TWI596193B - 液晶組成物及使用其之液晶顯示元件 - Google Patents
液晶組成物及使用其之液晶顯示元件 Download PDFInfo
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Description
本發明係關於作為液晶顯示材料有用之介電各向異性(Δε)顯示負值的向列型液晶組成物及使用其之液晶顯示元件。
液晶顯示元件係使用在以鐘錶、電算機為代表之家庭用各種電器、量測儀器、車用面板、文字處理機、電子筆記本、印表機、電腦、電視等。以液晶顯示方式而言,在其代表性者可舉出TN(扭轉向列)型、STN(超扭轉向列)型、DS(動態光散射)型、GH(賓/主)型、IPS(平面轉換)型、OCB(光學補償複折射)型、ECB(電控複折射)型、VA(垂直配向)型、CSH(彩色超垂直)型、或者FLC(鐵電性液晶)等。此外以驅動方式而言亦可舉出靜態驅動、多路驅動、單純矩陣式、以TFT(薄膜電晶體)或TFD(薄膜二極體)等而驅動之主動矩陣(AM)式。
該等之顯示方式中,IPS型、ECB型、VA型、或者CSH型等係具有使用Δε顯示負值之液晶材料這樣的特徴。該等之中尤其以AM驅動之VA型顯示方式,係使用於要求高速且廣視角之顯示元件,例如電視等用途。
在用於VA型等顯示方式之向列型液晶組成物,係要求低電壓驅動、高速反應及寬廣之操作溫度範圍。亦及,要求Δε為負且絕對值大、黏度低、向列相-等向性液體相轉移溫度(Tni)高。此外,有必要從折射率各向異性(Δn)與胞隙(d)之積Δn×d的設定將液晶材料之Δn配合胞隙而調整至合適之範圍。再因在將液晶顯示元件應用在電視等時,重視高速反應性,故要求黏度(η)低之液晶材料。
到目前為止,一直是藉由將Δε為負且其絕對值大之化合物進行各種研究而改良液晶組成物之特性。
作為Δε為負之液晶材料,揭示有使用具有如下之2,3-二氟伸苯骨架的液晶化合物(A)及(B)(參見專利文獻1)的液晶組成物。
該液晶組成物係使用液晶化合物(C)及(D)作為Δε近乎為0之化合物,但該液晶組成物係在液晶電視等要求高速反應之液晶組成物中並無達成實現足夠低之黏性。
另一方面,亦已揭示有使用了由式(E)表示之
化合物的液晶組成物,但其為組合了上述液晶化合物(D)的Δn為小之液晶組成物(參見專利文獻2)或為改善反應速度而添加了如液晶化合物(F)之在分子內具有烯基的化合物(烯基化合物)的液晶組成物(參見專利文獻3),在使高Δn與高可靠性並存上需要進一步研究。
此外,亦已揭示有使用了由式(G)表示之化合物的液晶組成物(參見專利文獻4),但該液晶組成物亦為如上所述之液晶化合物(F)一般含有包含烯基化合物之化合物的液晶組成物,故有容易產生烙印或顯示不均等顯示不良之弊病。
另外,已揭示有關於對於含烯基化合物之液晶組成物的顯示不良的影響(參見專利文獻5),但一般而言烯基化合物之含量若減少則液晶組成物之η上升,且高速反應之達成變得困難,故難以並存顯示不良之抑制與高速反應。
在僅組合如此之Δε顯示為負值的化合物與液晶化合物(C)、(D)及(F)方面,係難以開發使高Δn與低η並存,另且沒有或抑制了顯示不良的Δε為負之液晶組成物。
此處已揭示於式(A)及式(G)組合了Δε近為零之式(I)的液晶組成物(參見專利文獻6)。然而在液晶顯示元件之製造步驟方面在將液晶組成物注入液晶胞時因使其成為極低壓故蒸氣壓低之化合物會揮發,故認為不能增加含量。因此,該液晶組成物係會限制式(I)之含量,雖顯示大的Δn,但有黏度顯著地高這樣的問題。從而,追求高Δn與低黏度之並存。
[專利文獻1]日本特開平8-104869號
[專利文獻2]歐洲專利申請公開第0474062號
[專利文獻3]日本特開2006-37054號
[專利文獻4]日本特開2001-354967號
[專利文獻5]日本特開2008-144135號
[專利文獻6]WO2007/077872
本發明所欲解決之課題,係在於提供不使Δn及Tni降低、η足夠小、Δε為負且其絕對值大的液晶組成物,並進一步提供使用其之沒有或抑制VA型等之顯示不良的液晶顯示元件。
本發明人係藉由研究各種聯苯衍生物及氟苯衍生物,並組合特定之化合物而發現可解決前述課題,並達到完成本發明。
本發明係提供含有由式(I)表示之化合物作為第一成分,
其含量係5至25%,並含有介電各向異性(Δε)為負且其絕對值較3為大之化合物作為第二成分的液晶組成物,此外,提供使用其之液晶顯示元件。
本發明之Δε為負的液晶組成物,係因不使Δn及Tni降低、黏度足夠地低,故使用其之VA型等液晶顯示元件係高速反應、並抑制了顯示不良,故非常地有用。
本發明中之液晶組成物中,含有由式(I)表示之化合物作為第一成分,
而其含量係較佳為5至25%,以其下限值而言較佳為5%,較佳為8%,較佳為10%,較佳為11%,以其上限值而言較佳為20%,較佳為18%,較佳為15%。若進一步詳述,則要得到高Δn其含量係較佳為10至25%,但
在重視抑制在低溫之沉降時其含量係較佳為3至15%。
含有Δε為負且其絕對值較3為大之化合物作為第二成分,而其含量係較佳為10至90%,更佳為20至80%,特佳為40至70%。
具體而言,第二成分係選自由一般式(II-1)及(II-2)
更佳為式中之R1及R2係各自獨立地為直鏈狀
之碳原子數1至5之烷基、烷氧基或碳原子數2至5之烯基、烯氧基,特佳為R1係碳原子數1至5之烷基、R2係碳原子數1至5之烷氧基。
p及q係更佳為各自獨立地為0或1。
更佳為環A及環B係各自獨立地為反式-1,4-伸環己基、1,4-伸苯基、2-氟-1,4-伸苯基、3-氟-1,4-伸苯基、3,5-二氟-1,4-伸苯基或2,3-二氟-1,4-伸苯基,反式-1,4-伸環己基或1,4-伸苯基為特佳。
本發明之液晶組成物係含有1種或2種以上第二成分,但較佳為含有2種至10種。
本發明之液晶組成物係在25℃下之Δε為-2.0至-6.0,但更佳為-2.5至-5.0,特佳為-2.5至-3.5。在25℃下之Δn為0.08至0.13,但更佳為0.09至0.13,特佳為0.10至0.12。若進一步詳述,則在對應薄的胞隙時係較佳為0.10至0.13,對應厚的胞隙時係較佳為0.08至0.10。在20℃下之η為10至30mPa.s,但更佳為10至25mPa.s,特佳為10至20mPa.s。Tni為60℃至120℃,但更佳為70℃至100℃,特佳為70℃至85℃。
由一般式(II-1)表示之化合物,係更佳為選自由一般式(II-1A)及(II-1B)表示之化合物的1種或2種以上,由一般式(II-2)表示之化合物,係更佳為一般式(II-2A)。
R3及R4係更佳為各自獨立地為直鏈狀之碳原子數1至5之烷基或碳原子數2至5之烯基,特佳為碳原子數1至5之烷基。
由一般式(II-1A)、(II-1B)及一般式(II-2A)表示之化合物係亦可單獨使用,亦可組合由一般式(II-1A)及(II-1B)表示之化合物,組合由一般式(II-1A)及(II-2A)表示之化合物或組合由一般式(II-1B)及(II-2A)表示之化合物,亦可將由一般式(II-1A)、(II-1B)及一般式(II-2A)表示之化合物全部組合使用。
藉由該等組合,使液晶組成物之組成比的變動亦可抑制。
本發明之液晶組成物係亦可進一步含有1種或2種以上選自由一般式(III-A)至一般式(III-J)表示之化合物群之化合物作為第三成分,
但更佳為含有2種至10種選自一般式(III-A)、(III-D)、(III-F)、(III-G)及(III-H)之化合物。另外,R5係表示碳原子數1至5之烷基或碳原子數2至5之烯基、R6係碳原子數1至5之烷基、碳原子數1至5之烷氧基、碳原子數2至5之烯基或碳原子數2至5之烯氧基,但更佳為R5係碳原子數1至5之烷基、R6係碳原子數1至5之烷基或碳原子數1至5之烷氧基。另外,由一般式(III-F)表示之化合物係表示R5為甲基且R6為丙基時及表示R5為丙基且R6為甲基時係由於變成表示與由式(I)表示之化合物相同之化合物,故由一般式(III-F)表示之化合物係除去R5表示為甲基且R6為丙基之化合物及R5表示為丙基且R6為甲基之化合物。
本發明之液晶組成物,係較佳為同時含有式(I)、一般式(II-1A)、(II-2A)及一般式(III-A),較佳為同時含有式(I)、一般式(II-1B)、(II-2A)及一般式(III-A),特佳為同時含有式(I)、一般式(II-1A)、(II-1B)、(II-2A)及一般式(III-A)。
本發明之液晶組成物係除上述化合物以外,
亦可含有一般之向列型液晶、層列型液晶、膽固醇型液晶、抗氧化劑、紫外線吸收劑、聚合性單體等。
例如含有聯苯衍生物、聯三苯衍生物等聚合性化合物作為聚合性單體,其含量係較佳為0.01%至2%。若進一步詳述,則較佳為於本發明之液晶組成物含有一種或二種以上由一般式(IV)表示之聚合性單體作為第4成分,
(式中,R7及R8係各自獨立地表示以下之式(R-1)至式(R-15)
之任一者,X1至X8係各自獨立地表示三氟甲基、三氟甲氧基、氟原子或氫原子)。
一般式(IV)中之聯苯骨架之結構,係更佳為式(IV-11)至式(IV-14),特佳為式(IV-11)。
含有由式(IV-11)至式(IV-14)表示之骨架的聚合性化合物係聚合後之配向控制力最佳,可得良好的配向狀態。
例如,同時含有式(I)、一般式(II-1A)、(II-1B)、(II-2A)、一般式(III-A)及一般式(IV)的含聚合性化合物液晶組成物係達成有高Δn與低黏性,使用其而製成PSA模式或PSVA模式之液晶顯示元件時,由對應於高Δn之窄隙與液晶組成物之低黏度可實現高速反應,此外,有抑制或完全不發生顯示不均的優異特徴。
此外,以一般之向列型液晶、層列型液晶而言,含有具有烯基之液晶化合物者在液晶組成物之黏度降低方面為有效,在高速反應為有用,但引起VHR之降低,並會誘發顯示不良,故有必要分成重視反應速度者或重視可靠性者來使用。尤其欲抑制顯示不良時,減少或不含有具有烯基之液晶化合物的含量係為重要。以其含量而言,較佳為小於10%,更佳為小於5%,特佳為不
含有。此處所謂不含有係意指不積極地添加,意指不包含製造時之不純物等不可避免地含有者,較佳為0.5%以下,較佳為0.1%以下,較佳為偵測極限(在以氣相層析進行之測定係10ppm左右)以下。
此外,雖已揭示有含有具有氯基之液晶化合物的液晶組成物,但顯著地損害可靠性,引起顯示不良。因此,減少或不含有具有氯基之液晶化合物的含量係為重要。以其含量而言,較佳為小於10%,更佳為小於5%,特佳為不含有。此處所謂不含有係意指不積極地添加,意指不包含製造時之不純物等不可避免地含有者,較佳為0.5%以下,較佳為0.1%以下,較佳為偵測極限(在以氣相層析進行之測定係10ppm左右)以下。
使用本發明之液晶組成物的液晶顯示元件係在使高速反應與顯示不良之抑制並存為有用者,尤其,在主動矩陣驅動用液晶顯示元件為有用,可適用在VA模式、PSVA模式、PSA模式、IPS模式或ECB模式用。
下文中舉實施例進一步詳述本發明,但本發明係並非受該等實施例限制者。此外,以下實施例及比較例之組成物中之「%」係意指『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:在25℃下之折射率各向異性
Δε:在25℃下之介電各向異性
η:在20℃下之黏度(mPa.s)
下文中顯示所調製之液晶組成物與其物性值。
示於實施例1之向列型液晶組成物的物性值係Tni:75.5℃、Δn:0.108、Δε:-3.0、η:16.3mPa.s。此外,測定使用本液晶組成物的液晶顯示元件之反應速度後,為9.3msec。再者,測定電壓保持率(VHR),確認具有高的VHR。另外,胞厚係3.5um,配向膜係JALS2096
,反應速度之測定條件係:Von係5.5V、Voff係1.0V、測定溫度係20℃、且使用AUTRONIC-MELCHERS公司之DMS 301。VHR之測定條件係電壓5V、頻率60Hz、溫度60℃、且使用東陽technica股份有限公司之VHR-1。
此外,即使改變液晶胞注入之條件(壓力及ODF法)亦無法在物性值看到變化。
下文中顯示所調製之液晶組成物與其物性值。
示於比較例1之向列型液晶組成物的物性值係Tni:74.7℃、Δn:0.109、Δε:-3.0、η:17.3mPa.s。如同記載於參考文獻6之實施例2而含有2%由式(I)表示
之化合物時,黏度較實施例1為高。從而,可明白本發明之申請專利範圍含有5至20%式(I)者,係在要得到本發明之效果為非常之重要。此外,測定使用本液晶組成物之液晶顯示元件的反應速度後,為10.5msec。
在比較例1係顯示含有2%由式(I)表示之化合物的液晶顯示組成物之例,調製不使用該由式(I)表示之化合物,使側鏈碳原子數多的式(III-F)之R5為戊基、R6為甲基之化合物的含量從13%增加至15%之液晶組成物。顯示其物性值。
示於比較例2之向列型液晶組成物係不含本發明之式(I),其物性值係Tni:75.0℃、Δn:0.109、Δε:-3.0、η:17.6mPa.s。將含有2%由式(I)表示之化合物的比較例1及不含由式(I)表示之化合物的比較例2之物性
值與實施例1比較,則Tni、Δn及Δε係成為近乎同等之值,但η係在比較例1上升6%、在比較例2上升7%。
藉此明白如本發明一般藉由使由式(I)表示之化合物的含量増加,含有Δε為負之化合物的液晶組成物係可不使Δn與Tni降低、改善η。
下文中顯示所調製之液晶組成物與其物性值。
示於實施例2之向列型液晶組成物的物性值
係Tni:71.2℃、Δn:0.115、Δε:-2.7、η:15.5mPa.s。
下文中顯示所調製之液晶組成物與其物性值。
示於實施例3之向列型液晶組成物的物性值係Tni:75.3℃、Δn:0.095、Δε:-3.2、η:15.3mPa.s。
藉由對99.7%示於實施例1之向列型液晶組成物添加0.3%由式(IV-a)
表示之聚合性化合物並均勻溶解而調製聚合性液晶組成物CLC-1。CLC-1之物性係與示於實施例1之向列型液晶組成物之物性幾乎沒有不同。以真空注入法將CLC-1注入胞隙3.5μm且塗布了誘發垂面排列之聚醯亞胺配向膜的附ITO晶胞。測定該晶胞之預傾角(晶體旋轉法)後,一邊以頻率1kHz施加1.8V之矩形波,一邊經由濾除320nm以下之紫外線的過濾器,以高壓汞燈對液晶胞照射紫外線。調整使晶胞表面之照射強度成為10mW/cm2而照射600秒鐘,得到使聚合性液晶組成物中之聚合性化合物聚合的垂直配向性液晶顯示元件。可確認聚合性化合物藉由聚合,產生對液晶化合物之配向控制力。此外,確認垂直配向性液晶顯示元件係具有優異之光學特性及高速反應性。
藉由對示於實施例1之向列型液晶組成物99.7%添加由式(IV-b)
表示之聚合性化合物0.3%並均勻溶解而調製聚合性液晶組成物CLC-2。CLC-2之物性係與示於實施例1之向列型液晶組成物之物性幾乎沒有不同。以真空注入法將CLC-2注入胞隙3.5μm且塗布了誘發垂面排列之聚醯亞
胺配向膜的附ITO晶胞。測定該晶胞之預傾角(晶體旋轉法)後,一邊以頻率1kHz施加1.8V之矩形波,一邊經由濾除320nm以下之紫外線的過濾器,以高壓汞燈對液晶胞照射紫外線。調整使晶胞表面之照射強度成為10mW/cm2而照射600秒鐘,得到使聚合性液晶組成物中之聚合性化合物聚合的垂直配向性液晶顯示元件。可確認聚合性化合物藉由聚合,產生對液晶化合物之配向控制力。此外,確認垂直配向性液晶顯示元件係具有優異之光學特性及高速反應性。
藉由對示於實施例1之向列型液晶組成物99.7%添加由式(IV-c)
表示之聚合性化合物0.3%並均勻溶解而調製聚合性液晶組成物CLC-3。CLC-3之物性係與示於實施例1之向列型液晶組成物之物性幾乎沒有不同。以真空注入法將CLC-3注入胞隙3.5μm且塗布誘發垂面排列之聚醯亞胺配向膜的附ITO晶胞。測定該晶胞之預傾角(晶體旋轉法)後,一邊以頻率1kHz施加1.8V之矩形波,一邊經由濾除320nm以下之紫外線的過濾器,以高壓汞燈對液晶胞照射紫外線。調整使晶胞表面之照射強度成為10mW/cm2而照射600秒鐘,得到使聚合性液晶組成物中之聚合性化合物聚合的垂直配向性液晶顯示元件。可確認聚合性化
合物藉由聚合,產生對液晶化合物之配向控制力。此外,確認垂直配向性液晶顯示元件係具有優異之光學特性及高速反應性。
Claims (14)
- 一種液晶組成物,其特徵為,含有由式(I)表示之化合物作為第一成分,其含量為5至25%,
- 如申請專利範圍第1項之液晶組成物,其中在25℃下之△ε為-2.0至-6.0之範圍,在25℃下之折射率各向異性(△n)為0.08至0.13之範圍,在20℃下之黏度(η)為 10至30mPa.s之範圍,向列相-等向性液體相轉移溫度(Tni)為60至120℃之範圍。
- 如申請專利範圍第1或2項之液晶組成物,其中含有選自由一般式(II-1)及(II-2)表示之化合物群之1種或2種以上的化合物作為第二成分,
- 如申請專利範圍第1或2項之液晶組成物,其中第二成分之含量為10至90質量%。
- 如申請專利範圍第1或2項之液晶組成物,其中含有選自由一般式(II-1A)、(II-1B)及(II-2A)表示之化合物群之1種或2種以上的化合物作為第二成分,
- 如申請專利範圍第1或2項之液晶組成物,其中進一步含有1種或2種以上選自由一般式(III-A)至一般式(III-J)表示之化合物群之化合物作為第三成分,
- 如申請專利範圍第1或2項之液晶組成物,其中同時含有式(I)、一般式(II-1A)、(II-2A)及一般式(III-A),
- 如申請專利範圍第1或2項之液晶組成物,其中同時含有式(I)、一般式(II-1B)、(II-2A)及一般式(III-A),
- 如申請專利範圍第1或2項之液晶組成物,其中同時含有式(I)、一般式(II-1A)、(II-1B)、(II-2A)及一般式(III-A),
- 如申請專利範圍第3項之液晶組成物,其中具有氯原子之液晶化合物的含量小於10%。
- 如申請專利範圍第1或2項之液晶組成物,其中具有烯基之液晶化合物的含量小於10%。
- 一種液晶顯示元件,其使用如申請專利範圍第1至11項中任一項之液晶組成物。
- 一種主動矩陣驅動用液晶顯示元件,其使用如申請專利範圍第1至11項中任一項之液晶組成物。
- 一種液晶顯示元件,其用於VA模式、PSA模式、PSVA模式、IPS模式或ECB模式,其使用如申請專利範圍第1至11項中任一項之液晶組成物。
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KR101370952B1 (ko) | 2014-03-10 |
US20150034873A1 (en) | 2015-02-05 |
TWI541329B (zh) | 2016-07-11 |
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CN103459552B (zh) | 2015-02-25 |
EP3095833A3 (en) | 2016-12-07 |
KR20130116947A (ko) | 2013-10-24 |
CN103459552A (zh) | 2013-12-18 |
TW201629189A (zh) | 2016-08-16 |
EP2695929A1 (en) | 2014-02-12 |
TW201249967A (en) | 2012-12-16 |
US9879181B2 (en) | 2018-01-30 |
WO2012137810A1 (ja) | 2012-10-11 |
JPWO2012137810A1 (ja) | 2014-07-28 |
EP2695929B1 (en) | 2016-09-14 |
CN104498052A (zh) | 2015-04-08 |
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