TWI811475B - 用於包括彼的光學構件之黏著劑樹脂及黏著劑組成物 - Google Patents
用於包括彼的光學構件之黏著劑樹脂及黏著劑組成物 Download PDFInfo
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- TWI811475B TWI811475B TW108139889A TW108139889A TWI811475B TW I811475 B TWI811475 B TW I811475B TW 108139889 A TW108139889 A TW 108139889A TW 108139889 A TW108139889 A TW 108139889A TW I811475 B TWI811475 B TW I811475B
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Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/6715—Unsaturated monofunctional alcohols or amines
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/71—Monoisocyanates or monoisothiocyanates
- C08G18/718—Monoisocyanates or monoisothiocyanates containing silicon
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D133/062—Copolymers with monomers not covered by C09D133/06
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J133/00—Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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Abstract
本發明係關於用於包括彼的光學構件之黏著劑樹脂及黏著劑組成物,該黏著劑樹脂包括將單體混合物聚合所形成的丙烯酸共聚物,該單體混合物包括[式1]表示的單體、具有可交聯官能基的(甲基)丙烯酸單體、與(甲基)丙烯酸烷酯系單體。
Description
本申請案主張韓國專利申請案號10-2018-0156716之權益,此案在2018年12月7日於韓國智慧財產權局提出申請,以引用方式將其全部揭露併入本案作為參考。
本發明係關於用於包括彼之光學構件的黏著劑樹脂及黏著劑。更具體地說,本發明係關於用於包括彼之光學構件的即使當暴露於高溫時也沒有顯著性質變化和即使當長時間使用時也保持高耐久性的黏著劑樹脂及黏著劑組成物。
通常,液晶顯示裝置(LCD)設有包括液晶之液晶晶元、與偏光片,及使用黏著層以附接液晶晶元與偏光片。將丙烯酸樹脂、橡膠、胺甲酸酯系樹脂、聚矽氧系
樹脂、乙烯-乙酸乙烯酯(EVA)等用於形成黏著層的黏著劑。其中,廣泛使用具有透明度、抗氧化性、與抗黃化性之以丙烯酸樹脂為基礎的黏著劑。
同時,近年來,將包括偏光片之顯示裝置用於各種產品,比如可攜式產品、車載產品、室外電能表、電腦、電視等,並且其應用範圍日益擴大。正如其應用範圍變化多端,使用顯示裝置的環境日趨嚴苛。因此,顯示裝置即使在具有高溫度、高濕度與/或溫度或濕度極端變化之環境中也須具有高耐久性。因此,即使當長時間暴露於高溫度或高濕度環境時也須保持極佳黏著性。然而,到目前為止所開發之黏著劑不夠符合上述要求。因此,需要開發在嚴苛環境中能夠實現高耐久性的黏著劑組成物。
本發明係解決上述問題,提供用於包括彼的光學構件之黏著劑樹脂及黏著劑組成物,該黏著劑樹脂即使當暴露於高溫度時也沒有顯著性質變化和即使當長時間使用時也保持高耐久性。
根據本發明之一個態樣,提供一種黏著劑樹脂,其包括將單體混合物聚合所形成的丙烯酸共聚物,該單體混合物包括下[式1]表示之單體、具有可交聯官能基
的(甲基)丙烯酸單體、與(甲基)丙烯酸烷酯系單體。
其中,F1是-OH、-COOH、或-SH,X1是單鍵、-O-、-NH-、具有1至10個碳原子之伸烷基、或其組合,X2是單鍵、具有1至10個碳原子的伸烷基、-COO-、或其組合,R1是氫或具有1至4個碳原子之烷基,R2是單鍵或具有1至10個碳原子的伸烷基,及R3是具有6至20個碳原子之伸芳基或具有1至10個碳原子的伸烷基。
根據本發明之另一個態樣,提供一種用於光學構件的黏著劑組成物,該組成物包括根據本發明之黏著劑樹脂與多官能固化劑。
根據本發明之又一個態樣,提供一種偏光片與包括彼的顯示裝置,該偏光片包括黏著劑層,其具有用於光學構件之黏著劑組成物的固化產物。
在本發明中,當由包括作為原料的[式1]表示之單體製成共聚物時,形成具有多重交聯點與支鏈聚合物結構的共聚物。因此,本發明之黏著劑樹脂比包括具有相同重量平均分子量的線型共聚物之黏著劑樹脂具有其高
交聯度與更低的黏度。因此,即使當長時間暴露於高溫度與/或高濕度環境時,本發明之黏著劑樹脂也沒有顯著性質變化,藉此實現高耐久性。
在下文,將更詳細描述本發明。
在本說明書中,當使用比如「包括」、「具有」、與「是由~構成」之術語時,可能加入其他部件,除非使用了「~只」。單數形式的元件可能包括複數形式的元件,除非上下文清楚地指出為其他情况。
在解釋性元件中,應當解釋為包括誤差範圍,即使沒有單獨明確的陳述。
在本說明書中,「(甲基)丙烯酸的」是用於丙烯酸的與甲基丙烯酸的之通用術語。例如,術語「(甲基)丙烯酸酯」包括甲基丙烯酸酯與丙烯酸酯,及術語「(甲基)丙烯酸」包括丙烯酸與甲基丙烯酸。
在本說明書中,表示範圍之術語「X至Y」乃指「X或更大且Y或更小」。
在本說明書中,術語「支鏈聚合物結構」乃指具有以不同方向成長之二或多個長鏈的聚合物結構。
本發明人已反覆地進行研究以開發即使當長時間暴露於高溫度與/或高濕度環境時也能夠保持極佳耐久性之黏著劑組成物,及已發現當一起使用特定單體時,當產生丙烯酸共聚物時,可能形成具有多重交聯點與支鏈
聚合物結構的共聚物。本發明人還發現當使用該共聚物時可達到上述目的,及完成本發明。
在下文,將詳細描述根據本發明之丙烯酸黏著劑組成物。
黏著劑樹脂
根據本發明之黏著劑樹脂包括將單體混合物聚合所形成的丙烯酸共聚物,該單體混合物包括下[式1]表示之單體、具有可交聯官能基的(甲基)丙烯酸單體、與(甲基)丙烯酸烷酯系單體。
在上式1中,F1是-OH、-COOH、或-SH,X1是單鍵、-O-、-NH-、具有1至10個碳原子之伸烷基、或其組合,X2是單鍵、具有1至10個碳原子的伸烷基、-COO-、或其組合,R1是氫或具有1至4個碳原子之烷基,R2是單鍵或具有1至10個碳原子的伸烷基,及R3是具有6至20個碳原子之伸芳基或具有1至10個碳原子的伸烷基。
上[式1]表示之單體是包括可交聯官能基F1與在兩端的可聚合雙鍵之化合物。當將[式1]表示之單體作為原料時,下述具有可交聯官能基之(甲基)丙烯酸單體的可交聯官能基與上[式1]之F1官能基起交聯點作用,使
得可產生具有多重交聯點的丙烯酸共聚物。因此,使黏著劑組成物之交聯度增加以實現高耐久性。
具體地說,上[式1]表示之單體具有二或多個乙烯基,其中在自由基聚合反應中可個別地形成基團,藉此讓鏈以不同方向成長。因此,形成具有不同成長方向之二或多個鏈的支鏈聚合物。具有支鏈聚合物結構之丙烯酸共聚物具有比具有相同重量平均分子量的線型聚合物結構之丙烯酸共聚物更低的黏度,使得即使塗料液中固含量增加,也可實現極佳塗布性。
上[式1]表示之單體的具體實例包括選自由下列式1-1至1-4表示之化合物所組成的群組之一或多者,但不限於此。
同時,可能包括以100重量份之單體混合物為基準計,0.01至1重量份,較佳為0.05至1重量份,更佳為0.1至0.5重量份之量的上[式1]表示之單體。當[式1]表示之單體的含量少於0.01重量份時,改善耐久性之效果微不足道。當大於1重量份時,在聚合反應期間交聯反應進行,使得很難控制分子量與黏度增加。
接下來,具有可交聯官能基之(甲基)丙烯酸單體係用於改善黏著劑的耐久性、黏著性、與內聚性。其之例子可包括:含有羥基之單體、含有羧基之單體、或含有氮之單體,但不限於此。含有羥基之單體的具體實例可包括:(甲基)丙烯酸2-羥乙酯、(甲基)丙烯酸2-羥丙酯、(甲基)丙烯酸4-羥丁酯、(甲基)丙烯酸6-羥己酯、(甲基)丙烯酸8-羥辛酯、(甲基)丙烯酸2-羥基乙二醇酯、(甲基)丙烯酸2-羥基丙二醇酯等。含有羧基之單體的例子可包括:(甲基)丙烯酸、2-(甲基)丙烯醯氧基乙酸、3-(甲基)丙烯醯氧基丙酸、4-(甲基)丙烯醯氧基丁酸、丙烯酸二聚體、伊康酸、順丁烯二酸、順丁烯二酐等。含有氮之單體的例子可包括:(甲基)丙烯醯胺、N-乙烯基吡咯啶酮、或N-乙烯基己內醯胺等。然而,本發明之實施方式不限於此。
可能包括以100重量份之單體混合物為基準
計,0.1至15重量份,較佳為1至10重量份,更佳為1至5重量份之量的包括可交聯官能基之(甲基)丙烯酸單體。當包括可交聯官能基之(甲基)丙烯酸單體的含量符合上述範圍時,可獲得更佳黏著性與耐久性。
接下來,較佳為(甲基)丙烯酸烷酯系單體包括具有1至14個碳原子之烷基。當(甲基)丙烯酸烷酯系單體所包括的烷基太長時,黏著劑之內聚性惡化,並且可能很難控制玻璃轉化溫度(Tg)或黏著性。(甲基)丙烯酸烷酯系單體的例子可包括:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸異丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸三級丁酯、(甲基)丙烯酸二級丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸2-乙基丁酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸異辛酯、(甲基)丙烯酸異壬酯、(甲基)丙烯酸十二酯、與(甲基)丙烯酸十四酯。在本發明中,可能使用其之任一者或其之二或多者的混合物。
可能包括以100重量份之單體混合物為基準計,84至99.88重量份,較佳為89至98.95重量份,更佳為94.5至98.9重量份之量的(甲基)丙烯酸烷酯系單體。當(甲基)丙烯酸烷酯系單體之含量符合上述範圍時,可獲得極佳黏著性與耐久性。
根據一個實施方式,可將單體混合物聚合形成丙烯酸共聚物,該單體混合物包括以100重量份之單體混合物為基準計,84至99.89重量份的(甲基)丙烯酸烷酯系
單體、0.01至15重量份之包括可交聯官能基的(甲基)丙烯酸單體、與0.01至1重量份之[式1]表示的單體。
將上述單體各者混合以製備單體混合物,然後將該混合物聚合可製得根據本發明之丙烯酸共聚物。此時,聚合方法未特別限定。可使用本領域中已知的各種聚合方法,比如溶液聚合法、光聚合法、塊體聚合法、懸浮聚合法、與乳化聚合法。在聚合作用期間,還可能加入聚合反應引發劑、分子量控制劑等。各組分的注入時間未特別限定。亦即,可將組分一起加入,或者可在不同時間分批加入。
在本發明中,特別地藉由溶液聚合法可製得丙烯酸共聚物。較佳為在50℃至140℃的聚合溫度下在各單體被均勻地混合狀態下加入引發劑、分子量控制劑等來進行溶液聚合。可用於製程之引發劑的例子可包括慣用引發劑,例如偶氮系引發劑(比如偶氮雙異丁腈與偶氮二環己腈等)、及/或過氧化物(比如過氧化苯甲醯與過氧化乙醯)。可能使用其之任一者或其之二或多者的混合物,但引發劑不限於此。此外,作為分子量控制劑,可能使用硫醇類(比如三級十二基硫醇與正十二基硫醇)、萜類(比如雙戊烯與三級萜)、氯仿、四氯化碳的鹵化烴、或季戊四醇肆(3-巰基丙酸)酯等。然而,分子量控制劑不限於此。
如上述製得之本發明之丙烯酸共聚物可具有重量平均分子量為500,000至1,500,000g/mol,較佳為800,000至1,500,000g/mol。當丙烯酸共聚物的重量平均分
子量少於500,000g/mol時,由於固化效率惡化所引起之添加劑的內聚力不足,導致再剝離性惡化及在高溫度或高溫度/高濕度環境下之耐久性減少。當大於1,500,000g/mol時,由於高黏度導致塗布性惡化,使得可能很難產生均勻的黏著層。
此外,本發明之丙烯酸共聚物具有支鏈結構。和具有線型聚合物結構的丙烯酸共聚物比較,具有支鏈聚合物結構之丙烯酸共聚物具有低黏性。因此,即使當固含量高時,包括具有支鏈聚合物結構的丙烯酸共聚物的黏著劑樹脂也可能實現極佳塗布性。
黏著劑組成物
接下來,將描述根據本發明之黏著劑組成物。
根據本發明之黏著劑組成物包括上述根據本發明之黏著劑樹脂與多官能固化劑。由於上文已描述黏著劑樹脂,將在下文描述多官能固化劑。
多官能固化劑係用於改善與黏著物的界面黏著性,並且其類型未特別限定。可能使用本領域中使用之各種固化劑,例如,選自由下列所組成的群組之一或多者:異氰酸酯系化合物、環氧系化合物、吖系化合物、與金屬螯合物系化合物。
作為異氰酸酯系化合物,可能使用本領域中已知的任何典型異氰酸酯系化合物。例如,可能使用二異氰酸甲苯酯、2,4-三氯乙烯二異氰酸酯、2,6-三氯乙烯二
異氰酸酯、氫化的三氯乙烯二異氰酸酯、異構重組二異氰酸酯、1,3-二異氰酸二甲苯酯、1,4-二異氰酸二甲苯酯、二苯甲烷-4,4-二異氰酸酯、1,3-雙異氰酸甲基環己烷、四甲基伸苯二甲基二異氰酸酯、1,5-二異氰酸萘酯、六亞甲基二異氰酸酯、2,2,4-三甲基六亞甲基二異氰酸酯、2,4,4-三甲基六亞甲基二異氰酸酯、三羥甲基丙烷改質二異氰酸甲苯酯、三羥甲基丙烷改質二異氰酸甲苯酯、三羥甲基丙烷之三氯乙烯二異氰酸酯加成物、三羥甲基丙烷的二異氰酸二甲苯酯加成物、三苯甲烷三異氰酸酯、亞甲基雙三異氰酸酯、其多元醇(三羥甲基丙烷),或其混合物等。
作為環氧系化合物,可能使用例如乙二醇二環氧丙醚、三環氧丙醚、三羥甲基丙烷三環氧丙醚、N,N,N’,N’-四環氧丙基乙二胺、甘油二環氧丙醚、或其混合物。
作為吖系化合物,可能使用例如N,N’-甲苯-2,4-雙(1-吖羧醯胺)、N,N’-二苯甲烷-4,4’-雙(1-吖羧醯胺)、三伸乙基三聚氰胺、雙間苯二醯基-1-(2-甲基吖)、三-1-吖基膦氧化物、或其混合物。
金屬螯合物系化合物可為,例如,其中多價金屬比如鋁、鐵、鋅、錫、鈦、銻、鎂與/或釩和乙醯丙酮或乙醯乙酸乙酯等配位的化合物,但不限於此。
可能包括以100重量份之黏著劑樹脂為基準計,0.01至1重量份,較佳為0.01至0.5重量份之量的多官能固化劑。當多官能固化劑之含量少於0.01重量份時,改
善與黏著物的黏著性效果微不足道,及當大於1重量份時,黏著劑的物理性質可能隨時間而變化。
同時,為了控制物理性質,除了上述組分外,本發明之黏著劑組成物還可能另外包括其他組分,比如溶劑、矽烷偶合劑、交聯觸媒、黏著性賦予樹脂、與添加劑。
本發明之黏著劑組成物可能另外包括用於控制黏度的溶劑。此時,溶劑可為例如乙酸乙酯、正戊烷、異戊烷、新戊烷、正己烷、正辛烷、正庚烷、甲基乙基酮、丙酮、甲苯、或其組合,但不限於此。可能包括一量的溶劑,使得黏著劑組成物中固含量是30重量%或更大,較佳為30至60重量%。
此外,本發明之黏著劑組成物可能另外包括矽烷偶合劑。
矽烷偶合劑改善黏著劑與玻璃基板之間的黏著性與黏著穩定性,藉此改善耐熱性與抗濕性。此外,當將黏著劑長時間留在高溫度與/或高濕度條件下時,矽烷偶合劑改善黏著可靠性。可用於本發明的矽烷偶合劑的例子包括γ-環氧丙氧基丙基三乙氧基矽烷、γ-環氧丙氧基丙基三甲氧基矽烷、γ-環氧丙氧基丙基甲基二乙氧基矽烷、γ-環氧丙氧基丙基三乙氧基矽烷、3-巰丙基三甲氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷、γ-甲基丙烯醯氧基丙基三乙氧基矽烷、γ-胺基丙基三甲氧基矽烷、γ-胺基丙基三乙
氧基矽烷、3-異氰酸基丙基三乙氧基矽烷、γ-乙醯乙酸酯丙基三甲氧基矽烷、γ-乙醯乙酸酯丙基三乙氧基矽烷、β-氰乙醯基三甲氧基矽烷、β-氰乙醯基三乙氧基矽烷、與乙醯氧基乙酸根合三甲氧基矽烷,及可能使用其之任一者或其之二或多者的混合物。在本發明中,較佳為使用具有乙醯乙酸基或β-氰乙醯基之矽烷偶合劑,但本發明的實施方式不限於此。
例如,矽烷偶合劑可為下式2表示之化合物。
[式2](Ra)nSi(Rb)4-n
在上式2中,Ra是β-氰乙醯基、乙醯乙醯基或乙醯乙醯基烷基,Rb是烷氧基,及n是1至3的整數。此時,上式2所包括之烷基或烷氧基可具有1至20、1至16、1至12、1至8、或1至4個碳原子,及可為線型或支鏈的。
上式2表示之化合物的具體實例可能包括乙醯乙醯基丙基三甲氧基矽烷、乙醯乙醯基丙基三乙氧基矽烷、β-氰乙醯基三甲氧基矽烷、β-氰乙醯基三乙氧基矽烷等,但不限於此。
在本發明之組成物中,可能包括以100重量份之黏著劑樹脂為基準計,0.01重量份至5重量份,較佳為0.01重量份至1重量份之量的矽烷系偶合劑。
當偶合劑含量少於0.01重量份時,增加黏著性之效果微不足道。當大於5重量份時,耐久性可能惡化。
本發明之黏著劑組成物可能另外包括交聯觸媒。交聯觸媒係用於促進黏著層固化(交聯)。當黏著劑組成物包括交聯觸媒時,有在使基板表面經受塗布與乾燥後不必進行單獨老化程序的優點。作為交聯觸媒,可能使用例如雙(三正丁錫)氧化物、雙(三正丁錫)硫酸鹽、二正丁基二苯錫、二正丁錫雙(乙醯丙酮酸)鹽、二正丁錫雙(2-乙基己酸)鹽、二正丁錫二氯化物、二正丁錫二月桂酸鹽、二正丁錫氧化物、二甲基二苯錫、二甲錫二氯化物、二苯錫二氯化物、二苯錫氧化物、六正丁錫、六苯錫、四正丁錫、四苯錫、乙酸錫(II)、乙醯丙酮錫(II)、氯化錫(II)、碘化錫(II)、草酸錫(II)等,但本發明之實施方式不限於此。
同時,可能包括以100重量份之黏著劑樹脂為基準計,0.001重量份至0.5重量份,較佳為0.001重量份至0.1重量份之量的交聯觸媒。當交聯觸媒含量少於0.001重量份時,促進固化之效果微不足道。當大於0.5重量份時,耐久性可能惡化。
關於控制黏著性能,本發明之黏著劑組成物可能另外包括以100重量份之黏著劑樹脂為基準計,1重量份至100重量份的黏著性賦予樹脂。黏著性賦予樹脂之類型未特別限定。例如,可能使用下列中任一者或二或多者的混合物:(氫化)烴系樹脂、(氫化)松香樹脂、(氫化)松香酯樹脂、(氫化)萜烯樹脂、(氫化)萜烯酚樹脂、聚合松香樹脂、或聚合松香酯樹脂等。當黏著性賦予樹脂含量少
於1重量份時,加入該黏著性賦予樹脂的效果可能微不足道。當大於100重量份時,改善相容性與/或內聚性之效果可能惡化。
本發明之黏著劑組成物可能另外包括一或多種選自由下列所組成的群組之添加劑:環氧樹脂、固化劑、紫外線安定劑、抗氧化劑、著色劑、強化劑、填料、消泡劑、界面活性劑、與塑化劑,只要不影響本發明之效果。
和使用線型聚合物結構之丙烯酸共聚物且具有相同水平的重量平均分子量之典型黏著劑組成物比較,包括上述組分的根據本發明之黏著劑組成物具有低黏性。因此,即使當黏著劑組成物中固含量高時也可實現極佳塗布性。當根據本發明之黏著劑組成物的固含量是20至30重量%時,其在23℃的黏度是3,000cP或更低,較佳為1,000cP至3,000cP。此時,固含量可能是指將所製得之塗料溶液等形式的本發明之黏著劑組成物施加在黏著劑的製造過程中時之固含量。如上所述,當使用本發明之黏著劑組成物時,可增加塗料溶液中固含量而不使塗布性惡化,使得不僅生產力極佳,而且還可達到比如厚度的精確控制。
上述本發明之黏著劑組成物可有用地作為用於施用於顯示器等的光學構件的黏著劑。具體地說,黏著劑組成物可用於附接偏光片與液晶面板,亦即,可作為用於偏光片的黏著劑。
偏光片
接下來,將描述根據本發明之偏光片。
根據本發明之偏光片包括偏光膜及形成於該偏光片的一個表面或二個表面上並含有根據上述發明性概念之黏著劑組成物的固化產物之黏著層。
本發明所用之偏光膜類型未特別限定。可能使用本領域中已知的典型類型。例如,偏光膜可能包括偏光片與形成於該偏光片之一個表面或二個表面上的保護膜。
本發明之偏光片所包括的偏光片類型未特別限定。例如,會使用但不限於本領域中已知的典型類型,比如聚乙烯醇系偏光片。
偏光片是一種能夠從以各種方向振動時入射之光中只擷取以一個方向振動的光之功能膜。上述偏光片可為例如其中二向色性顏料被吸附到聚乙烯醇系樹脂膜上的形式。例如,將聚乙酸乙烯酯系樹脂形成膠凝可獲得構成偏光片之聚乙烯醇系樹脂。在這種情況下,所用的聚乙酸乙烯酯系樹脂可能包括乙酸乙烯酯之均聚物及乙酸乙烯酯和可與彼共聚合的另一種單體之共聚物。可與乙酸乙烯酯共聚合的單體之例子包括不飽和羧酸、烯烴、乙烯醚、不飽和磺酸、與具有銨基的丙烯醯胺中一者或二者或多者之混合物,但不限於此。聚乙烯醇系樹脂的膠凝程度典型為85莫耳%至100莫耳%,較佳為98莫耳%或更大。聚乙烯醇系樹脂可被另外改質。例如,也可能使用經醛基改質之聚乙烯甲醛或聚乙烯縮醛。另外,聚乙烯醇系樹脂的聚合
度典型上可為1,000至10,000,較佳為1,500至5,000。
可將上述聚乙烯醇系樹脂去膜以作為偏光片的碟片膜。用於將聚乙烯醇系樹脂去膜之方法未特別限定。可能使用本領域中已知的典型方法。
經聚乙烯醇系樹脂去膜的碟片膜之厚度未特別限定,並且可被適當地控制在例如1μm至150μm範圍內。考慮到易於拉長等,可將碟片膜厚度控制為10μm或更大。
可利用下列方式製造偏光片:將上述聚乙烯醇系樹脂膜拉長(例如同軸向拉長),然後用二向色性染料將經拉長之聚乙烯醇系樹脂膜著色並讓該二向色性染料被吸附,接著用硼酸水溶液處理吸附了二向色性染料的聚乙烯醇系樹脂膜,及在用硼酸水溶液處理後進行清洗。在上述中,可將碘或二向色性有機染料等作為二向色性顏料。
本發明之偏光膜也可能包括形成於偏光片之一個表面或二個表面上的保護膜。本發明之偏光片可能包括的保護膜類型未特別限定。例如,保護膜可能由下列形成:以纖維素為基礎之膜(比如三乙醯基纖維素膜)、以聚酯為基礎的膜(比如聚碳酸酯膜或聚對苯二甲酸乙二酯膜)、以聚醚碸為基礎之膜、與/或聚乙烯膜、聚丙烯膜、或具有以環為基礎或以降莰烯為基礎之結構的聚烯烴膜、或多層膜(其中將由以聚烯烴為基礎之膜比如乙烯丙烯共聚物膜構成的保護膜層合)。此時,保護膜厚度未特別限定。可形成典型厚度之保護膜。
同時,在本發明中,用於在偏光膜上形成黏著層之方法未特別限定。例如,藉由典型手段比如塗布棒在膜或裝置上施加黏著劑組成物(塗料液)並固化的方法,或者在可剝式基材表面上施加黏著劑組成物並固化,然後將所形成之黏著層轉移到偏光膜或裝置表面的方法。
在本發明中,較佳為在充分地移除揮發性組分或氣泡誘發組分(比如黏著劑組成物(塗料液)中的反應殘留物)後進行形成黏著層之方法。因此,可以防止由於黏著劑的交聯密度或分子量太低而使彈性模數降低,或由於存在於玻璃板與黏著層之間的氣泡變更大而在其中形成散射體之問題。
同時,在製造偏光片期間用於將本發明之黏著劑組成物固化的方法未特別限定。可進行本領域中已知的典型固化方法。例如,透過加熱等方式來保持可在所施加之黏著劑組成物中的可交聯官能基與多官能交聯劑之間觸發交聯反應的溫度可進行固化。
本發明之偏光片可能另外包括一或多種選自由下列所組成的群組之功能層:保護層、反射層、防眩光層、相位差片、寬視角補償膜、與亮度增強膜。
顯示裝置
接下來,將描述根據本發明之顯示裝置。
本發明之顯示裝置包括上述根據本發明之偏光片。
更具體地說,顯示裝置可為包括液晶面板之
液晶顯示裝置,其具有結合至其之一個表面或二個表面的根據本發明之偏光片。此時,液晶面板類型未特別限定。在本發明中,可能施用任何已知液晶面板而不限於其類型。例如,可能施用各種被動矩陣方法的液晶面板,其包括扭曲向列(TN)型、超扭曲中性(STN)型、鐵電(F)型、與聚合物分散(PD)LCD型,各種主動矩陣系統的液晶面板,其包括二端子型與三端子型、IPS模式面板、或VA模式面板。此外,本發明之液晶顯示裝置所包括的其他結構之類型與製造方法未特別限定。可利用與使用但不限於本領域中常見結構。
進行發明之模式
在下文,將根據具體實施例更詳細描述本發明。
實施例1
將包括98重量份的丙烯酸丁酯(BA)、1.6重量份之丙烯酸羥基丁酯(HBA)、與0.4重量份的式1至3表示之單體的單體混合物加到其中氮氣回流並安裝冷卻裝置以協助溫度控制之3L反應器中。之後,加入60重量份的乙酸乙酯(EAc)作為溶劑。之後,將氮氣吹驅60分鐘以移除氧氣,然後把溫度保持在70℃。之後,加入0.02重量份的偶氮雙(2,4-二甲基戊腈)(V-65,製造商:Wako)作為聚合反應引發劑,然後反應以製備丙烯酸共聚物A。
將100重量份的如上述製得之丙烯酸共聚物A與0.2重量份的多官能固化劑(coronate L,製造商:Nippon Polyurethane Co.,Ltd.)、0.01重量份之交聯觸媒(二月桂酸二正丁錫,Sigma Aldrich)、0.2重量份的矽烷偶合劑(含有β-氰基乙醯基之矽烷偶合劑,LG Chem,M812)摻混,然後用乙酸乙酯稀釋混合物,使得混合物的固體含量變成25重量%。之後,將經稀釋之混合物均勻混合以製備黏著劑組成物(塗料溶液)。
將所製得之黏著劑組成物施加在具有厚度為38μm的經釋離處理之聚對苯二甲酸乙二酯(離型PET)膜的經釋離處理之表面上,使得乾燥後其厚度變成23μm,然後乾燥以形成黏著劑塗層。之後,將黏著劑塗層在偏光片上層合以製造包括黏著劑層的偏光片。
實施例2至5與比較例1至4
以與實施例1相同之方式製備丙烯酸共聚物B至K,不同之處在於將用於製備丙烯酸共聚物的單體之類型與含量按表1與表2中所描述地改變,及如需要加入正十二基硫醇(n-DDM,Sigma Aldrich)作為分子量控制劑。
之後,將100重量份的如上述製備之丙烯酸共聚物B至K各者與多官能固化劑(coronate L,製造商:Nippon Polyurethane Co.,Ltd.)、交聯觸媒(二月桂酸二正丁錫,Sigma Aldrich)、矽烷偶合劑(含有β-氰乙醯基之矽烷偶合劑,LG Chem,M812)按表1與表2中所描述的量摻混,然後用乙酸乙酯稀釋混合物,使得混合物之固體含量
變成如表1與表2中所描述者。之後,將經稀釋之混合物均勻混合以製備黏著劑組成物(塗料溶液)。
將所製備之黏著劑組成物施加在具有厚度為38μm的經釋離處理之聚對苯二甲酸乙二酯(離型PET)膜的經釋離處理之表面上,使得乾燥後其厚度變成23μm,然後乾燥以形成黏著劑塗層。之後,將黏著劑塗層在偏光片上層合以製造包括黏著劑層的偏光片。
測量實施例1至9與比較例1至4各者所製備之丙烯酸共聚物、黏著劑組成物、與偏光片的物理性質,並且將測量結果顯示在下表1與表2中。
用於測量物理性質之方法
1.重量平均分子量:
在下列條件下使用GPC測量實施例與比較例各者所製備之丙烯酸共聚物的重量平均分子量。將Agilent系統的標準聚苯乙烯用於製造校準曲線。
<測量條件>
測量裝置:Agilent GPC(Agulent 1200 series,USA)
管柱:Two PL Mixed B connections
管柱溫度:40℃
洗提液:四氫呋喃
流率:1.0m/分鐘
濃度:~1mg/mL(100μL注入)。
2.聚合物結構
以下列方式評估實施例與比較例各者所製備之丙烯酸共聚物的聚合物結構。
首先,將相同(甲基)丙烯酸烷酯系單體與如丙烯酸共聚物(在下文「評估目標共聚物」),中使用的包括可交聯官能基之(甲基)丙烯酸單體混合製備單體混合物其聚合物結構被評估。此時,將單體混合物中的包括可交聯官能基之(甲基)丙烯酸單體的含量設為與評估目標共聚物中的包括可交聯官能基之(甲基)丙烯酸單體的含量相同。之後,將單體混合物聚合以製備具有相當於評估目標共聚物之重量平均分子量水平的重量平均分子量水平(誤差範圍±5%)之丙烯酸共聚物(在下文「標準共聚物」)。
之後,將乙酸乙酯溶劑加到標準共聚物與評估目標共聚物各者中以調整黏度水平,使得固體濃度為20至30重量%,及測量黏度。當如上述測得之評估目標共聚物黏度比標準共聚物黏度顯著低(例如30%或更大)時,該評估目標共聚物被評估為具有支鏈聚合物結構,而在其他情況下,該評估目標共聚物被評估為具有線型聚合物結構。
3.塗料固體含量(單位:%)
利用下列方法測量塗料固體。
首先,測量鋁皿重量(A)。然後,收集約0.3至0.5g(乾燥前樣品重量:S)之實施例或比較例各者所製成之黏著劑組成物並放置於已稱重的鋁皿中。此時,測量包括鋁皿重量之乾燥前樣品重量B(A+S)。然後,使用吸
量管將小量其中溶有聚合抑制劑(對苯二酚)的乙酸乙酯溶液(0.5重量%聚合抑制劑濃度)加到黏著劑組成物,然後在烘箱中在150℃乾燥約30分鐘以移除溶劑。之後,在室溫將經乾燥之樣品冷卻15分鐘至30分鐘,然後測量包括鋁皿重量A之包括乾燥後樣品重量C的重量。根據下列方程式(1)計算出塗料固體含量:
方程式(1);塗料固體含量(%)={(C-A)/(B/A)} X 100
在方程式(1)中,A是鋁皿重量(單位:g),而C是包括鋁皿重量A之乾燥後樣品重量(單位:g)。B是包括鋁皿重量A的乾燥前樣品重量(單位:g)。
4.塗料黏度(單位:cP)
根據下列程序使用測量裝置(Brookfield數位式黏度計,RV DV2T)評估黏著劑組成物的塗料黏度。
將220mL黏著劑組成物放入250mL PE瓶中,然後密合瓶蓋並用封口膜等緊密封以防止溶劑揮發。之後,把黏著劑組成物留在恆溫度/濕度(23℃,50%相對濕度)條件下以移除氣泡。然後,移除密封與蓋子。之後,將轉軸以不使氣泡產生的角度放入黏著劑組成物中,及將轉軸連接黏度計然後調整,使得黏著劑組成物之液位與轉軸的溝槽一致。之後,在其中扭矩為20%(±1%)的rpm條件下測量黏度。
5.潛變(單位:μm)
將實施例與比較例各者所製成之偏光片裁切
成寬度10mm與長度10mm的大小以製備樣品。之後,把附接至黏著層的離型PET膜剝離,及使用2kg滾筒根據JIS Z 0237規則將偏光片附接至無鹼玻璃以製備測量用樣品。之後,把測量用樣品在恆溫度/濕度條件(23℃,50% R.H.)下儲存5日。使用結構分析器(TA,製造商:Stable Micro Systems,UK)測量各潛變。具體地說,測量距離(單位:μm)來獲得潛變,該距離係當用1,000g荷重將測量用樣品之偏光片拉伸1,000秒時,使偏光片從玻璃基板推動的距離。
6.室溫黏著力(單位:gf/25mm)
將實施例與比較例各者所製成之偏光片在恆溫度/濕度條件(23℃,50% R.H.)下儲存5日,然後裁切成寬度25mm與長度100mm的大小以製備樣品。之後,把附接至黏著層的離型PET膜剝離,及使用2kg滾筒根據JIS Z 0237規則將偏光片附接至無鹼玻璃以製備測量用樣品。
將測量用樣品在恆溫度/濕度條件(23℃,50% R.H.)下儲存4小時。之後,使用結構分析器(TA,製造商:Stable Micro Systems,UK)測量在300mm/分鐘的剝離速率與180度的剝離角度下拉動偏光片使偏光片與玻璃基板完全分離所需要之力量,以測量在室溫的黏著力(單位:gf/25mm)。
此外,將測量用樣品在恆溫度/濕度條件(23℃,50% R.H.)下儲存4小時,然後在80℃老化24小時。使用結構分析器(TA,製造商:Stable Micro Systems,UK)測
量在300mm/分鐘的剝離速率與180度的剝離角度下拉動偏光片使偏光片與玻璃基板完全分離所需要之力量,以測量在室溫老化後的黏著力(單位:gf/25mm)。
7.耐久性評估
將實施例與比較例各者所製成之偏光片裁切成180mm X 250mm(長度X寬度)的大小以製備樣品,及把樣品附接在玻璃基板上以製備測量用樣品。
將測量用樣品分別靜置500小時與1000小時,及觀測氣泡或剝離的發生以評估耐熱性。
此外,將測量用樣品留在85℃的溫度與85% R.H.的相對溼度下500小時,然後觀測氣泡或剝離的發生以評估抗濕性與耐熱性。
<評估準則>
OK:無氣泡與剝離
NG:氣泡與/或剝離
如表1與表2所顯示,和比較例1至4各者之黏著劑組成物比較,其中使用包括具有[式1]表示的單體之丙烯酸共聚物的黏著劑樹脂之實施例1至9各者的黏著劑組成物在高溫度與高溫度/高濕度環境中具有極佳耐久性,且在黏著層物理性質上較少隨時間而變化。
Claims (11)
- 如請求項1之黏著劑樹脂,其中該丙烯酸共聚物具有重量平均分子量為500,000g/mol至1,500,000g/mol。
- 如請求項1之黏著劑樹脂,其中該丙烯酸共聚物具有支鏈聚合物結構。
- 如請求項1之黏著劑樹脂,其中該單體混合物包含以100重量份之該單體混合物為基準計,0.01重量份至1重量份之量的[式1]表示之單體。
- 如請求項1之黏著劑樹脂,其中該單體混合物包含:以100重量份之該單體混合物為基準計,84重量份至99.89重量份之(甲基)丙烯酸烷酯系單體;0.1至15重量份之具有可交聯官能基的(甲基)丙烯酸單體;及0.01至1重量份之上[式1]表示之單體。
- 一種用於光學構件之黏著劑組成物,該組成物包含如請求項1至6中任一項之黏著劑樹脂與多官能 固化劑。
- 如請求項7之黏著劑組成物,其中包括以100重量份之該黏著劑樹脂為基準計,0.01至1重量份的量之該多官能固化劑。
- 一種偏光片,其包含黏著劑層,該黏著劑層包括用於如請求項7之光學構件的黏著劑組成物之固化產物。
- 一種顯示裝置,其包含如請求項10之偏光片。
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EP3760687B1 (en) | 2024-02-14 |
WO2020116782A1 (ko) | 2020-06-11 |
CN111971361B (zh) | 2022-05-06 |
EP3760687A1 (en) | 2021-01-06 |
KR102259745B1 (ko) | 2021-06-02 |
US20210147728A1 (en) | 2021-05-20 |
JP2021527725A (ja) | 2021-10-14 |
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