乙氧化雙酚A二(甲基)丙烯酸酯、乙氧化三羥甲基丙烷三(甲基)丙烯酸酯、乙氧化丙三醇三(甲基)丙烯酸酯、乙氧化季戊四醇四(甲基)丙烯酸酯、乙氧化二季戊四醇六(甲基)丙烯酸酯、乙氧化異三聚氰酸三(甲基)丙烯酸酯、參(2-(甲基)丙烯醯基氧乙基)異氰脲酸酯、ε-己內酯改
質參-(2-(甲基)丙烯醯氧乙基)異氰脲酸酯、聚丙三醇單環氧乙烷聚(甲基)丙烯酸酯、聚丙三醇聚乙二醇聚(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、三環癸烷二甲醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯等。
此外,多官能(甲基)丙烯酸化合物係可作為市售品而取得,該具體例係可列舉:NK ESTER A-200、A-400、A-600、A-1000、A-9300、A-9300-1CL、A-TMPT、A-TMM-3、A-TMM-3L、A-TMP、A-TMMT、A-DPH、UA-53H、1G、2G、3G、4G、9G、14G、23G、ABE-300、A-BPE-4、A-BPE-6、A-BPE-10、A-BPE-20、A-BPE-30、BPE-80N、BPE-100N、BPE-200、BPE-500、BPE-900、BPE-1300N、A-GLY-3E、A-GLY-9E、A-GLY-20E、A-TMPT-3EO、A-TMPT-9EO、ATM-4E、ATM-35E、AT-20E(新中村化學工業(股)製)、KAYARAD(註冊商標)DPEA-12、PEG400DA、THE-330、RP-1040(日本化藥(股)製)、ARONIX(註冊商標)M-210、M-303、M-305、M-306、M-309、M-306、M-310、M-313、M-315、M-321、M-350、M-360、M-400、M-402、M-403、M-404、M-405、M-406、M-408、M-450、M-452、M-460(東亞合成(股)製)、KAYARAD(註冊商標)DPHA、NPGDA、PET30(日本化藥(股)製)、NK ESTER A-DPH、A-TMPT、A-DCP、A-HD-N、TMPT、DCP、NPG、HD-N(新
中村化學工業(股)製)、NK OLIGO U-15HA(新中村化學工業(股)製)、NK polymer VANARESIN GH-1203(新中村化學工業(股)製)、EBECRYL(註冊商標)11、40、135、140、145、150、180、1142、OTA480、IRR214-K、PEG400DA-D(ALLNEX公司製)等。
此外,多官能(甲基)丙烯酸化合物,亦可使用:多官能胺基甲酸酯丙烯酸酯之EBECRYL(註冊商標)204、205、210、215、220、230、244、245、270、284、285、264、265、294/25HD、1259、1290、4820、4858、5120、8210、8254、8301R、8405、8465、8296、8307、8402、8311、8411、8701、8800、8804、8807、9260、9270、9277EA、KRM7735、8200、8452、8528、8667、8904(ALLNEX公司製);UV-1700B、UV-6300B、UV-7510B、UV-7550V、UV-7550B、UV-7600B、UV-7605B、UV-7610B、UV-7620EA、UV-7630B、UV-7640B、UV-7650B、(日本合成化學工業(股)製);多官能聚酯丙烯酸酯之EBECRYL(註冊商標)436、438、446、450、524、525、800、810、811、812、1830、846、851、852、853、1870、884、885(ALLNEX公司製);環氧丙烯酸酯之EBECRYL(註冊商標)600、605、645、648、860、1606、3500、3603、3608、3700、3701、3702、3703、3708、6040(ALLNEX公司製)等。
酸酐化合物,係只要使2分子之羧酸脫水縮合而成的羧酸酐則無特別限定。該具體例係可列舉:鄰苯
二甲酸酐、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐、納迪克酸酐、甲基納迪克酸酐、馬來酸酐、琥珀酸酐、辛基琥珀酸酐、十二烯基琥珀酸酐等於分子內具有1個酸酐基者;1,2,3,4-環丁烷四羧酸二酐、苯均四酸酐、3,4-二羧-1,2,3,4-四氫-1-萘琥珀酸二酐、雙環[3.3.0]辛烷-2,4,6,8-四羧酸二酐、5-(2,5-二氧代四氫-3-呋喃)-3-甲基-3-環己烯-1,2-二羧酸酐、1,2,3,4-丁烷四羧酸二酐、3,3’,4,4’-二苯基酮四羧酸二酐、3,3’,4,4’-聯苯四羧酸二酐、2,2-雙(3,4-二羧苯基)六氟丙烷二酐、1,3-二甲基-1,2,3,4-環丁烷四羧酸二酐等於分子內具有2個之酸酐基者等。
含有封端化異氰酸酯之化合物,係只要於1分子中具有2個以上異氰酸酯基(-NCO)藉由適當的保護基加以封端而成之封端化異氰酸酯基,且若暴露於熱硬化時之高溫,則保護基(封端部分)會熱解離而偏離,所產生的異氰酸酯基在其與樹脂之間引起交聯反應者則無特別限定,可列舉例如:於1分子中具有2個以上(另外,此等之基係可為相同者,亦可為彼此相異者)以下述式所表示之基的化合物。
(式中,Rb係表示封端部之有機基)。
如此之化合物,例如,可使適當的封端劑對於1分子中具有2個以上之異氰酸酯基的化合物產生反應而得到。
1分子中具有2個以上之異氰酸酯基的化合物,係可列舉例如:異佛酮二異氰酸酯、1,6-六亞甲基二異氰酸酯、亞甲基雙(4-環己基異氰酸酯)、三甲基六亞甲基二異氰酸酯等之聚異氰酸酯、此等之二聚物及三聚物、以及此等與二醇類、三醇類、二胺類或三胺類之反應物等。
封端劑係可列舉例如:甲醇、乙醇、異丙醇、n-丁醇、2-乙氧基己醇、2-N,N-二甲基胺基乙醇、2-乙氧基乙醇、環己醇等之醇類;酚、o-硝基酚、p-氯酚、o-、m-或p-甲酚等之酚類;ε-己內醯胺等之內醯胺類;丙酮肟、甲基乙基酮肟、甲基異丁基酮肟、環己酮肟、苯乙酮肟、二苯基酮肟等之肟類;吡唑、3,5-二甲基吡唑、3-甲基吡唑等之吡唑類;十二烷硫醇、苯硫醇等之硫醇類等。
含有封端化異氰酸酯的化合物係可作為市售品而取得,該具體例係可列舉:B-830、B-815N、B-842N、B-870N、B-874N、B-882N、B-7005、B-7030、B-7075、B-5010(三井化學(股)製)、DURANATE(註冊商標)17B-60PX、TPA-B80E、MF-B60X、MF-K60X、E402-B80T(Asahi Kasei Chemicals(股)製)、Karenz MOI-BM(註冊商標)(昭和電工(股)製)等。
胺基塑料化合物,係只要1分子中具有2個以上甲氧基亞甲基者則無特別限定。可列舉例如:CYMEL(註冊商標)303(六甲氧基甲基三聚氰胺)、1170(四丁氧基甲基乙炔脲)、1123(四甲氧基甲基苯代三聚氰二胺)(ALLNEX公司製)等之Cymel系列、甲基化三聚氰胺樹脂之NIKALAC(註冊商標)MW-30HM、MW-390、MW-100LM、MX-750LM、甲基化脲樹脂之MX-270、MX-280、MX-290(SANWA CHEMICAL(股)製)等之NIKALAC系列等的三聚氰胺系化合物。
氧雜環丁烷化合物,係只要於1分子中具有2個以上氧雜環丁烷基者則無特別限定,可列舉例如:含有氧雜環丁烷基之OXT-221、OX-SQ-H、OX-SC(東亞合成(股)製)。
酚醛塑料化合物,係於1分子中具有2個以上羥亞甲基,且曝露於熱硬化時之高溫時,會在其與本發明所使用之超枝化聚合物之間藉由脫水縮合反應而進行交聯反應者。酚醛塑料化合物係可列舉例如:2,6-二羥甲基-4-甲基酚、2,4-二羥甲基-6-甲基酚、雙(2-羥-3-羥甲基-5-甲基苯基)甲烷、雙(4-羥-3-羥甲基-5-甲基苯基)甲烷、2,2-雙(4-羥-3,5-二羥甲基苯基)丙烷、雙(3-甲醯基-4-羥苯基)甲烷、雙(4-羥-2,5-二甲基苯基)甲醯基甲烷、α,α-雙(4-羥-2,5-二甲基苯基)-4-甲醯基甲苯(formyltoluene)等。
酚醛塑料化合物亦可作為市售品而取得,該具體例係可列舉:26DMPC、46DMOC、DM-BIPC-F、
DM-BIOC-F、TM-BIP-A、BISA-F、BI25X-DF、BI25X-TPA(旭有機材工業(股)製)等。
交聯劑A,較佳為藉由交聯形成基間之鏈長為長而使分子量成為1,000以上者,具體而言,較佳為藉由具有聚醚結構、聚酯結構、聚胺基甲酸酯結構等而使交聯形成基間之鏈長增長者。上述之交聯劑當中,交聯劑A係可列舉:NK ESTER A-GLY-20E、ATM-35E、AT-20E、23G、A-BPE-20BPE-900、BPE-1300N(新中村化學工業(股)製)、EBECRYL(註冊商標)204、205、210、215、230、244、245、270、284、285、264、265、294/25HD、1259、1290、4820、8254、8301R、8405、8465、8296、8307、8411、8701、8800、8804、9260、9277EA、KRM8200、8452、8528、8667、8904、436、438、446、450、525、1830、846、1870、884、885、860、3708(ALLNEX公司製)、UV-1700B、UV-6300B、UV-7510B、UV-7550V、UV-7550B、UV-7600B、UV-7605B、UV-7610B、UV-7620EA、UV-7630B、UV-7640B、UV-7650B、(日本合成化學(股)製)等。此等當中,較佳為NK ESTER A-GLY-20E、ATM-35E等。
此外,上述之交聯劑當中,分子量未達1,000之交聯劑B係可列舉:ARONIX(註冊商標)M-303、M-305、M-305、M-306、M-400、M-402、M-403、M-404、M-405、M-406、M-450、M-452(東亞合成(股)製)、NK ESTER A-9300、A-9300-1CL、A-TMM-3、A-TMM-3L、
A-TMPT、A-TMP、A-TMMT、A-DPH、1G、2G、3G、4G、9G、14G、ABE-300、A-BPE-4、A-BPE-6、A-BPE-10、A-BPE-20、A-BPE-30、BPE-80N、BPE-100N、BPE-200、BPE-500(新中村化學工業(股)製)、EBECRYL(註冊商標)11、40、135、140、145、150、180、800、853、860、1142、4858、5129、8210、600、605、645、648、1606、3500、3603、3608、3700、3701、3702、3703、6040OTA480(ALLNEX公司製)等。此等當中,較佳為ARONIX(註冊商標)M-303、M-305、M-305、M-306、M-400、M-402、M-403、M-404、M-405、M-406、M-450、M-452(東亞合成(股)製)、NK ESTER A-9300、A-9300-1CL(新中村化學工業(股)製)等。
就可抑制因交聯劑摻合所致之折射率降低,並且迅速地進行硬化反應的觀點而言,交聯劑A及B方面,係較佳為多官能(甲基)丙烯酸化合物。
交聯劑A及B,係可分別單獨使用,亦可將2種以上組合使用。交聯劑A之使用量,雖較佳為相對於含三嗪環之超枝化聚合物100質量份而言,為0.1~30質量份,但若考慮溶劑耐性,則其下限,較佳為1質量份,更佳為5質量份,進而,若考慮控制折射率,則其上限,較佳為25質量份,更佳為20質量份。交聯劑B之使用量,係較佳為相對於交聯劑A 100質量份而言,為0.5~400質量份,更佳為50~200質量份。未達0.5質量份時,有透明導電膜之保護效果未獲得改善的情況,若超過400質
量份,則有導致折射率明顯降低的情況。
較佳為於本發明之組成物中,添加各種溶劑,使含三嗪環之超枝化聚合物溶解而使用。於此情況中,溶劑係可與在聚合時所使用的溶劑相同者或相異者。該溶劑,係只要不損及與聚合物之相溶性則無特別限定。
可使用的溶劑之具體例係可列舉:甲苯、p-二甲苯、o-二甲苯、m-二甲苯、乙基苯、苯乙烯、乙二醇二甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丙二醇、丙二醇單乙基醚、乙二醇單乙基醚、乙二醇單異丙基醚、乙二醇甲基醚乙酸酯、丙二醇單甲基醚乙酸酯、乙二醇乙基醚乙酸酯、二乙二醇二甲基醚、丙二醇單丁基醚、乙二醇單丁基醚、二乙二醇二乙基醚、二丙二醇單甲基醚、二乙二醇單甲基醚、二丙二醇單乙基醚、二乙二醇單乙基醚、三乙二醇二甲基醚、二乙二醇單乙基醚乙酸酯、二乙二醇、1-辛醇、乙二醇、己二醇、三亞甲基二醇、1-甲氧-2-丁醇、環己醇、二丙酮醇、糠醇、四氫糠醇、丙二醇、苄醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、γ-丁內酯、丙酮、甲基乙基酮、甲基異丙基酮、二乙基酮、甲基異丁基酮、甲基n-丁基酮、環己酮、乙酸乙酯、乙酸異丙酯、乙酸n-丙酯、乙酸異丁酯、乙酸n-丁酯、乳酸乙酯、甲醇、乙醇、異丙醇、tert-丁醇、烯丙醇、n-丙醇、2-甲基-2-丁醇、異丁醇、n-丁醇、2-甲基-1-丁醇、1-戊醇、2-甲
基-1-戊醇、2-乙基己醇、1-甲氧-2-丙醇、四氫呋喃、1,4-二噁烷、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、N-甲基吡咯啶酮、1,3-二甲基-2-咪唑啶酮、二甲基亞碸、N-環己基-2-吡咯酮等。此等係可1種單獨使用,亦可2種以上混合而使用。
此時,組成物中之固體成分濃度,係只要為不對保存安定性造成影響的範圍則無特別限定,只要因應作為目的之膜的厚度適當設定即可。具體而言,就溶解性及保存安定性的觀點而言,固體成分濃度較佳為0.1~50質量%,更佳為0.2~40質量%。
於本發明之組成物中,亦可摻合因應各交聯劑之起始劑。另外,如上述般,於使用多官能環氧化合物及/或多官能(甲基)丙烯酸化合物作為交聯劑的情況中,雖不使用起始劑亦可進行光硬化而賦予硬化膜,但亦可於此情況中使用起始劑。
於使用多官能環氧化合物作為交聯劑的情況中,係可使用光酸產生劑或光鹼產生劑。
光酸產生劑係只要由周知者適當選擇來使用即可,可使用例如:重氮鹽、鋶鹽、錪鹽等之鎓鹽衍生物。該具體例係可列舉:苯基重氮六氟磷酸鹽、4-甲氧苯基重氮六氟銻酸鹽、4-甲基苯基重氮六氟磷酸鹽等之芳基重氮鹽;二苯基錪六氟銻酸鹽、二(4-甲基苯基)錪六氟磷
酸鹽、二(4-tert-丁基苯基)錪六氟磷酸鹽等之二芳基錪鹽;三苯基鋶六氟銻酸鹽、參(4-甲氧苯基)鋶六氟磷酸鹽、二苯基-4-硫代苯氧基苯基鋶六氟銻酸鹽、二苯基-4-硫代苯氧基苯基鋶六氟磷酸鹽、4,4’-雙(二苯基鋶基)苯基硫化物-雙六氟銻酸鹽、4,4’-雙(二苯基鋶基)苯基硫化物-雙六氟磷酸鹽、4,4’-雙[二(β-羥乙氧基)苯基鋶基]苯基硫化物-雙六氟銻酸鹽、4,4’-雙[二(β-羥乙氧基)苯基鋶基]苯基硫化物-雙-六氟磷酸鹽、4-[4’-(苯甲醯基)苯基硫]苯基-二(4-氟苯基)鋶六氟銻酸鹽、4-[4’-(苯甲醯基)苯基硫]苯基-二(4-氟苯基)鋶六氟磷酸鹽等之三芳基鋶鹽等。
此等之鎓鹽係可使用市售品,該具體例係可列舉:SUN-AID SI-60、SI-80、SI-100、SI-60L、SI-80L、SI-100L、SI-L145、SI-L150、SI-L160、SI-L110、SI-L147(三新化學工業(股)製)、UVI-6950、UVI-6970、UVI-6974、UVI-6990、UVI-6992(Union Carbide Corporatione公司製)、CPI-100P、CPI-100A、CPI-200K、CPI-200S(SAN-APRO(股)製)、ADEKA OPTOMER SP-150、SP-151、SP-170、SP-171((股)ADEKA製)、Irgacure(註冊商標)261(BASF公司製)、CI-2481、CI-2624、CI-2639、CI-2064(日本曹達(股)製)、CD-1010、CD-1011、CD-1012(Sartomer公司製)、DS-100、DS-101、DAM-101、DAM-102、DAM-105、DAM-201、DSM-301、NAI-100、NAI-101、NAI-105、NAI-106、SI-100、SI-101、SI-105、SI-106、PI-105、NDI-105、BENZOIN
TOSYLATE、MBZ-101、MBZ-301、PYR-100、PYR-200、DNB-101、NB-101、NB-201、BBI-101、BBI-102、BBI-103、BBI-109(Midori Kagaku(股)製)、PCI-061T、PCI-062T、PCI-020T、PCI-022T(日本化藥(股)製)、IBPF、IBCF(SANWA CHEMICAL(股)製)等。
光鹼產生劑亦只要由周知者適當選擇即可,可使用例如:Co-胺錯合物系、肟羧酸酯系、硫胺甲酸酯系、四級銨鹽系光鹼產生劑等。該具體例係可列舉:2-硝苄基環己基胺甲酸酯、三苯基甲醇、O-胺甲醯基羥基醯胺、O-胺甲醯基肟、[[(2,6-二硝苄基)氧基]羰基]環己基胺、雙[[(2-硝苄基)氧基]羰基]己烷1,6-二胺、4-(甲基硫苄醯基)-1-甲基-1-嗎啉乙烷、(4-嗎啉苄醯基)-1-苄基-1-二甲基胺基丙烷、N-(2-硝基苄氧羰基)吡咯啶、六氨鈷(III)參(三苯甲基硼酸酯)、2-苄基-2-二甲基胺基-1-(4-嗎啉苯基)-庚酮、2,6-二甲基-3,5-二乙醯-4-(2’-硝苯基)-1,4-二氫吡啶、2,6-二甲基-3,5-二乙醯-4-(2’,4’-二硝苯基)-1,4-二氫吡啶等。此外,光鹼產生劑係可使用市售品,該具體例係可列舉:TPS-OH、NBC-101、ANC-101(以上皆為製品名、Midori Kagaku(股)製)等。
於使用光酸產生劑或光鹼產生劑的情況中,較佳為相對於多官能環氧化合物100質量份而言,使用0.1~15質量份之範圍,更佳為1~10質量份之範圍。
另外,可因應需要以相對於多官能環氧化合物100質量份而言為1~100質量份之量摻合環氧樹脂硬
化劑。
另一方面,於使用多官能(甲基)丙烯酸化合物的情況中,係可使用光自由基聚合起始劑。光自由基聚合起始劑,係只要由周知者適當選擇而使用即可,可列舉例如:苯乙酮類、二苯基酮類、米希勒之苄醯基苯甲酸酯、醯胺肟酯、一硫化四甲基秋蘭姆及噻噸酮等。
尤以光開裂型之光自由基聚合起始劑為佳。針對光開裂型之光自由基聚合起始劑,係記載於最新UV硬化技術(第159頁、發行人:高薄一弘、發行所:技術情報協會(股)、1991年發行)。
市售之光自由基聚合起始劑,係可列舉例如:Irgacure(註冊商標)127、184、369、379、651、500、819、907、784、2959、OXE01、OXE02、CGI1700、CGI1750、CGI1850、CG24-61、DAROCUR 1116、1173、Lucirin TPO(BASF公司製)、UVECRYL(註冊商標)P36(Cytec Surface Specialties公司製)、ESACURE(註冊商標)KIP150、KIP65LT、KIP100F、KT37、KT55、KTO46、KIP75/B(LAMBERTI公司製)等。
於使用光自由基聚合起始劑的情況中,較佳為相對於多官能(甲基)丙烯酸酯化合物100質量份而言,使用0.1~15質量份之範圍,更佳為0.1~10質量份之範圍。
本發明之膜形成用組成物,亦可在不損及本發明之效果的範圍內,包含其他成分,例如:整平劑、界面活性劑等。
整平劑或界面活性劑係可列舉例如:聚氧乙烯月桂基醚、聚氧乙烯硬脂基醚、聚氧乙烯鯨蠟醚、聚氧乙烯油基醚等之聚氧乙烯烷基醚類、聚氧乙烯辛基酚醚、聚氧乙烯壬基酚醚等之聚氧乙烯烷基烯丙基醚類、聚氧乙烯.聚氧丙烯嵌段共聚物類、山梨醇酐單月桂酸酯、山梨醇酐單棕櫚酸酯、山梨醇酐單硬脂酸酯、山梨醇酐單油酸酯、山梨醇酐三油酸酯、山梨醇酐三硬脂酸酯等之山梨醇酐脂肪酸酯類、聚氧乙烯山梨醇酐單月桂酸酯、聚氧乙烯山梨醇酐單棕櫚酸酯、聚氧乙烯山梨醇酐單硬脂酸酯、聚氧乙烯山梨醇酐三油酸酯、聚氧乙烯山梨醇酐三硬脂酸酯等之聚氧乙烯山梨醇酐脂肪酸酯類等之非離子系界面活性劑;EFTOP(註冊商標)EF301、EF303、EF352(Mitsubishi Materials Electronic Chemicals(股)製)、MEGAFAC(註冊商標)F171、F173、R-08、R-30、R-40、R-43、F-553、F-554、F-556、F-559、RS-75、RS-72-K(DIC(股)製)、FLUORAD(註冊商標)FC430、FC431(3M公司製)、AashiGuard(註冊商標)AG710(旭硝子(股)製)、SURFLON(註冊商標)S-382、SC101、SC102、SC103、SC104、SC105、SC106(AGC SEIMI CHEMICAL(股)製)等之氟系界面活性劑;有機矽氧烷聚合物KP341(信越化學工業(股)製)、BYK-302、BYK-307、BYK-322、BYK-323、BYK-330、
BYK-333、BYK-370、BYK-375、BYK-378(BYK公司製)等。
此等係可1種單獨或將2種以上組合而使用。界面活性劑之使用量,係較佳為相對於含三嗪環之超枝化聚合物100質量份而言,為0.0001~5質量份,更佳為0.001~1質量份,再更佳為0.01~0.5質量份。
另外,上述其他成分係可在調製本發明之組成物時的任意步驟中進行添加。
本發明之透明導電膜用保護膜,係可藉由將上述之形成透明導電膜用保護膜之組成物塗佈於透明導電膜,因應需要進行加熱使溶劑蒸發之後,進行加熱或光照射而形成。
保護膜之膜密度較佳為1.20~1.45g/cm3,更佳為1.30~1.45g/cm3。膜密度未達1.20g/cm3時,有導致電阻值之變化率增大的情況。
本發明之保護膜的折射率之範圍,係下限值較佳為1.60,更佳為1.65,再更佳為1.70。上限值雖無特別限定,但為1.95~2.00左右。
本發明之保護膜的膜厚係較佳為10~1,000nm,更佳為50~200nm。
此外,形成有本發明之保護膜的透明導電膜之霧度值,係較佳為1.5%以下,更佳為1.0%以下。
組成物之塗佈方法係為任意,可採用例如:旋轉塗佈法、浸漬法、淋塗法、噴墨法、噴塗法、棒塗法、凹版塗佈法、縫隙塗佈法、輥式塗佈法、轉印法、刷毛塗佈、刮刀塗佈法、氣刀塗佈法等之方法。
作為透明導電膜,係較佳為ITO薄膜、IZO薄膜、具有金屬奈米粒子、金屬奈米線、金屬奈米網目等之導電性奈米結構的透明導電膜,更佳為具有導電性奈米結構的透明導電膜。構成導電性奈米結構的金屬雖無特別限定,但可列舉:銀、金、銅、鎳、鉑、鈷、鐵、鋅、釕、銠、鈀、鎘、鋨、銥、此等之合金等。亦即,較佳為具有銀奈米粒子、銀奈米線、銀奈米網目、金奈米粒子、金奈米線、金奈米網目、銅奈米粒子、銅奈米線、銅奈米網目等的透明導電膜,尤以具有銀奈米線的透明導電膜為佳。
燒成溫度,係在使溶劑蒸發的目的下並無特別限定,例如,可以40~400℃進行。燒成方法並無特別限定,例如,只要使用加熱板或烘箱,在大氣、氮等之惰性氣體、真空中等之適當的環境下使溶劑蒸發即可。燒成溫度及燒成時間,係只要選擇適於作為目的之電子裝置的製程步驟之條件即可,且只要選擇所得到的膜之物性值適於電子裝置的要求特性般之燒成條件即可。
進行光照射時之條件亦無特別限定,只要因應所使用之含三嗪環之超枝化聚合物及交聯劑,而採用適當的照射能量及時間。例如,可以50~1,000mJ/cm2來進
行。此外,光照射較佳為在大氣或氮等之惰性氣體的環境下進行。
本發明之保護膜,特別適合作為具有導電性奈米結構的透明導電膜之保護膜。具有導電性奈米結構的透明導電膜,係有由於藉由導電性奈米結構而引起光之漫射因此容易白濁化,而使視認性變差的情況。本發明之保護膜,係由於透明性及折射率高,因此可防止白濁化,而改善視認性,該白濁化係起因於使用了導電性奈米結構之透明導電膜的光之漫射。進而,由於具有高耐熱性或高溫高濕耐性,因此對於透明導電膜之劣化防止亦可有所貢獻。因而,本發明之保護膜係適合作為透明電極用構件。此外,由於可進一步達成高溶解性及低體積收縮,因此適合利用作為製作液晶顯示器、有機電致發光(EL)顯示器、觸控面板、光半導體(LED)元件、固體攝像元件、有機薄膜太陽能電池、色素增感太陽能電池、有機薄膜電晶體(TFT)等之電子裝置時的一部分材料。
以下,雖列舉合成例、調製例、實施例及比較例來更具體地說明本發明,但本發明並不限定於下述之實施例。另外,實施例所使用的各測定裝置係如以下所述。
裝置:Varian NMR System 400NB(400MHz)
JEOL-ECA700(700MHz)
測定溶劑:DMSO-d6
基準物質:四甲基矽烷(TMS)(δ 0.0ppm)
裝置:TOSOH(股)製HLC-8200 GPC
管柱:Shodex KF-8041+KF-8051
管柱溫度:40℃
溶劑:四氫呋喃(THF)
檢測器:UV(254nm)
檢量曲線:標準聚苯乙烯
裝置:J.A.Woollam Japan(股)製多入射角分光橢圓偏光計VASE
裝置:Rigaku(股)製TG-8120
昇溫速度:10℃/分
測定溫度:25-750℃
裝置:ESPEC(股)製Light spec恆溫(恆濕)器LHU-113
裝置:日本電色工業(股)製HAZE METER NDH5000
裝置:OLYMPUS(股)製研究用系統顯微鏡BX51
裝置:NAPSON(股)EC-80
裝置:Bruker AXS公司製多功能薄膜材料評估X射線繞射裝置D8 DISCOVER
在氮環境下,於1,000mL四口燒瓶中添加二甲基乙醯胺(DMAc)456.02g,藉由丙酮-乾冰浴冷卻至-10℃,添加2,4,6-三氯-1,3,5-三嗪[1](84.83g、0.460mol、Evonik Degussae公司製)並進行溶解。其後,滴下溶解於DMAc 304.01g的m-苯二胺[2](62.18g、0.575mol)及苯胺(14.57g、0.156mol)。滴下後攪拌30分鐘,藉由送液泵花費1小時將該反應溶液滴下至預先於2,000mL四口燒瓶中添加DMAc 621.85g並在油浴中加熱至85℃的槽,攪拌1小時進行聚合。
然後,添加苯胺(113.95g、1.224mol),攪拌1小時結束反應。藉由冰浴冷卻至室溫後,滴下三乙基胺(116.36g、1.15mol),攪拌30分鐘將鹽酸淬火。其後,將
析出後的鹽酸鹽予以過濾去除。使經過濾的反應溶液於28質量%氨水(279.29g)與離子交換水8,820g之混合溶液中再沉澱。將沉澱物過濾,以減壓乾燥機以150℃進行乾燥8小時後,使其再溶解於THF 833.1g,於離子交換水6,665g中再沉澱。將所得到的沉澱物過濾,以減壓乾燥機以150℃進行乾燥25小時,而得到作為目的之超枝化聚合物[3](以下,稱為HB-TmDA40)118.0g。
將HB-TmDA40之1H-NMR光譜的測定結果顯示於第1圖。HB-TmDA40之Mw為4,300,分散度為3.44。
針對合成例1所得到的HB-TmDA40,將TG-DTA測定的結果顯示於第2圖。5%重量減少係419℃。
將合成例1所得到的HB-TmDA40 0.5g溶解於環己酮4.5g中,而得到淡黃色透明溶液。使用旋轉塗佈機以200rpm、5秒鐘,以2,000rpm、30秒鐘將所得到的溶液旋轉塗佈於玻璃基板上,以150℃加熱1分鐘,以250℃加熱5分鐘來去除溶劑,而得到膜厚500nm之被膜。測定所得到的被膜之折射率的結果,於550nm之折射率為1.790。
使合成例1所得到的HB-TmDA40 100g溶解於環己酮384.0g、離子交換水16.0g之混合溶劑中,而調製20質量%之溶液(以下,稱為HB-TmDA40V1)。
將銀奈米線分散液50g(ClearOhm、Cambrios Technologies Corporation公司製)以異丙醇50g進行稀釋,而調製出導電性油墨A。
利用旋轉塗佈法以200rpm、5秒鐘,其後以900rpm、30秒鐘使調製例2所調製的導電性油墨A於無鹼玻璃基板上成膜,之後,在加熱板上,以120℃,進行乾燥1分鐘,而製作透明導電膜。
添加調製例1所調製出的HB-TmDA40V1 5.0g、10質量%環己酮溶液之A-9300(分子量423、新中村化學工業(股)製)0.5g、60質量%環己酮溶液之乙氧化季戊四醇四丙烯酸酯(ATM-35E、350mPa.s、分子量1,892、新中村化學工業(股)製)0.167g、5質量%環己酮溶液之光自由基起始劑Irgacure 184(BASF公司製)1.6g、1質量%環己酮溶液之界面活性劑MEGAFAC R-30-N(DIC(股)製)0.05g、離子交換水1.35g、及環己酮32.4g,以目視確認已溶解,而調
製出總固體成分濃度3質量%之清漆(以下,稱為HB-TmDA40VF1)。
添加調製例1所調製出的HB-TmDA40V1 1.0g、10質量%環己酮溶液之M-403[5官能丙烯酸酯(分子量524)與6官能丙烯酸酯(分子量579)之混合物、亞東合成(股)製]0.4g、10質量%環己酮溶液之乙氧化季戊四醇四丙烯酸酯(ATM-35E、350mPa.s、分子量1,892、新中村化學工業(股)製)0.2g、5質量%環己酮溶液之光自由基起始劑Irgacure 184(BASF公司製)0.32g、1質量%環己酮溶液之界面活性劑MEGAFAC R-30-N(DIC(股)製)0.01g、離子交換水0.29g、及環己酮8.47g,以目視確認已溶解,而調製出總固體成分濃度3質量%之清漆(以下,稱為HB-TmDA40VF2)。
添加調製例1所調製出的HB-TmDA40V1 1.0g、60質量%環己酮溶液之乙氧化丙三醇三丙烯酸酯(A-GLY-20E、200mPa.s、分子量1,295、新中村化學工業(股)製)0.033g、60質量%環己酮溶液之乙氧化季戊四醇四丙烯酸酯(ATM-35E、分子量1,892、350mPa.s、新中村化學工業(股)製)0.033g、5質量%環己酮溶液之光自由基起始劑Irgacure 184(BASF公司製)0.32g、1質量%環己酮溶液之
界面活性劑MEGAFAC R-30-N(DIC(股)製)0.01g、離子交換水0.37g、及環己酮8.47g,以目視確認已溶解,而調製出總固體成分濃度3質量%之清漆(以下,稱為HB-TmDA40VF3)。
使用旋轉塗佈機以200rpm、5秒鐘,以1,000rpm、30秒鐘將在實施例1~3所調製出的各清漆旋轉塗佈於鈉鈣二氧化矽玻璃基板上,使用烘箱以130℃進行3分鐘燒成。其後,使用高壓水銀燈,在大氣下(實施例4及6)或氮環境下(實施例5),以累計曝光量400mJ/cm2使其硬化,而得到膜厚100nm之硬化膜。將所得到的膜之折射率的測定結果顯示於表1。
使用旋轉塗佈機以200rpm、5秒鐘,以1,000rpm、30秒鐘將在實施例1~3所調製出的各清漆旋轉塗佈於矽晶圓基板上,使用烘箱以130℃進行3分鐘燒成。其後,
使用高壓水銀燈,在大氣下或氮環境下,以累計曝光量400mJ/cm2使其硬化,而得到膜厚100nm之硬化膜。針對此等之硬化膜進行XRR測定,而算出膜密度。於表2顯示於各實施例中所使用的清漆、曝光環境、膜密度之測定結果。
將在實施例1~3所調製出的各清漆以成為固體成分2%的方式以環己酮進行稀釋,並使用旋轉塗佈機以200rpm、5秒鐘,以1,000rpm、30秒鐘旋轉塗佈於在調製例3所製作出的透明導電膜上,使用烘箱以130℃進行3分鐘燒成。其後,使用高壓水銀燈,在大氣下或氮環境下,以累計曝光量400mJ/cm2使其硬化,形成膜厚50nm之保護膜,測定霧度值(實施例10~14)。另外,作為比較例1而測定在調製例3所製作出的透明導電膜本身之霧度值。於表3顯示於各實施例中所使用的清漆、曝光環境、及在實施例、比較例所測定出的霧度值之測定結果。
此外,針對在實施例10~14、比較例1所使用的試料,於設定為槽內溫度85℃、相對濕度85%之恆溫恆濕試驗器中裝入各試料,測定保持了47、168、360及500小時之後的薄片電阻變化。將該結果顯示於表4。另外,表4中之0h係顯示剛試料製作之後的薄片電阻。
透明導電膜之導電性的降低係對裝置的性能造成較大影響。可知:本發明之保護膜,係有改善透明導電膜之視認性,而抑制透明導電膜之劣化的效果。可知:特別是於實施例12中,電阻值之變化率亦小。
使合成例1所得到的HB-TmDA40 100g溶解於環戊酮384.0g、離子交換水16.0g之混合溶劑中,而調製20質量%之溶液(以下,稱為HB-TmDA40VP1)。
添加調製例4所調製出的HB-TmDA40VP1 0.08g、10質量%環戊酮/離子交換水(96/4)混合溶液之DN0075(3,000~5,000mPa.s日本化藥(股)製)0.78g、10質量%環戊酮/離子交換水(96/4)混合溶液之乙氧化季戊四醇四丙烯酸酯(ATM-35E、分子量1,892、350mPa.s、新中村化學工業(股)製)0.033g、5質量%環己酮溶液之光自由基起始劑Irgacure 127(BASF公司製)0.06g、1質量%環己酮溶液之界面活性劑MEGAFAC R-40(DIC(股)製)0.002g、離子交換水0.16g、及環己酮3.88g,以目視確認已溶解,而調製出總固體成分濃度2質量%之清漆(以下,稱為HB-TmDA40VPF1)。
使用旋轉塗佈機以200rpm、5秒鐘,以1,500rpm、30秒鐘將在實施例15所調製出的HB-TmDA40VPF1旋轉塗佈於鈉鈣玻璃基板上,使用烘箱以120℃進行3分鐘燒成。其後,使用高壓水銀燈,在氮環境下,以累計曝光量400mJ/cm2使其硬化,而得到膜厚57nm之硬化膜。所得
到的膜之折射率為1.5683(波長550nm)。
使用旋轉塗佈機以200rpm、5秒鐘,以1,500rpm、30秒鐘將在實施例15所調製出的HB-TmDA40VPF1旋轉塗佈於在調製例3所製作的透明導電膜上,使用烘箱以120℃進行3分鐘燒成。其後,使用高壓水銀燈,在氮環境下,以累計曝光量400mJ/cm2使其硬化,形成膜厚80nm之保護膜,測定霧度值的結果為0.74%。
將在實施例17所得到的試料裝入設定為槽內溫度85℃、相對濕度85%之恆溫恆濕試驗器中,測定保持了168、500小時之後的薄片電阻變化。將該結果顯示於表5。另外,表5中之0h係顯示剛試料製作之後的薄片電阻。
Claims (14)
- 一種形成透明導電膜用保護膜之組成物,其特徵為,含有:包含以下述式(1)所表示的重複單元結構之含三嗪環之超枝化聚合物及分子量1,000以上之交聯劑A,及分子量未達1,000之交聯劑B,惟,該組成物不含下述式(A)所示化合物之可賦予線性聚合物的有機單體,式中,R及R’係各自獨立表示氫原子、烷基、烷氧基、芳基或芳烷基,Ar係表示由以式(2)~(13)所表示之基所成之群中選出的至少1種之基, 式中,R1~R92係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基,R93及R94係表示氫原子或碳數1~10之烷基,W1及W2係各自獨立表示單鍵、-C(R95)(R96)-、-C(O)-、-O-、-S-、-S(O)-、-S(O)2-或-N(R97)-,R95及R96係各自獨立表示氫原子或碳數1~10之烷基,於R95及R96皆為烷基時,此等係可相互鍵結而與鍵結此等之碳原子一起形成環,R97係表示氫原子或碳數1~10之烷基,X1及X2係各自獨立表示單鍵、碳數1~10之伸烷基或以式(14)所表示之基;式中,R98~R101係各自獨立表示氫原子、鹵素原子、羧基、碸基、碳數1~10之烷基或碳數1~10之烷氧基,Y1及Y2係各自獨立表示單鍵或碳數1~10之伸烷基,式中,R102及R104各自獨立表示氫原子、碳数1~10之烷基,或含有聚合性碳-碳雙鍵之基,R103表示氫原子、碳数1~10之烷基,惟,R102及R104之任一者為含有聚合性碳-碳雙鍵之基,且R102及R104兩者不同時為含有聚合性碳-碳雙鍵之基。
- 如請求項1之組成物,其中,交聯劑A為多官能(甲基)丙烯酸化合物。
- 如請求項1或2之組成物,其中,相對於前述含三嗪環之超枝化聚合物100質量份而言,包含0.1~30質量份之交聯劑A。
- 如請求項1之組成物,其中,交聯劑B為多官能(甲基)丙烯酸化合物。
- 如請求項1之組成物,其中,相對於交聯劑A 100質量份而言,包含0.5~400質量份之交聯劑B。
- 如請求項1或2之組成物,其中,進一步包含溶劑。
- 如請求項1之組成物,其中,進一步包含起始劑。
- 如請求項1之組成物,其中,進一步包含整平劑或界面活性劑。
- 一種透明導電膜用保護膜,其係使如請求項1~8中任一項之組成物硬化而得。
- 如請求項9之保護膜,其中,透明導電膜係具有導電性奈米結構的透明導電膜。
- 如請求項10之保護膜,其中,導電性奈米結構為銀奈米線。
- 一種透明電極,其係具備透明導電膜與形成於該透明導電膜上之如請求項9之保護膜。
- 一種電子裝置,其係具備透明導電膜與形成於該透明導電膜上之如請求項9之保護膜。
- 如請求項13之電子裝置,其係有機電致發光顯示器。
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JP5880452B2 (ja) * | 2011-02-15 | 2016-03-09 | 日産化学工業株式会社 | 光硬化型膜形成用組成物および硬化膜の製造方法 |
JP5721601B2 (ja) | 2011-09-30 | 2015-05-20 | 富士フイルム株式会社 | タッチパネル、及びタッチパネルの製造方法 |
CN102527621B (zh) * | 2011-12-27 | 2014-07-09 | 浙江科创新材料科技有限公司 | 一种雾度可调柔性透明导电薄膜的制备方法 |
CN104272145B (zh) * | 2012-05-11 | 2018-01-23 | 日产化学工业株式会社 | 膜形成用组合物 |
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JPWO2015093510A1 (ja) | 2017-03-23 |
KR20160099637A (ko) | 2016-08-22 |
JP6645188B2 (ja) | 2020-02-14 |
EP3085750A4 (en) | 2017-07-26 |
WO2015093510A1 (ja) | 2015-06-25 |
EP3085750A1 (en) | 2016-10-26 |
US10266701B2 (en) | 2019-04-23 |
CN105980497A (zh) | 2016-09-28 |
US20160319132A1 (en) | 2016-11-03 |
TW201529725A (zh) | 2015-08-01 |
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