JPH0118579B2 - - Google Patents
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- Publication number
- JPH0118579B2 JPH0118579B2 JP58108785A JP10878583A JPH0118579B2 JP H0118579 B2 JPH0118579 B2 JP H0118579B2 JP 58108785 A JP58108785 A JP 58108785A JP 10878583 A JP10878583 A JP 10878583A JP H0118579 B2 JPH0118579 B2 JP H0118579B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- etching
- resist
- insulating film
- insulating
- 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
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- Silicon Compounds (AREA)
- Weting (AREA)
Description
【発明の詳細な説明】
本発明は、任意の基板表面の所望部分に二酸化
ケイ素(SiO2)の絶縁膜を部分的に形成する方
法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for partially forming an insulating film of silicon dioxide (SiO 2 ) on a desired portion of an arbitrary substrate surface.
SiO2の絶縁膜は、例えば液晶表示パネル用の
透明電極用配向膜をはじめ、電流カツト用絶縁層
の用途などに広く適用されている。しかもこの絶
縁膜は、全面一様に施す形態もあるが、むしろ所
望部分にパターン状に形成することのほうが多
い。しかしながら、SiO2膜はその化学的性質が
極めて安定であり、パターン化の手法として従来
知られている方法としては、
フツ化水素酸による湿式エツチング
マスク蒸着法
リフトオフ法
等にすぎない。これらの従来法の欠点としては、
′ フツ化水素酸によりSiO2膜を除去すること
は可能であるが、フツ化水素酸は強烈な酸であ
り、これに耐えるレジスト膜として実用的なも
のが見い出しにくい。 SiO 2 insulating films are widely used, for example, as alignment films for transparent electrodes in liquid crystal display panels and as insulating layers for current cut. Moreover, although there is a form in which this insulating film is applied uniformly over the entire surface, it is more often formed in a pattern on a desired portion. However, the chemical properties of the SiO 2 film are extremely stable, and conventionally known methods for patterning include only wet etching with hydrofluoric acid, mask evaporation, and lift-off. The disadvantages of these conventional methods are that although it is possible to remove the SiO 2 film with hydrofluoric acid, hydrofluoric acid is a strong acid, and there are no practical resist films that can withstand this. Hard to find.
′ マスク蒸着法は、量産性に乏しくコスト高
を招くほか、SiO2膜として得られるパターン
の位置合わせ精度およびパターン自体の精確さ
を出しにくい。'The mask vapor deposition method is not suitable for mass production and leads to high costs, and it is difficult to achieve alignment accuracy of the pattern obtained as a SiO 2 film and accuracy of the pattern itself.
′ リフトオフ法は、その手法上、どうしても
SiO2膜の端部に乱れが生じやすく、また、リ
フトオフ材の残渣等で被着面が汚れており、こ
の汚れのためSiO2膜の被着面への密着性が劣
るという欠点がある。′ The lift-off method is unavoidable due to its method.
Disturbances tend to occur at the edges of the SiO 2 film, and the adhering surface is dirty with lift-off material residue, etc., and this dirt has the disadvantage of poor adhesion of the SiO 2 film to the adhering surface.
本発明は以上のような従来法に鑑み、パターン
化された二酸化ケイ素の絶縁膜を上記したような
欠点を生ずることなく形成する方法を提供するも
のである。 In view of the above-mentioned conventional methods, the present invention provides a method for forming a patterned silicon dioxide insulating film without causing the above-mentioned drawbacks.
すなわち、本発明は、二酸化ケイ素の絶縁膜を
部分的に形成すべき面の全面に、テトラアルコキ
シシランの単量体もしくはポリマーの塗膜を形成
する工程、続いて100〜140℃の仮焼成を行なつて
前記塗膜を硬膜とする工程、しかる後、該硬膜上
に耐アルカリ性のレジスト膜を所望部分に施し、
レジスト膜が施されていない硬膜をアルカリ液に
てエツチング除去する工程、しかる後450〜600℃
の本焼成を行なうことにより前記硬膜を二酸化ケ
イ素の被膜とする工程を具備することを特徴とす
る絶縁膜の形成方法である。 That is, the present invention involves a step of forming a coating film of a monomer or polymer of tetraalkoxysilane on the entire surface on which an insulating film of silicon dioxide is to be partially formed, followed by pre-baking at 100 to 140°C. a step of hardening the coating film, and then applying an alkali-resistant resist film to desired areas on the hardening film,
The process of etching away the dura film on which the resist film is not applied using an alkaline solution, and then heating at 450 to 600℃.
This method of forming an insulating film is characterized by comprising the step of converting the hard film into a silicon dioxide film by performing main firing.
本発明の方法の一例を示す図面の第1図から第
6図に基いて、以下詳細に説明する。この例では
ガラス等の透明基板の片面に透明導電膜を施した
透明電極に対して絶縁膜を施すものであるが、第
1図において、透明基板1の片面に透明導電膜2
を所望の形状に施された面の全面に、浸漬法、ロ
ールコート法、スプレー法等の手段により、テト
ラアルコキシシランの単量体もしくはポリマーの
溶液を塗布して塗膜3を形成する。テトラアルコ
キシシランは、
一般式:Si(OR)4
<Rはアルキル基>
で表わされる有機ケイ素化合物であり、これの単
量体もしくは縮合した低分子ポリマーの溶液、例
えばアルコール溶液を用いることにより、塗膜3
が形成される。この状態では塗膜3は言わば有機
質の軟質膜であり、後加工に適さないうえに、ア
ルカリ液に対するエツチング適性も良好ではな
い。そこで第2図に示すように、仮焼成を行な
い、塗膜3を硬膜4とする。温度100〜140℃、焼
成時間20〜60分程度の仮焼成を行なうことによ
り、前述のテトラアルコキシシランは、加水分解
等を生じ有機分が除去されSi、O、Hを構成元素
とするシロキサン化合物に変化すると考えられ
る。この仮焼成により、膜の硬膜化と、アルカリ
液に対するエツチング適性が得られるものであ
る。 A detailed explanation will be given below based on FIGS. 1 to 6 of the drawings showing an example of the method of the present invention. In this example, an insulating film is applied to a transparent electrode with a transparent conductive film formed on one side of a transparent substrate such as glass, but in FIG.
A solution of a tetraalkoxysilane monomer or polymer is applied to the entire surface of the surface that has been formed into a desired shape by a dipping method, a roll coating method, a spraying method, or the like to form a coating film 3. Tetraalkoxysilane is an organosilicon compound represented by the general formula: Si(OR) 4 <R is an alkyl group>, and by using a solution of its monomer or condensed low-molecular polymer, such as an alcohol solution, Paint film 3
is formed. In this state, the coating film 3 is, so to speak, a soft organic film, which is not suitable for post-processing, and also has poor etching suitability for alkaline solutions. Therefore, as shown in FIG. 2, temporary firing is performed to form the coating film 3 into a hardened film 4. By performing preliminary firing at a temperature of 100 to 140°C for a firing time of about 20 to 60 minutes, the above-mentioned tetraalkoxysilane undergoes hydrolysis, etc., and organic components are removed, resulting in a siloxane compound containing Si, O, and H as constituent elements. It is thought that this will change. This pre-calcination hardens the film and makes it suitable for etching with an alkaline solution.
次に、第3図に示すように、絶縁膜として残し
たい部分に耐アルカリ性のレジスト膜5をパター
ン状に形成する。形成手段としては、スクリーン
印刷法によりレジストインキを直刷りする手段
が、簡便である。レジストインキは、エツチング
終了後の剥離性を考慮して有機溶媒可溶型インキ
を用いると良い。レジスト膜5の形成手段として
は、上記のようなスクリーン印刷法のほかに、フ
オトレジストを用いる写真的手段により形成する
こともできる。但し、この手段は、パターン精度
が高いが、手間を要する。 Next, as shown in FIG. 3, an alkali-resistant resist film 5 is formed in a pattern on a portion desired to remain as an insulating film. As a forming means, direct printing of resist ink using a screen printing method is convenient. As the resist ink, it is preferable to use an organic solvent soluble ink in consideration of releasability after etching. In addition to the screen printing method described above, the resist film 5 can also be formed by a photographic method using a photoresist. However, although this method has high pattern accuracy, it requires time and effort.
続いて、アルカリ液による湿式エツチングを行
ない、レジスト膜5によつて覆われていない部分
の硬膜4を溶解除去する。エツチング液として
は、水酸化ナトリウムや水酸化カリウムの20〜30
重量%溶液を用い、液温40〜60℃、エツチング時
間は膜厚に応じて設定すれば良い。エツチングの
仕様は、浸漬法やスプレーエツチング法等、通常
の仕様を用いることができる。第4図は硬膜4に
対するエツチングが終了した時点を示している。 Subsequently, wet etching with an alkaline solution is performed to dissolve and remove portions of the dura mater 4 that are not covered by the resist film 5. As an etching solution, use sodium hydroxide or potassium hydroxide with a concentration of 20 to 30%.
A wt% solution may be used, the solution temperature may be 40 to 60°C, and the etching time may be set according to the film thickness. As for the etching specifications, normal specifications such as a dipping method or a spray etching method can be used. FIG. 4 shows the point at which the etching of the dura mater 4 has been completed.
次に、第5図に示すようにレジスト膜5を剥離
する。レジスト膜5がインキ膜の場合、インキ溶
剤にて溶解できるし、フオトレジスト膜にあつて
は所定の剥膜液を用いれば良い。 Next, as shown in FIG. 5, the resist film 5 is peeled off. If the resist film 5 is an ink film, it can be dissolved with an ink solvent, and if it is a photoresist film, a predetermined film stripping solution may be used.
以上のようにしてパターン化された硬膜4を
450〜600℃の本焼成を行なうことにより、ここで
始めて二酸化ケイ素の絶縁膜6となりうる。焼成
時間は20〜60分程度で充分であることが多い。 The dura mater 4 patterned as above is
By performing the main firing at 450 to 600°C, the insulating film 6 of silicon dioxide can be formed for the first time. A firing time of about 20 to 60 minutes is often sufficient.
以下に本発明の実施例を述べるが、これによつ
て本発明が限定されるものではないことはもちろ
んである。 Examples of the present invention will be described below, but it goes without saying that the present invention is not limited thereto.
実施例
ガラス基板上に酸化インジウム〜酸化錫からな
る透明導電膜を所望の形状に形成した透明電極板
を、テトラアルコキシシランポリマーのメタノー
ル溶液(日本曹達(株)製、商品名「NSi310」:SiO2
換算含量5.9重量%)に浸漬し、引き上げ速度15
cm/minで約1000Åの塗膜が得られた。次に120
℃、30分間の仮焼成を行ない、塗膜を硬膜化し、
エツチング適性をもたせた後、スクリーン印刷法
にて、耐アルカリ性インキ(太陽インキ(株)製、商
品名「ケミカルインキ150P」を所望部分に約10
ミクロン厚に印刷し、レジスト膜とした。続い
て、30重量%の苛性ソーダ水溶液(液温55℃)に
約3分間浸漬することで、レジスト膜によつて被
覆されていない硬膜をエツチング除去した。Example A transparent electrode plate on which a transparent conductive film made of indium oxide to tin oxide was formed in a desired shape on a glass substrate was coated with a methanol solution of tetraalkoxysilane polymer (manufactured by Nippon Soda Co., Ltd., product name "NSi310": SiO 2
(equivalent content 5.9% by weight) and pulling speed 15
A coating film of approximately 1000 Å was obtained at cm/min. then 120
℃ for 30 minutes to harden the coating film.
After making it suitable for etching, apply an alkali-resistant ink (manufactured by Taiyo Ink Co., Ltd., trade name "Chemical Ink 150P") to the desired area for about 10 minutes using a screen printing method.
It was printed to a micron thickness to form a resist film. Subsequently, the hard film not covered by the resist film was etched away by immersing it in a 30% by weight aqueous solution of caustic soda (liquid temperature: 55°C) for about 3 minutes.
水洗乾燥後、1,1,1−トリクロロエタンに
よりレジスト膜を溶解除去し、しかる後、500℃
30分間の本焼成を行ない、二酸化ケイ素の絶縁膜
が得られた。得られた絶縁膜は、パターン端部に
乱れがなく、透明電極板への密着性も良好で、透
明導電膜と絶縁層の間に異物が浸潤するような間
隙もなかつた。 After washing with water and drying, the resist film was dissolved and removed with 1,1,1-trichloroethane, and then heated to 500°C.
Main firing was performed for 30 minutes, and a silicon dioxide insulating film was obtained. The obtained insulating film had no disturbance at the pattern end, had good adhesion to the transparent electrode plate, and had no gap between the transparent conductive film and the insulating layer where foreign matter could infiltrate.
本発明の絶縁膜の形成方法は以上のようなもの
であり、本発明によれば、化学的性質が安定であ
るためエツチング法によるパターン化が困難とさ
れた二酸化ケイ素の被膜をエツチング技術にて作
成することに成功したものであり、得られた絶縁
膜は、位置合わせ精度が高く、リフトオフ法にて
作成した場合のように、パターン端部に乱れがな
く、しかもSiO2膜は清浄な面に形成されること
になるので密着性が良好となり、絶縁性能も一段
と信頼の高いものとなる。本発明の方法は、途中
に仮焼成と本焼成の二回の操作が介在するが、レ
ジスト膜を印刷法で印刷する手段を用いるなど、
量産性に適した方法であり、高い品質の絶縁層が
得られる実用的な形成方法である。 The method for forming an insulating film of the present invention is as described above.According to the present invention, a silicon dioxide film, which is difficult to pattern by etching because of its stable chemical properties, can be etched using etching technology. The resulting insulating film has high alignment accuracy, has no disturbances at the pattern edges unlike when created using the lift-off method, and the SiO 2 film has a clean surface. Since the film is formed on the substrate, the adhesion is good and the insulation performance is even more reliable. Although the method of the present invention involves two operations, pre-baking and final baking, there are several steps such as printing a resist film using a printing method.
This method is suitable for mass production, and is a practical method of forming a high-quality insulating layer.
第1図から第6図までは、本発明の絶縁膜の形
成方法の一実施例を工程順に示す説明断面図であ
る。
1……透明基板、2……透明導電膜、3……塗
膜、4……硬膜、5……レジスト膜、6……絶縁
膜。
FIG. 1 to FIG. 6 are explanatory cross-sectional views showing one embodiment of the insulating film forming method of the present invention in the order of steps. DESCRIPTION OF SYMBOLS 1...Transparent substrate, 2...Transparent conductive film, 3...Coating film, 4...During film, 5...Resist film, 6...Insulating film.
Claims (1)
トラアルコキシシランの単量体もしくはポリマー
の塗膜を形成し、100〜140℃の仮焼成を行なつて
前記塗膜を硬膜とし、しかる後、該硬膜上に耐ア
ルカリ性のレジスト膜を所望部分に施し、レジス
ト膜が施されていない硬膜をアルカリ液にてエツ
チング除去し、しかるのち450〜600℃の本焼成を
行なうことにより前記硬膜を二酸化ケイ素の被膜
とすることを特徴とする絶縁膜の形成方法。1. A coating film of a monomer or polymer of tetraalkoxysilane is formed on the entire surface on which an insulating film is to be partially formed, and the coating film is hardened by pre-baking at 100 to 140°C, After that, an alkali-resistant resist film is applied to desired areas on the dura film, and the dura film on which the resist film is not applied is removed by etching with an alkaline solution, and then main firing is performed at 450 to 600°C. A method for forming an insulating film, characterized in that the dura film is a silicon dioxide film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10878583A JPS601711A (en) | 1983-06-17 | 1983-06-17 | Method of forming insulated film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10878583A JPS601711A (en) | 1983-06-17 | 1983-06-17 | Method of forming insulated film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS601711A JPS601711A (en) | 1985-01-07 |
| JPH0118579B2 true JPH0118579B2 (en) | 1989-04-06 |
Family
ID=14493415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10878583A Granted JPS601711A (en) | 1983-06-17 | 1983-06-17 | Method of forming insulated film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS601711A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2625453B2 (en) * | 1987-12-09 | 1997-07-02 | セントラル硝子 株式会社 | Pattern film formation method |
| JP2001302227A (en) * | 2000-04-26 | 2001-10-31 | Ube Nitto Kasei Co Ltd | Method for producing silica particles |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57191219A (en) * | 1981-05-20 | 1982-11-25 | Tokyo Denshi Kagaku Kabushiki | Formation of silica coating pattern |
-
1983
- 1983-06-17 JP JP10878583A patent/JPS601711A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS601711A (en) | 1985-01-07 |
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