JPS62269117A - Vertical orientation-treatment of liquid crystal display element - Google Patents

Vertical orientation-treatment of liquid crystal display element

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Publication number
JPS62269117A
JPS62269117A JP11199386A JP11199386A JPS62269117A JP S62269117 A JPS62269117 A JP S62269117A JP 11199386 A JP11199386 A JP 11199386A JP 11199386 A JP11199386 A JP 11199386A JP S62269117 A JPS62269117 A JP S62269117A
Authority
JP
Japan
Prior art keywords
substrates
dmoap
water
soln
liquid crystal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP11199386A
Other languages
Japanese (ja)
Inventor
Minoru Tanaka
実 田中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Stanley Electric Co Ltd
Original Assignee
Stanley Electric Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Stanley Electric Co Ltd filed Critical Stanley Electric Co Ltd
Priority to JP11199386A priority Critical patent/JPS62269117A/en
Publication of JPS62269117A publication Critical patent/JPS62269117A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To obtain good visibility, durability and arrangement stability by immersing substrates into a DMOAP (N,N-dimethyl-N-octadecyl-3-aminopropylmethoxyl chloride) soln. or bringing the same into contact with said liquid, then washing away the excess DMOAP with water and forming only the min. monomolecular - several molecular film necessary for vertical orientation. CONSTITUTION:The substrates formed with transparent electrodes 2 and insulating films 3 is immersed into an aq. soln. (more preferably an aq. soln. of pure water) of the DMOAP. The concn. of the DMOAP in this stage is adequately 0.1-10g/l and the liquid temp. as immersion conditions is a room temp. or higher temp. The immersion time of 10sec-30min is practicable. The above-mentioned immersion is preferably executed by stirring the aq. soln. by a pump, stirrer or the like to create water flow or vertically oscillating the transparent substrates 1 or applying ultrasonic waves to a container contg. the aq. soln. to finely oscillate the soln. The substrates are thereafter pulled up and are cleaned with the water to wash away the excess DMOAP sticking to the substrates. After the substrates are cleaned with an org. solvent having compatibility with water, the substrates are immersed in the heated vapor of the org. solvent and is dried by which the substrates are subjected to a heating treatment.

Description

【発明の詳細な説明】 (技術分野) 本発明は、液晶分子を基板面に対して垂直に配列させる
ための液晶表示素子の垂直配向処理方法に関するもので
ある。
DETAILED DESCRIPTION OF THE INVENTION (Technical Field) The present invention relates to a method for vertical alignment processing of a liquid crystal display element for aligning liquid crystal molecules perpendicularly to a substrate surface.

(従来技術) 垂直配向剤DMOAP(N、N−ツメチル−N−オクタ
デシル−3−アミノプロピルトリメトキシルクロライド
)を用いた垂直配向処理は、次のような手順で行ってい
る。
(Prior Art) Vertical alignment treatment using a vertical alignment agent DMOAP (N,N-tumethyl-N-octadecyl-3-aminopropyltrimethoxyl chloride) is performed in the following procedure.

(1)0表示のための透明電極を有する基板にSiO□
などの透明な絶縁膜を形成する。
(1) SiO□ on a substrate with transparent electrodes for 0 display
Form a transparent insulating film such as

(ii)、  (i)項の処理を行った基板をDMOA
Pの12/を水浴液に15分間浸漬する。
(ii), The substrate treated in (i) is DMOA
12/ of P is immersed in a water bath solution for 15 minutes.

(iii)、  次に、純水に15分間浸漬した後、引
上げて乾燥する。
(iii) Next, after immersing it in pure water for 15 minutes, it is pulled out and dried.

11V)、  120°Cで加分間加熱処理する。11V) and 120°C for addition.

しかし、このような垂直配向処理をポノタイゾのダスト
・ホスト型液晶表示素子に適用した場合、僅かであつ1
も往々にして部分的なムラを生じ、これが視認性を損ね
たり、表示コントラストのムラによる不快感を誘ったり
する。また、温度600C1湿気95%の雰囲気に長期
間放置した場合に垂直配向性が著しく劣悪になるなど、
耐久性に問題がある。
However, when such vertical alignment treatment is applied to Ponotaizo's dust-host type liquid crystal display element, it is only slightly
However, local unevenness often occurs, which impairs visibility and causes discomfort due to uneven display contrast. In addition, when left in an atmosphere with a temperature of 600C and humidity of 95% for a long period of time, vertical alignment becomes extremely poor, etc.
There is a problem with durability.

(発明の目的) 本発明の目的は、良好な視認性、耐久性及び配列安定性
が期待でき、しかも短時間での処理が可能な液晶表示素
子の垂直配向処理方法を提供することにある。
(Object of the Invention) An object of the present invention is to provide a method for vertical alignment of a liquid crystal display element, which can be expected to have good visibility, durability, and alignment stability, and which can be processed in a short time.

(発明の概要) 本発明は、表示のための透明電極を形成し、更に少なく
ともこの透明電極を含む表示領域を透明な絶縁膜で被覆
した透明基板をDMOAPの0.1f/l〜10 f 
/ を水溶液に攪拌、振動あるいは超音波を加えながら
浸漬あるいは接触させた後、水洗し、次いでアルコール
類、ケトン類など、水と相溶性を有する有機溶剤で洗浄
し、この後、アルコール類、ケトン類あるいはハロダン
化炭化水素などの有機溶剤の加熱蒸気に浸漬して乾燥さ
せ、更に加熱処理して垂直配向膜を形成することを特徴
とするものである。
(Summary of the Invention) The present invention provides a transparent substrate having a transparent electrode for display and further covering at least a display area including the transparent electrode with a transparent insulating film.
/ is immersed in or brought into contact with an aqueous solution while stirring, applying vibration or ultrasonic waves, then washed with water, and then washed with an organic solvent that is compatible with water, such as alcohols or ketones. The film is characterized by being immersed in heated vapor of an organic solvent such as a hydrocarbon or a halodanide hydrocarbon, dried, and further heat-treated to form a vertical alignment film.

(実施例) 本発明の垂直配向処理方法は、DMOAPなる化学物質
を用いて垂直配向膜を形成する方法であり、第1図に示
すような構造の液晶表示素子に適用する。
(Example) The vertical alignment processing method of the present invention is a method of forming a vertical alignment film using a chemical substance called DMOAP, and is applied to a liquid crystal display element having a structure as shown in FIG.

第1図において、1はガラス板、プラスチックフィルム
などを用いた透明基板で、そのセル内面となる面に表示
のための透明電極2を酸化インジウムあるいは酸化スズ
などによって形成し、更に少なくともこの透明電極2を
含む表示領域にシリコン、チタンなどの酸化物あるいは
アクリル樹脂、工2キシ樹脂などの合成樹脂で透明な絶
縁膜3を形成する。この絶縁膜3の膜厚は100〜20
00 ’、が適当である。
In FIG. 1, reference numeral 1 denotes a transparent substrate made of a glass plate, a plastic film, etc., on which a transparent electrode 2 for display is formed of indium oxide or tin oxide on the surface that becomes the inner surface of the cell, and furthermore, at least this transparent electrode 2 is formed of indium oxide or tin oxide. A transparent insulating film 3 is formed on the display area including the display area 2 using an oxide such as silicon or titanium, or a synthetic resin such as acrylic resin or acryl resin. The thickness of this insulating film 3 is 100 to 20
00' is appropriate.

次に、透明電極2、絶縁膜3を形成した基板1をDMO
APの水溶液(好ましくは純水の水溶液)に浸漬する。
Next, the substrate 1 with the transparent electrode 2 and the insulating film 3 formed thereon is DMO
Immerse in an aqueous solution of AP (preferably an aqueous solution of pure water).

この時のDMOAPの濃度はo、ir/z〜lOf/l
が適当である。また、浸漬条件としては、液温は室温あ
るいはそれ以上の温度とし、浸漬時間はlO秒〜蜀分が
実用的である。この浸漬の際、水溶液をポンプ、攪拌機
などで攪拌して水流を作るとか、透明基板1を上下に振
動させるとか、あるいは水浴液の入った容器に超音波を
加えて微振動させることが好ましい。
The concentration of DMOAP at this time is o, ir/z ~ lOf/l
is appropriate. Further, as for the dipping conditions, it is practical that the liquid temperature is room temperature or higher, and the dipping time is 10 seconds to 10 minutes. During this immersion, it is preferable to stir the aqueous solution with a pump, stirrer, etc. to create a water flow, to vibrate the transparent substrate 1 up and down, or to apply ultrasonic waves to the container containing the water bath liquid to cause slight vibrations.

この後、基板1を引上げ、水で洗浄して基板lに付着し
ている余分なりMOAPを洗い流す。この洗浄水は純水
が好ましい。また、洗い流しの条件は、温度については
制約がなく、時間は1秒〜x秒程度とする。
After this, the substrate 1 is pulled up and washed with water to wash away any excess MOAP adhering to the substrate 1. This washing water is preferably pure water. Furthermore, the washing conditions are not limited to the temperature, and the time is about 1 second to x seconds.

次に、メチルアルコール、エチルアルコール、イソプロ
ピルアルコールなどのアルコール類、アセトン、メチル
エチルケトンなどのケトン類など、水と相溶性のある有
機溶剤で洗浄する。この時の温度は室温でも、加温され
ていてもよ(、洗浄時間は1秒〜10分でよい。また、
この溶剤による洗浄は、2段あるいはそれ以上の回数と
してもよい。
Next, it is washed with an organic solvent that is compatible with water, such as alcohols such as methyl alcohol, ethyl alcohol, and isopropyl alcohol, and ketones such as acetone and methyl ethyl ketone. The temperature at this time may be room temperature or heated (the cleaning time may be 1 second to 10 minutes.
This cleaning with the solvent may be performed in two stages or more times.

その場合、例えば2段洗浄であれば、第1段がイソプロ
ピルアルコールによる室温で5分の洗浄とし、第2段が
イソプロピルアルコール(第1段とは別なもの)による
室温で10秒の洗浄とする。
In that case, for example, if there is a two-stage cleaning, the first stage is cleaning with isopropyl alcohol for 5 minutes at room temperature, and the second stage is cleaning with isopropyl alcohol (different from the first stage) at room temperature for 10 seconds. do.

この後、メチルアルコール、エチルアルコール、イソプ
ロピルアルコールなどのアルコール類、アセトン、メチ
ルエチルケト/などのケトン類あるいはトリクロロエチ
レン(トリクレン)、トリクロルトリフルオルエタンな
どのハロゲン化炭化水素類などの有機溶剤の加熱蒸気に
浸漬して乾燥させる。この時の温度は、好ましくはこれ
ら有機溶剤の煮沸温度、例えばイソプロピルアルコール
であれば沸点82.4°f:!、)りクロルトリフルオ
ルエタンは47.7°Cである。時間は1分〜5分で十
分である。
After this, it is immersed in the heated vapor of an organic solvent such as alcohols such as methyl alcohol, ethyl alcohol, and isopropyl alcohol, ketones such as acetone, methyl ethyl keto/etc., or halogenated hydrocarbons such as trichloroethylene (triclene) and trichlorotrifluoroethane. and dry. The temperature at this time is preferably the boiling temperature of these organic solvents, for example, isopropyl alcohol has a boiling point of 82.4°F:! , ) dichlorotrifluoroethane is 47.7°C. A time of 1 to 5 minutes is sufficient.

次いで、加熱処理する。この条件は、80″C〜200
°Cでio分〜表示領域に化学蒸着法(CVD)、によ
り酸化シリコンの絶縁膜(膜厚2000 A )を形成
シタ後、DMOAP ()−v シリコーンの5RX−
679シラン、DMOAP5Q%メチルセロソロブ溶液
)の1 g/l水溶液(純水と混合)に超音波を加えな
がら10分間浸漬した。この後、取出して純水が常時流
入、流出している容器で1秒間すすぎ洗いし、次いでイ
ソプロピルアルコール中に5分間浸漬し、更に2番目の
イソプロピルアルコールに10秒間イ子漬し、最後にト
リクロルトリフルオルエタンの加熱煮沸した蒸気に5分
間曝露した。そして、1100Cで1時間加熱処理した
。これで、垂直配向膜の形成が完了する。
Next, heat treatment is performed. This condition is 80″C~200
After forming an insulating film of silicon oxide (film thickness 2000 A) on the display area by chemical vapor deposition (CVD) for ~io minutes at °C, DMOAP()-v of silicone 5RX-
The sample was immersed in a 1 g/l aqueous solution (mixed with pure water) of 679 silane and DMOAP (5Q% methyl cellosolub solution) for 10 minutes while applying ultrasound. After this, it was taken out and rinsed for 1 second in a container with pure water constantly flowing in and out, then immersed in isopropyl alcohol for 5 minutes, further immersed in a second isopropyl alcohol for 10 seconds, and finally rinsed with trichloroalcohol. Exposure to heated boiling vapor of trifluoroethane for 5 minutes. Then, heat treatment was performed at 1100C for 1 hour. This completes the formation of the vertical alignment film.

このようにして垂直配向膜を形成した2枚の基板を周辺
部にシール材を介在させて重ね合わせ、シール材を硬化
させてセル(容器)とし、このセル内に青色の二色性色
素を含む誘電異方性が負のネマチック液晶を充填して液
晶表示素子を作製した。1時間とする。この加熱処理で
基板lに垂直配向膜4が形成される。この垂直配向膜4
は、液晶表示素子としての端子、コネクタ一部あるいは
シール部に被覆されていても、それらの目的には何等影
響を与えない単分子〜数分子の膜厚で形成される。
The two substrates on which vertical alignment films have been formed in this way are stacked with a sealant interposed around the periphery, the sealant is cured to form a cell (container), and a blue dichroic dye is placed inside this cell. A liquid crystal display element was fabricated by filling a nematic liquid crystal with negative dielectric anisotropy. It will be 1 hour. Through this heat treatment, a vertical alignment film 4 is formed on the substrate l. This vertical alignment film 4
Even if it is coated on a terminal as a liquid crystal display element, a part of a connector, or a sealing part, it is formed with a film thickness of a single molecule to a few molecules, which does not affect the purpose in any way.

5は透明基板で、前記基板1と同様にその一面に透明電
極6、絶縁7、垂直配向膜8が形成される。
5 is a transparent substrate, and like the substrate 1, a transparent electrode 6, an insulator 7, and a vertical alignment film 8 are formed on one surface thereof.

両基板1.5をスペーサなどを用いて一定間隔に保持し
、周辺部をエポキシ接着剤、紫外線硬化接着剤などのシ
ール材9でシールしてセル(容器)とし、このセル内に
液晶10を充填して液晶表示素子としている。
Both substrates 1.5 are held at a constant distance using a spacer or the like, and the peripheral portions are sealed with a sealing material 9 such as epoxy adhesive or ultraviolet curing adhesive to form a cell (container), and a liquid crystal 10 is placed in this cell. It is filled to form a liquid crystal display element.

なお、上記実施例では浸漬によってDMOAPを付着さ
せたが、DMOAP水溶液をシャワー、水膜、噴流ど゛
して基板に接触させてもよい。この時の接触条件は上述
の浸漬条件と同様である。
In the above embodiment, DMOAP was attached by dipping, but the DMOAP aqueous solution may be brought into contact with the substrate by showering, water film, jetting, etc. The contact conditions at this time are similar to the above-mentioned immersion conditions.

次に、具体例を示す。Next, a specific example will be shown.

具体例I。Specific example I.

ガラス基板に酸化スズで表示のための透明電極を形成し
、この液晶表示素子を偏光顕微鏡などで観察したところ
、全面均一な垂直配向であった。
A transparent electrode for display was formed using tin oxide on a glass substrate, and when this liquid crystal display element was observed using a polarizing microscope, it was found that the entire surface was uniformly vertically aligned.

また、素子に交流電圧5vを印加したところ、ポノタイ
グのムラのない青色表示となった。更に、素子を温度6
0°C1湿度95%の雰囲気に1000時間放置した後
、観察した結果、垂直配向性は全く正常であり、5vの
電圧印加でコントラスト及び応答性に大きな変化は見ら
れなかった。消費電流は約2倍に増加しただけであった
Furthermore, when an AC voltage of 5 V was applied to the element, a blue display with no unevenness was obtained. Furthermore, the element was heated to a temperature of 6
After being left in an atmosphere of 0° C. and 95% humidity for 1000 hours, observation revealed that the vertical alignment was completely normal, and no significant change in contrast or responsiveness was observed upon application of a voltage of 5 V. The current consumption only increased by about twice.

(発明の効果) (1)、D M OA P液に基板を浸漬あるいは接触
させた後、余分なりMOAPを水で洗い流して垂直配向
に必要な最低限の単分子〜数分子膜のみ形成するので、
DMOAPが液晶に悪影響を及ぼすおそれがなくなると
ともに、悪条件の雰囲気でも高い耐久性を有する。
(Effects of the invention) (1) After the substrate is immersed in or brought into contact with the DMOAP solution, excess MOAP is washed away with water to form only the minimum monomolecular to several molecular film necessary for vertical alignment. ,
There is no fear that DMOAP will have an adverse effect on the liquid crystal, and it has high durability even in adverse atmosphere conditions.

(2)、D M OA P液に基板を浸漬あるいは接触
させる際に攪拌、振動、超音波などを加えることにより
、基板全面に均一に垂直配向膜を形成することができる
(2) By applying stirring, vibration, ultrasonic waves, etc. when the substrate is immersed or brought into contact with the D M OA P solution, a vertical alignment film can be uniformly formed over the entire surface of the substrate.

(3)、  D M OA Pは基板に容易に分子膜を
形成するので、その処理は浸漬でも、接触でも短時間で
行うことができ、作業性にすぐれている。
(3) Since DMOAP easily forms a molecular film on the substrate, the treatment can be carried out in a short time by immersion or contact, and has excellent workability.

(4ル DMOAPの垂直配向膜は分子膜の程度の厚さ
であるので、基板の外面に膜付けがあっても外観的に人
間の目で見えることはなく、また端子部、シール部など
に膜付けがあっても、電気的特性、接着力に何等影響を
与えない。
(4) The vertical alignment film of DMOAP is as thick as a molecular film, so even if the film is attached to the outer surface of the substrate, it will not be visible to the human eye, and it will not be visible to the human eye. Even if a film is attached, the electrical properties and adhesive strength are not affected in any way.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明方法で垂直配向処理した液晶表示素子の
構造を示す断面図である。 1及び5・・・・・・透明基板、  2及び6・・・・
・・透明電極、3及び7・・・・・・絶縁膜、 4及び8・・・・・・DMOAPの垂直配向膜、9・・
・・・・シール材、10・・・・・・液晶。 特許出願人  スタンレー電気株式会社−一−−;、。 代 理  人   秋   元   輝   雄  で
”;−、−:二5 同      秋  元  不  二  ?′S七テ
FIG. 1 is a cross-sectional view showing the structure of a liquid crystal display element subjected to vertical alignment treatment by the method of the present invention. 1 and 5...transparent substrate, 2 and 6...
...Transparent electrode, 3 and 7...Insulating film, 4 and 8...DMOAP vertical alignment film, 9...
... Seal material, 10 ... Liquid crystal. Patent applicant: Stanley Electric Co., Ltd. Agent Teruo Akimoto;-,-:25 Same person Fuji Akimoto?'S7te

Claims (1)

【特許請求の範囲】[Claims] 表示のための透明電極を形成し、更に少なくともこの透
明電極を含む表示領域を透明な絶縁膜で被覆した透明基
板をDMOAPの0.1g/l〜10g/l水溶液に攪
拌、振動あるいは超音波を加えながら浸漬あるいは接触
させた後、水洗し、次いでアルコール類、ケトン類など
、水と相溶性を有する有機溶剤で洗浄し、この後、アル
コール類、ケトン類あるいはハロゲン化炭化水素などの
有機溶剤の加熱蒸気に浸漬して乾燥させ、更に加熱処理
して垂直配向膜を形成することを特徴とする液晶表示素
子の垂直配向処理方法。
A transparent substrate on which a transparent electrode for display is formed and at least a display area including the transparent electrode is coated with a transparent insulating film is stirred, vibrated, or subjected to ultrasonic waves in a 0.1 g/l to 10 g/l aqueous solution of DMOAP. After immersion or contact with water while adding water, washing with water, then washing with an organic solvent that is compatible with water, such as alcohols or ketones, and then washing with an organic solvent such as alcohols, ketones, or halogenated hydrocarbons. 1. A vertical alignment processing method for a liquid crystal display element, which comprises immersing it in heated steam, drying it, and further heat-treating it to form a vertical alignment film.
JP11199386A 1986-05-16 1986-05-16 Vertical orientation-treatment of liquid crystal display element Pending JPS62269117A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11199386A JPS62269117A (en) 1986-05-16 1986-05-16 Vertical orientation-treatment of liquid crystal display element

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11199386A JPS62269117A (en) 1986-05-16 1986-05-16 Vertical orientation-treatment of liquid crystal display element

Publications (1)

Publication Number Publication Date
JPS62269117A true JPS62269117A (en) 1987-11-21

Family

ID=14575256

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11199386A Pending JPS62269117A (en) 1986-05-16 1986-05-16 Vertical orientation-treatment of liquid crystal display element

Country Status (1)

Country Link
JP (1) JPS62269117A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03186817A (en) * 1989-12-18 1991-08-14 Canon Inc Production of liquid crystal element
EP0492417A2 (en) * 1990-12-21 1992-07-01 Matsushita Electric Industrial Co., Ltd. Method of manufacturing chemically adsorbed film
JP2005242282A (en) * 2003-11-21 2005-09-08 Dainippon Ink & Chem Inc Method for solving display defect of nematic liquid crystal display element

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JPS50145152A (en) * 1974-05-11 1975-11-21
JPS56138716A (en) * 1980-04-01 1981-10-29 Asahi Glass Co Ltd Liquid crystal element
JPS57105722A (en) * 1980-12-24 1982-07-01 Alps Electric Co Ltd Liquid crystal display element
JPS57114121A (en) * 1981-01-07 1982-07-15 Hitachi Ltd Formation of liquid crystal orienting film
JPS581129A (en) * 1981-06-26 1983-01-06 Alps Electric Co Ltd Two-layer type and guest-host type liquid crystal display element and its manufacture
JPS60136717A (en) * 1983-12-26 1985-07-20 Matsushita Electric Ind Co Ltd Liquid crystal orienting film for vertical orientation

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JPS50145152A (en) * 1974-05-11 1975-11-21
JPS56138716A (en) * 1980-04-01 1981-10-29 Asahi Glass Co Ltd Liquid crystal element
JPS57105722A (en) * 1980-12-24 1982-07-01 Alps Electric Co Ltd Liquid crystal display element
JPS57114121A (en) * 1981-01-07 1982-07-15 Hitachi Ltd Formation of liquid crystal orienting film
JPS581129A (en) * 1981-06-26 1983-01-06 Alps Electric Co Ltd Two-layer type and guest-host type liquid crystal display element and its manufacture
JPS60136717A (en) * 1983-12-26 1985-07-20 Matsushita Electric Ind Co Ltd Liquid crystal orienting film for vertical orientation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03186817A (en) * 1989-12-18 1991-08-14 Canon Inc Production of liquid crystal element
EP0492417A2 (en) * 1990-12-21 1992-07-01 Matsushita Electric Industrial Co., Ltd. Method of manufacturing chemically adsorbed film
JP2005242282A (en) * 2003-11-21 2005-09-08 Dainippon Ink & Chem Inc Method for solving display defect of nematic liquid crystal display element

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