JPS6159352B2 - - Google Patents
Info
- Publication number
- JPS6159352B2 JPS6159352B2 JP55162775A JP16277580A JPS6159352B2 JP S6159352 B2 JPS6159352 B2 JP S6159352B2 JP 55162775 A JP55162775 A JP 55162775A JP 16277580 A JP16277580 A JP 16277580A JP S6159352 B2 JPS6159352 B2 JP S6159352B2
- Authority
- JP
- Japan
- Prior art keywords
- organic
- film
- good
- insulating film
- paste
- 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.)
- Expired
Links
- -1 aluminum compound Chemical class 0.000 claims description 7
- 150000003377 silicon compounds Chemical class 0.000 claims description 7
- 150000003755 zirconium compounds Chemical class 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 7
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 2
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
- 210000002858 crystal cell Anatomy 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- FPFOSIXCIBGKOH-MTOQALJVSA-J (z)-4-oxopent-2-en-2-olate;zirconium(4+) Chemical compound [Zr+4].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O FPFOSIXCIBGKOH-MTOQALJVSA-J 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
- 241000726103 Atta Species 0.000 description 1
- 241000018344 Ehrlichia sp. 'CGE agent' Species 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229940007550 benzyl acetate Drugs 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Landscapes
- Liquid Crystal (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Paints Or Removers (AREA)
- Chemically Coating (AREA)
- Inorganic Insulating Materials (AREA)
Description
本発明は、液晶セル等の透明絶縁被膜に係り、
特に液晶セルの下部基板等よりのアルカリイオン
溶出防止膜、基板上に形成された電極層と、液晶
層とを分離する絶縁膜、TN型液晶表示装置等に
おける液晶配向膜、などとして用いられる透明絶
縁被膜及び透明絶縁被膜形成用ペーストに関す
る。
従来、この種の透明絶縁被膜は、SiO2を主成
分とした膜で、真空蒸着法、浸漬法などにより形
成していた。しかし、真空蒸着法は、生産性が悪
るく、設備も大型になりがちであつた。又、浸漬
法は、不必要な箇所にも被膜が形成され、パター
ンの微細化に対応できない欠点があつた。
これらの欠点を解消するため、スクリーン印刷
法により基板上等にペーストを所望形状に印刷
し、焼成して透明絶縁被膜を形成する方法が試み
られているが、形成された被膜は、もろく、ポー
ラスであることが多く、被膜自体の特性は、真空
蒸着法、浸漬法により形成された被膜より劣つて
いた。
本発明は、叙上の欠点を解消し、成膜性がよ
く、電気絶縁性も良く、透明度良好、被膜強度
大、液晶分子に対する配向性が良く、スクリーン
印刷により形成可能な透明絶縁被膜を提供する目
的でなされたものである。
本発明の第１の特徴は、透明絶縁被膜の成分と
して、酸素の直接結合した、有機アルミニウム化
合物と有機ジルコニウム化合物と有機シリコン化
合物とを焼成して得られるAl2O3とZrO2とSiO2と
を選択したことである。被膜組成物として、被膜
強度大で絶縁性良好な被膜をもたらすAl2O3と、
成膜性の良い被膜をもたらすZrO2とをSiO2に添
加することにより、優れた特性の透明絶縁被膜の
形成に成功した。第２の特徴は、透明絶縁被膜を
形成するためのペーストの成分として、酸素の直
接結合した、有機アルミニウム化合物と有機ジル
コニウム化合物と有機シリコン化合物との混合物
を使用したことである。透明絶縁被膜をスクリー
ン印刷法にて形成可能ならしめるには、アルミニ
ウム化合物、ジルコニウム化合物及びシリコン化
合物が、高沸点（180℃以上）有機溶媒に、安定
に溶解する必要があり、かつ、ペーストの焼成温
度450〜700℃で完全に酸化物となるものでなけれ
ばならず、トリスアセチルアセトナートアルミニ
ウム（Al（acac）3）等の有機アルミニウム化合
物、テトラアセチルアセトナートジルコニウム
（Zr（acac）4等の有機ジルコニウム化合物、及び
ビニルトリス（２−メトキシエトキシ）シラン
（Ｖ−5000）等の有機シリコン化合物が該当す
る。有機アルミニウム化合物と、有機ジルコニウ
ム化合物と、有機シリコン化合物との混合物を、
有機溶媒に溶解させ、さらに粘性剤を添加し、混
合して透明絶縁被膜形成用ペーストを作成する
が、有機溶媒としては、前記混合物に対して反応
性が乏しく、沸点が180〜350℃の性質があるもの
でなければならず、ベンジルアルコール、ジプロ
ピレングリコール等の高沸点アルコール類、ベン
ジルアセテート、カルビトールアセテート等の高
沸点エステル類、ブチルセロソルブ等の高沸点エ
ーテル類などの高沸点有機溶媒が適用できる。前
記有機溶媒は、二種以上を混合使用してよい。次
に、粘性剤としては、前記有機溶媒に対して溶解
能がよく、ペーストの焼成温度450〜700℃で完全
に熱分解するものでなければならないが、エチル
セルローズ、ニトロセルローズ等のセルローズ系
粘性剤が適用できる。
本発明ペーストを、スクリーン印刷により、絶
縁基板上に印刷、焼成して得られる絶縁被膜は、
成膜性よく、電気絶縁性大、透明度良く、被膜強
度大で、しかも液晶分子に対する配向性が良いも
のであつた。
以下実施例をもとに、本発明をさらに詳しく説
明する。
実施例
有機ジルコニウム化合物として、テトラアセチ
ルアセトナートジルコニウム（Zr（acac）4）、有
機アルミニウム化合物として、トリスアセチルア
セトナートアルミニウム（Al（acac）3）、さらに
有機シリコン化合物として、ビニルトリス（２−
メトキシエトキシ）シラン（Ｖ−5000）を用い、
これら有機金属化合物の混合比を変え、下記の組
成により、ペーストを作成した。
金属部（Zr（acac）4
＋Al（acac）3＋Ｖ−5000） 5wt％
溶媒部（ブチルセロソルブ） 83wt％
粘性剤（エチルセルローズ） 12wt％
又、金属部として、有機シリコン化合物Ｖ−
5000のみを用いてペーストを作成し、比較例とし
た。作成したペーストを、ステン250メツシユ、
レジスト厚10μｍのスクリーン版を用いて、ソー
ダガラス絶縁基板上に印刷し、150℃で15分間予
備乾燥し、500℃で30分間焼成し、被膜を形成し
た。
第１表は、これら被膜の特性比較結果である。
The present invention relates to a transparent insulating coating for liquid crystal cells, etc.
In particular, a transparent film used as a film to prevent alkali ion elution from the lower substrate of a liquid crystal cell, an insulating film that separates an electrode layer formed on a substrate from a liquid crystal layer, a liquid crystal alignment film in a TN type liquid crystal display device, etc. The present invention relates to a paste for forming an insulating film and a transparent insulating film. Conventionally, this type of transparent insulating film is a film mainly composed of SiO 2 and has been formed by vacuum evaporation, dipping, or the like. However, the vacuum deposition method has poor productivity and tends to require large equipment. In addition, the dipping method has the disadvantage that a film is formed in unnecessary locations and cannot correspond to finer patterns. In order to overcome these drawbacks, attempts have been made to print a paste into a desired shape onto a substrate using screen printing and bake it to form a transparent insulating film, but the formed film is brittle and porous. In many cases, the properties of the film itself were inferior to those formed by vacuum evaporation or immersion methods. The present invention eliminates the above-mentioned drawbacks, provides a transparent insulating film that has good film formability, good electrical insulation, good transparency, high film strength, good orientation for liquid crystal molecules, and can be formed by screen printing. It was done for the purpose of The first feature of the present invention is that Al 2 O 3 , ZrO 2 , and SiO 2 obtained by firing an organic aluminum compound, an organic zirconium compound, and an organic silicon compound to which oxygen is directly bonded are used as components of the transparent insulating film . This is the choice made. As a coating composition, Al 2 O 3 which provides a coating with high coating strength and good insulation properties,
By adding ZrO 2 to SiO 2 , which produces a film with good film formability, we succeeded in forming a transparent insulating film with excellent properties. The second feature is that a mixture of an organic aluminum compound, an organic zirconium compound, and an organic silicon compound to which oxygen is directly bonded is used as a component of the paste for forming the transparent insulating film. In order to be able to form a transparent insulating film using the screen printing method, the aluminum compound, zirconium compound, and silicon compound must be stably dissolved in a high boiling point (180°C or higher) organic solvent, and the paste must be baked. It must completely become an oxide at a temperature of 450 to 700°C, and organic aluminum compounds such as trisacetylacetonatoaluminum (Al(acac) 3 ), tetraacetylacetonate zirconium (Zr(acac) 4 etc.) This includes organic zirconium compounds and organic silicon compounds such as vinyltris(2-methoxyethoxy)silane (V-5000).A mixture of an organic aluminum compound, an organic zirconium compound, and an organic silicon compound,
A paste for forming a transparent insulating film is created by dissolving it in an organic solvent, adding a viscosity agent, and mixing it.As an organic solvent, it has poor reactivity with the mixture and has a boiling point of 180 to 350°C. High boiling point organic solvents such as high boiling point alcohols such as benzyl alcohol and dipropylene glycol, high boiling point esters such as benzyl acetate and carbitol acetate, and high boiling point ethers such as butyl cellosolve are applicable. can. The organic solvents may be used in combination of two or more. Next, the viscosity agent must be one that has good solubility in the organic solvent and completely thermally decomposes at the paste firing temperature of 450 to 700°C. agent can be applied. The insulating coating obtained by printing and baking the paste of the present invention on an insulating substrate by screen printing is as follows:
It had good film forming properties, high electrical insulation, good transparency, high film strength, and good orientation to liquid crystal molecules. The present invention will be explained in more detail below based on Examples. Examples Tetraacetylacetonatozirconium (Zr(acac) 4 ) is used as an organic zirconium compound, trisacetylacetonatoaluminum (Al(acac) 3 ) is used as an organic aluminum compound, and vinyltris (2-
Using methoxyethoxy)silane (V-5000),
Pastes were prepared with the following compositions by changing the mixing ratio of these organometallic compounds. Metal part (Zr (acac) 4
+Al (acac) 3 +V-5000) 5wt% Solvent part (butyl cellosolve) 83wt% Viscous agent (ethyl cellulose) 12wt% Also, as the metal part, organic silicon compound V-
A paste was prepared using only 5000 and used as a comparative example. Add the paste you created to 250 meters of stainless steel,
A screen plate with a resist thickness of 10 μm was used to print on a soda glass insulating substrate, pre-dried at 150° C. for 15 minutes, and baked at 500° C. for 30 minutes to form a film. Table 1 shows the results of comparing the characteristics of these films.
【表】
×：不良、○：良好、◎：極めて良好
第１表よりわかるように、本発明ペーストを用
いて得られる透明絶縁被膜は、密着強度大で、表
面抵抗が高く、透明度良好であつあた。又、印刷
性、成膜性の良好なペーストが得られた。[Table] ×: Poor, ○: Good, ◎: Very good As shown in Table 1, the transparent insulating film obtained using the paste of the present invention has high adhesion strength, high surface resistance, and good transparency. Atta. Moreover, a paste with good printability and film-forming properties was obtained.
Claims (1)
物と、有機アルミニウム化合物と、有機シリコン
化合物との混合物を焼成して得られる、ZrO2−
Al2O3−SiO2系酸化物を含有した透明絶縁被膜。1 ZrO 2 − obtained by firing a mixture of an organic zirconium compound, an organic aluminum compound, and an organic silicon compound to which oxygen is directly bonded.
A transparent insulating film containing Al 2 O 3 −SiO 2 oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55162775A JPS5785861A (en) | 1980-11-19 | 1980-11-19 | Transparent insulating film and paste for forming transparent insulating film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55162775A JPS5785861A (en) | 1980-11-19 | 1980-11-19 | Transparent insulating film and paste for forming transparent insulating film |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5004886A Division JPS6230225A (en) | 1986-03-06 | 1986-03-06 | Paste for forming transparent insulating film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5785861A JPS5785861A (en) | 1982-05-28 |
| JPS6159352B2 true JPS6159352B2 (en) | 1986-12-16 |
Family
ID=15760979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP55162775A Granted JPS5785861A (en) | 1980-11-19 | 1980-11-19 | Transparent insulating film and paste for forming transparent insulating film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5785861A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007033588A (en) * | 2005-07-25 | 2007-02-08 | Sony Corp | Liquid crystal display element and liquid crystal projector |
-
1980
- 1980-11-19 JP JP55162775A patent/JPS5785861A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5785861A (en) | 1982-05-28 |
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