TWI567178B - A nematic liquid crystal composition, and a liquid crystal display device using the same - Google Patents
A nematic liquid crystal composition, and a liquid crystal display device using the same Download PDFInfo
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- TWI567178B TWI567178B TW102120661A TW102120661A TWI567178B TW I567178 B TWI567178 B TW I567178B TW 102120661 A TW102120661 A TW 102120661A TW 102120661 A TW102120661 A TW 102120661A TW I567178 B TWI567178 B TW I567178B
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Description
本發明係關於一種作為液晶顯示材料而有用之介電各向異性(Δε)顯示負值之向列型液晶組成物及使用其之液晶顯示元件。
液晶顯示元件被應用於以鐘錶、計算器為代表之各種測定機器、汽車用面板、文字處理機、電子記事本、印表機、電腦、電視、鐘錶、廣告顯示板等中。作為液晶顯示方式,具有代表性者有TN(扭轉向列)型、STN(超扭轉向列)型、使用TFT(薄膜電晶體)之VA(垂直配向)型或IPS(橫向電場效應)型等。對於該等液晶顯示元件所使用之液晶組成物,要求對水分、空氣、熱、光等外部因素具有穩定性,且要求於以室溫為中心時儘可能廣之溫度範圍內顯示液晶相、為低黏性、且驅動電壓較低。進而,液晶組成物由數種至數十種化合物構成以使介電各向異性(Δε)或/及折射率各向異性(Δn)等相對於各顯示元件為最佳值。
於垂直配向型顯示器中,使用Δε為負之液晶組成物,並將其廣泛地應用於液晶電視等。另一方面,對於所有驅動方式,均要求低電壓驅動、高速應答、較廣之動作溫度範圍。即,要求Δε之絕對值較大、黏度(η)較小、向列相-等向性液體相轉移溫度(Tni)較高。又,由於Δn與單元間隙(d)之積即Δn×d之設定,因此必需配合單元間隙來將液晶組成物之Δn調節為適當之範圍。此外,於將液晶顯示元件應用於電視等之
情形時,由於重視高速應答性,故而要求有旋轉黏性(rotational viscosity,γ 1)較小之液晶組成物。尤其近年來,為使單元間隙變薄以實現高速應答化,必需於減小黏度之同時增大Δn。因此,於專利文獻1或專利文獻2中,亦已揭示有使用具有經氟取代之聯三苯(terphenyl)結構之化合物之液晶組成物。
另一方面,為使液晶組成物實用地使用於液晶顯示元件,必需於顯示品質中不良情況不會發生。尤其於由TFT元件等驅動之主動矩陣驅動液晶顯示元件所使用之液晶組成物中,必需具有較高之比電阻值或較高之電壓保持率。此外,亦必需相對於光或熱等外部刺激具有穩定性。針對於此,揭示有用以提高對熱之穩定性之抗氧化劑或使用其之液晶組成物(參照專利文獻3及專利文獻4),但該等未必稱得上充分,尤其由於具有較大之Δn之液晶化合物對於光或熱之穩定性相對較差,故而此種液晶組成物中之品質穩定性稱不上充分。
又,隨著液晶顯示元件之用途進一步擴大,可見到其使用方法、製造方法亦發生較大變化,為應對該等情況,要求使如習知之基本物性值以外之特性最佳化。即,隨著使用液晶組成物之液晶顯示元件廣泛地使用VA(垂直配向)型或IPS(橫向電場效應)型等,而能朝著使用實用化之其大小為50型以上之超大型尺寸之顯示元件。隨著基板尺寸之大型化,液晶組成物向基板中之注入方法亦由習知之真空注入法變為成為注入方法之主流的滴下注入(ODF)法(參照專利文獻5),但將液晶組成物向基板滴下時之滴下痕導致顯示品質降低之問題已浮上檯面。進而,以液晶顯示元件中之液晶材料之預傾角之生成與高速應答性為目的,開發出PS液晶顯示元件(polymer stabilized,聚合物穩定化)、PSA液晶顯示元件(polymer sustained alignment,聚合物維持配向)(參照專利文獻6),但滴下痕問題成為更大之問題。即,該等顯示元件之特徵在於,將單體添加至液晶組成物
中,並使組成物中之單體發生硬化,於多數之情形時,藉由對組成物照射紫外線而使單體發生硬化。因此,當添加對光之穩定性較差之成分時,有導致比電阻值或電壓保持率之降低,視情況而同時誘發滴下痕之產生,由顯示不良導致液晶顯示元件之良率變差之問題。
如此,要求開發一種可維持高速應答性等作為液晶顯示元件所要求之特性或性能,同時對光或熱等之穩定性較高,且難以產生滴下痕或線殘像等顯示不良之液晶顯示元件。
[專利文獻1]日本特開2003-327965號
[專利文獻2]WO2007/077872號
[專利文獻3]日本特開平9-124529號
[專利文獻4]日本特開2006-169472號
[專利文獻5]日本特開平6-235925號
[專利文獻6]日本特開2002-357830號
本發明所欲解決之課題在於提供一種具有較廣溫度範圍之液晶相、黏度或旋轉黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負的液晶組成物,進而提供一種藉由使用該液晶組成物而使顯示品質優異、難以產生滴下痕或線殘像等顯示不良之VA型或PSVA(polymer sustained vertical alignment,聚合物穩定垂直配向)型等高速應答之液晶顯示元件。
本發明人對各種液晶化合物及各種化學物質進行研究,結果
發現藉由組合特定之化合物可解決上述課題,從而完成本發明。
本發明提供一種於25℃下具有絕對值為2至8之負介電各向異性之向列型液晶組成物,進而提供一種使用其之液晶顯示元件,該向列型液晶組成物之特徵在於:含有具有絕對值為4以上之負介電各向異性之液晶化合物1種或2種以上並且其含量為3%以上,且含有通式(II-1)所表示之抗氧化劑1種或2種以上,
(式中,My表示碳數1至25之烴(該烴中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意的氫原子可由氟原子取代,Xy表示碳數1至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CF2CF2-、-CH=CH-COO-、-CH=CH-OCO-、-COO-CH=CH-、-OCO-CH=CH-、-CH=CH-、-C≡C-、單鍵、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意之氫原子可由氟原子取代,l表示2~6之整數)。
本發明之液晶組成物可獲得非常低之黏度或旋轉黏性,於低溫下之溶解性良好,比電阻或電壓保持率較高,因熱或光而受到之變化極其小,故而製品之實用性較高,使用該液晶組成物之VA型或PSVA型等液
晶顯示元件可達成高速應答,滴下痕或線殘像等顯示不良得到抑制,從而非常有用。
於本發明之液晶組成物中,含有具有絕對值為4以上之負介電各向異性之液晶化合物1種或2種以上,其含量為3質量%以上,較佳為5質量%以上,進而較佳為10質量%以上,特佳為20質量%以上。進而具體而言,較佳為3質量%至70質量%,進而較佳為5質量%至60質量%,進而較佳為10質量%至60質量%,特佳為20質量%至60質量%。再者,液晶化合物之介電各向異性表示於25℃下之值。
於本發明之液晶組成物中,含有通式(II-1)所表示之抗氧化劑1種或2種以上,
(式中,My表示碳數1至25之烴(該烴中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意的氫原子可由氟原子取代,Xy表示碳數1至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直
接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CF2CF2-、-CH=CH-COO-、-CH=CH-OCO-、-COO-CH=CH-、-OCO-CH=CH-、-CH=CH-、-C≡C-、單鍵、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意之氫原子可由氟原子取代,1表示2~6之整數)。
My較佳為碳數1至25之烴(該烴中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)。Xy較佳為碳數2至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、單鍵、1,4-伸苯基、反式-1,4-伸環己基。1較佳為2~4,尤佳為2。
作為通式(II-1)所表示之抗氧化劑,更佳為以下之通式(II-2)所表示之化合物,
(式中,Mx表示碳數1至25之烴(該烴中之1個或2個以上之-CH2-可
以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-),X表示碳數1至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CF2CF2-、-CH=CH-COO-、-CH=CH-OCO-、-COO-CH=CH-、-OCO-CH=CH-、-CH=CH-、-C≡C-、單鍵、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意的氫原子可由氟原子取代,a、b、c、d分別獨立表示0或1,a+b+c+d表示2以上)。
Mx較佳為碳數2至15之烴(該烴中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-),X較佳為碳數2至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、單鍵、1,4-伸苯基、反式-1,4-伸環己基,a+b+c+d更佳為2至4,特佳為2。
進而具體而言,較佳為通式(II)之受阻酚衍生物,
(式中,M表示碳數1至15之伸烷基(該伸烷基中之1個或2個以上之-CH2-可以氧原子不直接鄰接之方式取代為-O-、-CO-、-COO-、-OCO-)、-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CF2CF2-、-CH=CH-COO-、-CH=CH-OCO-、-COO-CH=CH-、-OCO-CH=CH-、-CH=CH-、-C≡C-、單鍵、1,4-伸苯基、反式-1,4-伸環己基,1,4-伸苯基之任意的氫原子可由氟原子取代)。
通式(II)中之M進而較佳為碳數1至15之伸烷基,若考
慮揮發性則較佳為碳數為較大之數值,若考慮黏度則較佳為碳數不會過大者。由以上可知,通式(II)中之M更佳為碳數2至15,特佳為碳數2至10。
進而具體而言,較佳為式(II-a)所表示之化合物。
本發明之液晶組成物含有抗氧化劑1種或2種以上,其含量較佳為0.001至1質量%,更佳為0.001至0.5質量%,特佳為0.01至0.3質量%。
作為本發明之液晶組成物所含有的具有絕對值為4以上之負介電各向異性之液晶化合物,較佳為通式(I-a)所表示之化合物,具體而言,較佳為通式(I-a1)至(I-a10)所表示之化合物,
(式中,R1及R2分別獨立表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基,環A及環B分別獨立表示反式-1,4-伸環己基或1,4-伸苯基,1,4-伸苯基之任意的氫原子可由氟原子取代,Z1表示-OCH2-、-CH2O-、-CF2O-、-OCF2-、-CH2CH2-、-CF2CF2-或單鍵,m表示0、1或2),
式中,R7表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基,較佳為碳數1至5之烷基、碳數2至5之烯基,更佳為碳數2至5之烷基;R8表示碳數1至8之烷氧基或碳數2至8之烯氧基,較佳為碳數1至5之烷氧基、碳數2至5之烯氧基,更佳為碳數1至5之烷氧基;R9表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基,較佳為碳數1至5之烷氧基或碳數2至5之烯氧基,更佳為碳數1至5之烷氧基。更佳為通式(I-a)中之Z1為-CH2O-之通式(I-a6)至(I-a10)所表示之化合物。
於25℃下具有絕對值為4以上之負介電各向異性的通式(I-a)所表示之液晶化合物例如可列舉如下者。
再者,delta-ep表示各液晶化合物於25℃下之介電各向異性Δε,其值係以如下方式求出:相對於在25℃下介電各向異性約為0之液晶組成物,製備分別添加有各液晶化合物10質量%之組成物,自該組成物之介電各向異性Δε之測定值進行外插而求出。
本發明之液晶組成物所含有的具有絕對值為4以上之負介電各向異性之液晶化合物,為通式(I-b)或(I-bb)所表示之化合物亦佳。
式中,R3及R4分別獨立表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基;R3較佳為碳數1至5之烷基、碳數2至5之烯基,R4較佳為碳數1至5之烷基、碳數1至5之烷氧基。環C及環D分別獨立表示反式-1,4-伸環己基或1,4-伸苯基,1,4-伸苯基之任意的氫原子可由氟原子取代,較佳為反式-1,4-伸環己基。Z21及Z22分別獨立表示-OCH2-、-CH2O-、-CF2O-、-OCF2-、-CH2CH2-、-CF2CF2-、-COO-、-OCO-、-CH=CH-或單鍵,n表示0、1或2,較佳為0或1。
於25℃下具有絕對值為4以上之負介電各向異性的通式(I-b)或(I-bb)所表示之液晶化合物例如可列舉如下者。
再者,delta-ep表示各液晶化合物之於25℃下之介電各向異
性Δε,其值係以如下方式求出:相對於在25℃下介電各向異性約為0之液晶組成物,製備分別添加有各液晶化合物10質量%之組成物,自該組成物之介電各向異性Δε之測定值進行外插而求出。
本發明之液晶組成物所含有的具有絕對值為4以上之負介電各向異性之液晶化合物,為通式(I-c)或(I-cc)所表示之化合物亦佳。
式中,R5及R6分別獨立表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基;R5較佳為碳數1至5之烷基、碳數2至5之烯基;R6較佳為碳數1至5之烷基、碳數1至5之烷氧基。環E及環F分別獨立表示反式-1,4-伸環己基或1,4-伸苯基,1,4-伸苯基之任意的氫原子可由氟原子取代,較佳為反式-1,4-伸環己基。Z31及Z32分別獨立表示-OCH2-、-CH2O-、-CF2O-、-OCF2-、-CH2CH2-、-CF2CF2-、-COO-、-OCO-、-CH=CH-或單鍵,p表示0、1或2,較佳為0或1。
於25℃下具有絕對值為4以上之負介電各向異性的通式(I-c)或(I-cc)所表示之液晶化合物例如可列舉如下者。
再者,delta-ep表示各液晶化合物之於25℃下之介電各向異性Δε,其值係以如下方式求出:相對於在25℃下介電各向異性約為0之液晶組成物,製備分別添加有各液晶化合物10質量%之組成物,自該組成物之介電各向異性Δε之測定值進行外插而求出。
本發明之液晶組成物含有具有絕對值為4以上之負介電各向異性之液晶化合物1種或2種以上,更佳為含有具有絕對值為4.5以上之負介電各向異性之液晶化合物,特佳為含有具有絕對值為5以上之負介電各向異性之液晶化合物。
本發明之液晶組成物亦較佳為進而含有通式(III)所表示之化合物。
式中,R10或R11表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基。
本發明之液晶組成物較佳為含有通式(III)所表示之化合物1種至5種,其含量較佳為3至30質量%,更佳為5至25質量%。
本發明之液晶組成物可進而含有通式(IV-a)至(IV-d)所表示之化合物。
式中,R41至R48分別獨立表示碳數1至8之烷基、碳數1至8之烷氧基、碳數2至8之烯基或碳數2至8之烯氧基。
於本發明之液晶組成物中,較佳為含有通式(IV-a)至(IV-d)所表示之化合物1種至10種,更佳為含有1種至8種,其含量較佳為5至80質量%,更佳為10至70質量%,特佳為20至60質量%。
本發明之液晶組成物之於25℃下之介電各向異性Δε為-2.0至-8.0,較佳為-2.0至-6.0,更佳為-2.0至-5.0,特佳為-2.5至-4.0。
本發明之液晶組成物之於20℃下之折射率各向異性Δn為0.08至0.14,更佳為0.09至0.13,特佳為0.09至0.12。若進一步詳細敍述,當對應於較薄之單元間隙之情形時,較佳為0.10至0.13,當對應於較厚之
單元間隙之情形時,較佳為0.08至0.10。
本發明之液晶組成物之於20℃下之黏度η為10至30mPa.s,更佳為10至25mPa.s,特佳為10至22mPa.s。
本發明之液晶組成物之於20℃下之旋轉黏性γ 1為60至130mPa.s,更佳為60至110mPa.s,特佳為60至100mPa.s。
本發明之液晶組成物之Tni為60℃至120℃,更佳為70℃至100℃,特佳為70℃至85℃。
本發明之液晶組成物除上述化合物以外,亦可含有通常之向列型液晶、層列型液晶、膽固醇狀液晶、聚合性單體等。
為製作PS模式、PSA模式或PSVA模式等液晶顯示元件,本發明之液晶組成物亦可含有聚合性化合物。作為可使用之聚合性化合物,可列舉藉由光等能量射線進行聚合之光聚合性單體等,例如可列舉聯苯衍生物、聯三苯衍生物等具有六員環連結複數個而成之液晶骨架的聚合性化合物等。進而具體而言,較佳為通式(V)所表示之二官能單體。
式中,X51及X52分別獨立表示氫原子或甲基,Sp1及Sp2分別獨立表示單鍵、碳數1至8之伸烷基或-O-(CH2)s-(式中,s表示2至7之整數,氧原子鍵結於芳香環上),Z51表示-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CH2CH2-、-CF2CF2-、-CH=CH-COO-、-CH=CH-OCO-、-COO-CH=CH-、-OCO-CH=CH-、-COO-CH2CH2-、-OCO-CH2CH2-、-CH2CH2-COO-、-CH2CH2-OCO-、-COO-CH2-、-OCO-CH2-、-CH2-COO-、-CH2-OCO-、-CY1=CY2-
(式中,Y1及Y2分別獨立表示氟原子或氫原子)、-C≡C-或單鍵,M51表示1,4-伸苯基、反式-1,4-伸環己基或單鍵,1,4-伸苯基之任意的氫原子可由氟原子取代。Xa至Xh分別獨立表示氫原子、氟原子或甲基。
X51及X52表示氫原子之二丙烯酸酯衍生物、X51及X52具有甲基之二甲基丙烯酸酯衍生物均較佳,X51及X52之一者表示氫原子、另一者表示甲基之化合物亦較佳。該等化合物之聚合速度係二丙烯酸酯衍生物最快,二甲基丙烯酸酯衍生物較慢,非對稱化合物處於二者中間,可根據其用途來使用較佳之態樣。於PSA顯示元件中,特佳為二甲基丙烯酸酯衍生物。
Sp1及Sp2分別獨立表示單鍵、碳數1至8之伸烷基或-O-(CH2)s-,於PSA顯示元件中,較佳為至少一者為單鍵,且較佳為Sp1及Sp2均表示單鍵之化合物或一者為單鍵、另一者表示碳數1至8之伸烷基或-O-(CH2)s-之態樣。於該情形時,較佳為1至4之烷基,s較佳為1至4。
Z51較佳為-OCH2-、-CH2O-、-COO-、-OCO-、-CF2O-、-OCF2-、-CH2CH2-、-CF2CF2-或單鍵,更佳為-COO-、-OCO-或單鍵,特佳為單鍵。
M51表示任意之氫原子可由氟原子取代之1,4-伸苯基、反式-1,4-伸環己基或單鍵,較佳為1,4-伸苯基或單鍵。於M51表示單鍵以外之環結構之情形時,Z51亦較佳為單鍵以外之連結基,於M51為單鍵之情形時,Z51較佳為單鍵。
就該等方面而言,於通式(V)中,具體而言,Sp1及Sp2之間之環結構較佳為以下所記載之結構。
於通式(V)中,於M51表示單鍵,環結構由2個環形成之情形時,較佳為表示以下之式(Va-1)至式(Va-5),更佳為表示式(Va-1)至式(Va-3)。
(式中,兩端鍵結於Sp1或Sp2上)
包含該等骨架之聚合性化合物的聚合後之配向限制力最適合於PSA型液晶顯示元件,由於可獲得良好之配向狀態,故而顯示不均得到抑制或完全不產生顯示不均。
於將單體添加至本發明之液晶組成物中之情形時,即便於不存在聚合起始劑之情形時亦進行聚合,但為促進聚合亦可含有聚合起始劑。作為聚合起始劑,可列舉:安息香醚類、二苯基酮類、苯乙酮類、苯偶醯縮酮類(benzil ketal)、醯基氧化膦類等。
含有本發明之聚合性化合物之液晶組成物藉由經紫外線照射使其中所含之聚合性化合物進行聚合而賦予液晶配向能,從而用於利用液晶組成物之折射率各向異性來控制光之透射光量的液晶顯示元件。作為液晶顯示元件,對AM-LCD(主動矩陣液晶顯示元件)、TN(向列型液晶顯示元件)、STN-LCD(超扭轉向列型液晶顯示元件)、OCB-LCD及IPS-LCD(橫向電場效應液晶顯示元件)有用,尤其對AM-LCD有用,可用於透射型或反射型之液晶顯示元件中。
本發明之液晶顯示元件具有:第一基板,其具備由透明導電
性材料所構成之共用電極;第二基板,其具備由透明導電性材料所構成之像素電極與控制各像素所具備之像素電極之薄膜電晶體;及液晶組成物,其夾持於上述第一基板與第二基板之間,且該液晶組成物中之液晶分子未施加電壓時之配向大致垂直於上述基板,更具體而言係如下所述。
液晶顯示元件所使用之液晶單元之2片基板可使用玻璃或如塑膠之具有柔軟性之透明材料,另一方面亦可為矽等不透明材料。具有透明電極層之透明基板例如可藉由在玻璃板等透明基板上濺鍍氧化銦錫(ITO)而獲得。
彩色濾光片例如可藉由顏料分散法、印刷法、電鍍法或染色法等製成。若以利用顏料分散法之彩色濾光片之製成方法作為一例進行說明,將彩色濾光片用硬化性著色組成物塗佈於該透明基板上,實施圖案化處理,藉由加熱或光照射使其發生硬化。藉由對紅、綠、藍之3色分別實施該步驟,可製成彩色濾光片用像素部。此外,亦可於該基板上設置設有TFT、薄膜二極體、金屬絕緣體、金屬比電阻元件等主動元件之像素電極。
以透明電極層成為內側之方式使上述基板相對。於該情形時,可經由間隔物來調整基板之間隔。此時,較佳為以所獲得之調光層之厚度成為1至100μm之方式進行調整。進而較佳為1.5至10μm,於使用偏光板之情形時,較佳為以對比度成為最大之方式調整液晶之折射率各向異性Δn與單元厚度d之積。又,於有兩片偏光板之情形時,亦可以調整各偏光板之偏光軸而使視角或對比度變得良好之方式進行調整。進而,亦可使用用以擴大視角之相位差膜。作為間隔物,例如可列舉玻璃粒子、塑膠粒子、氧化鋁粒子或光阻材料等。其後,將環氧系熱硬化性組成物等密封劑以設有液晶注入口之形狀之形式於該基板進行絲網印刷,並且使該基板彼此貼合,進行加熱使密封劑熱硬化。
使含有聚合性化合物之液晶組成物夾持於2片基板間之方
法可使用通常之真空注入法或ODF法等,於真空注入法中雖不產生滴下痕,但注入之後會有殘留之課題,於本發明中,更佳可使用ODF法來用於製造之顯示元件。
本發明之液晶顯示元件亦可為於施加電壓下或未施加電壓下使該液晶組成物中所含有之聚合性化合物聚合而製作之液晶顯示元件,更具體而言係如下所述。
為獲得液晶之良好之配向性能,由於較理想為適當之聚合速度,故而使聚合性化合物聚合之方法較佳為藉由單獨或併用或依序照射紫外線或電子束等活性能量射線而使其聚合之方法。於使用紫外線之情形時,可使用偏光光源,亦可使用非偏光光源。又,於使含有聚合性化合物之液晶組成物以夾持於2片基板間之狀態進行聚合之情形時,至少照射面側之基板必須相對於活性能量射線而賦有適當之透明性。又,亦可使用如下手段:於進行光照射時使用遮罩而僅使特定之部分聚合之後,藉由改變電場或磁場、或溫度等條件使未聚合部分之配向狀態發生變化,進而照射活性能量射線使其聚合。尤其於進行紫外線曝光時,較佳為一面對含有聚合性化合物之液晶組成物施加交流電場一面進行紫外線曝光。所施加之交流電場較佳為頻率10Hz至10kHz之交流,更佳為頻率60Hz至10kHz之交流,電壓係依賴於液晶顯示元件所需之預傾角而選擇。即,可藉由所施加之電壓而控制液晶顯示元件之預傾角。於MVA(multi-domain vertical alignment,多域垂直配向)模式之液晶顯示元件中,就配向穩定性及對比度之觀點而言,較佳為將預傾角控制在80度至89.9度。
照射時之溫度較佳為處於保持本發明之液晶組成物之液晶狀態的溫度範圍內。較佳為於接近室溫之溫度、即典型而言於15至35℃之溫度下進行聚合。作為產生紫外線之燈,可使用金屬鹵素燈、高壓水銀燈或超高壓水銀燈等。又,作為所照射之紫外線之波長,較佳為不在照射液
晶組成物之吸收波長區域的波長區域之紫外線,且較佳為視需要將紫外線截斷而使用。所照射之紫外線之強度較佳為0.1mW/cm2至100W/cm2,更佳為2mW/cm2至50W/cm2。所照射之紫外線之能量可適當地進行調整,較佳為10mJ/cm2至500J/cm2,更佳為100mJ/cm2至200J/cm2。於照射紫外線時,可改變強度。照射紫外線之時間係根據所照射之紫外線強度而適當地選擇,較佳為10秒至3600秒,更佳為10秒至600秒。
使用本發明之液晶組成物之液晶顯示元件係同時實現高速應答與滴下痕或線殘像等顯示不良之抑制之有用者,尤其於主動矩陣驅動用液晶顯示元件中有用,可應用於VA模式、PSVA模式、PSA模式、IPS模式或ECB(electrically controlled birefringence,電控雙折射)模式用液晶顯示元件中。
[實施例]
以下,列舉實施例進一步詳細地敍述本發明,但本發明並非限定於該等實施例者。又,以下實施例及比較例之組成物中之「%」表示『質量%』。
實施例中,所測定之特性係如下所述。
Tni:向列相-等向性液體相轉移溫度(℃)
Δn:20℃下之折射率各向異性
Δε:25℃下之介電各向異性
η:20℃下之黏度(mPa.s)
γ 1:20℃下之旋轉黏性(mPa.s)
RT:20℃下之應答速度(msec)(單元厚度3.5μm之VA單元)
VHR(Init):於頻率60Hz、施加電壓1V之條件下之60℃下之電壓保持率(%)
VHR(HEAT):於100℃之狀態下放置48小時之後所測定的於頻率60
Hz、施加電壓1V之條件下之60℃下之電壓保持率(%)
滴下痕:液晶顯示裝置之滴下痕之評價係以目視對整體顯示黑色之情形時呈白色浮現之滴下痕進行以下4個等級之評價。
◎:無滴下痕
○:略微有滴下痕但為可容許之程度
△:有滴下痕且為無法容許之程度
×:有滴下痕且為相當差之程度
線殘像:液晶顯示元件之線殘像試驗係於使顯示區域內顯示規定之固定圖案2000小時之時,以目視對固定圖案之邊界部分所產生的線狀殘像之程度進行以下4個等級之評價。
◎:無線殘像
○:略微有線殘像但為可容許之程度
△:有線殘像且為無法容許之程度
×:有線殘像且為相當差之程度
再者,於實施例中,對化合物之記載使用以下略號。
(側鏈)
-n -CnH2n+1 碳數n之直鏈狀烷基
n- CnH2n+1- 碳數n之直鏈狀烷基
-On -OCnH2n+1 碳數n之直鏈狀烷氧基
nO- CnH2n+1O- 碳數n之直鏈狀烷氧基
-V -CH=CH2
V- CH2=CH-
-V1 -CH=CH-CH3
1V- CH3-CH=CH-
(環結構)
(實施例1、比較例1、比較例2及比較例3)
製備液晶組成物LC-A(比較例1),且製備相對於LC-A 99.95%而添加有抗氧化劑(II-a)0.05%之液晶組成物LC-1(實施例1)。進而,製備相對於LC-A 99.95%而分別添加有抗氧化劑(St-1)及(St-2)0.05%之液晶組成物LC-A1(比較例2)及LC-A2(比較例3)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
再者,抗氧化劑(St-1)及(St-2)為如下所表示之化合物。
於VHR(HEAT)、滴下痕之有無、線殘像之有無中確認到顯著之差異。自該等之結果可確認,本發明之液晶組成物LC-1係具有較廣溫度範圍之液晶相、黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例2、比較例4、比較例5及比較例6)
製備液晶組成物LC-B(比較例4),且製備相對於LC-B 99.98%而添加有抗氧化劑(II-a)0.02%之液晶組成物LC-2(實施例2)。進而,製備相對於LC-B 99.98%而分別添加有抗氧化劑(St-1)及(St-2)0.02%之液晶組成物LC-B1(比較例5)及LC-B2(比較例6)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-2係具有較廣溫度範圍之液晶相、黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例3、比較例7、比較例8及比較例9)
製備液晶組成物LC-C(比較例7),且製備相對於LC-C 99.9%而添加有抗氧化劑(II-a)0.1%之液晶組成物LC-3(實施例3)。進而,製備相對於LC-C 99.9%而分別添加有抗氧化劑(St-1)及(St-2)0.1%之液晶組成物LC-C1
(比較例8)及LC-C2(比較例9)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-3係具有較廣溫度範圍之液晶相、黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例4、比較例10、比較例11及比較例12)
製備液晶組成物LC-D(比較例10),且製備相對於LC-D 99.8%而添加
有抗氧化劑(II-a)0.2%之液晶組成物LC-4(實施例4)。進而,製備相對於LC-D 99.8%而分別添加有抗氧化劑(St-1)及(St-2)0.2%之液晶組成物LC-D1(比較例11)及LC-D2(比較例12)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-4係具有較廣溫度範圍之液晶相、黏性較小,於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例5及比較例13)
製備液晶組成物LC-E(比較例13),且製備相對於LC-E 99.8%而添加有抗氧化劑(II-a)0.2%之液晶組成物LC-5(實施例5)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-5係具有較廣溫度範圍之液晶相、黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例6、實施例7、比較例14及比較例15)
製備液晶組成物LC-F(比較例14),且製備相對於LC-F 99.95%而添加
有抗氧化劑(II-a)0.05%之液晶組成物LC-6(實施例6)。又,製備液晶組成物LC-G(比較例15),且製備相對於LC-G 99.95%而添加有抗氧化劑(II-a)0.05%之液晶組成物LC-7(實施例7)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-6及LC-7係具有較廣溫度範圍之液晶相、黏性較小、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定
之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例8及比較例16)
製備液晶組成物LC-H(比較例16),且製備相對於LC-H 99.99%而添加有抗氧化劑(II-a)0.01%之液晶組成物LC-8(實施例8)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-8係具有較廣溫度範圍之液晶相、黏性較小、
於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
(實施例9及比較例17)
製備液晶組成物LC-I(比較例17),且製備相對於LC-I 99.99%而添加有抗氧化劑(II-a)0.01%之液晶組成物LC-9(實施例9)。對該等之物性值之測定、VHR(Init)及VHR(HEAT)之測定、滴下痕之有無、線殘像之有無進行評價,結果如下表所示。
可確認,LC-9係具有較廣溫度範圍之液晶相、於低溫下之溶解性良好、比電阻或電壓保持率較高、對熱或光穩定之Δε為負之液晶組成物,且使用其之液晶顯示元件之顯示品質優異,難以產生滴下痕或線殘像等顯示不良。
Claims (9)
- 一種向列型液晶組成物,其具有25℃下絕對值為2至8之負介電各向異性,含有具有絕對值為4以上之負介電各向異性之液晶化合物1種或2種以上並且其含量為3質量%以上,且含有通式(II)所表示之抗氧化劑1種或2種以上並且其含量為0.001質量%至1質量%,
- 如申請專利範圍第1項之向列型液晶組成物,其中具有絕對值為4以上之負介電各向異性之液晶化合物為通式(I-a),
- 如申請專利範圍第1或2項之向列型液晶組成物,其進而含有:具有絕對值為4以上之負介電各向異性之液晶化合物即通式(I-b)或(I-bb),
- 如申請專利範圍第1或2項之向列型液晶組成物,其進而含有:具有絕對值為4以上之負介電各向異性之液晶化合物即通式(I-c)或(I-cc),
- 如申請專利範圍第1或2項之向列型液晶組成物,其中通式(II)所表示之抗氧化劑為通式(II-a)所表示之化合物,
- 如申請專利範圍第2項之向列型液晶組成物,其中通式(I-a)中之Z1為-CH2O-。
- 如申請專利範圍第1或2項之向列型液晶組成物,其含有聚合性化合物1種或2種以上。
- 一種液晶顯示元件,係具有:第一基板,其具備由透明導電性材料所構成之共用電極;第二基板,其具備由透明導電性材料所構成之像素電極與控制各像素所具備之像素電極之薄膜電晶體;及液晶組成物,其被夾持於上述第一基板與第二基板之間;該液晶組成物中之液晶分子未施加電壓時之配向係對上述基板呈80度至89.9度;該液晶顯示元件使用有申請專利範圍第1至7項中任一項之向列型液晶組成物作為該液晶組成物。
- 一種液晶顯示元件,其係使用申請專利範圍第7項之向列型液晶組成物,於施加電壓下或未施加電壓下使該液晶組成物中所含之聚合性化合物聚合而製作。
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