JPS6184380A - Formation of conductive oxide tin film on base body - Google Patents
Formation of conductive oxide tin film on base bodyInfo
- Publication number
- JPS6184380A JPS6184380A JP20686884A JP20686884A JPS6184380A JP S6184380 A JPS6184380 A JP S6184380A JP 20686884 A JP20686884 A JP 20686884A JP 20686884 A JP20686884 A JP 20686884A JP S6184380 A JPS6184380 A JP S6184380A
- Authority
- JP
- Japan
- Prior art keywords
- base body
- group
- oxycarboxylate
- glass
- film
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明はガラス等の基体表面に導電性酸化錫膜を形成す
る方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for forming a conductive tin oxide film on the surface of a substrate such as glass.
従来の技術
400℃以上の高温でガラス等の表面に塩化第2錫、有
機錫塩化物などの錫塩化物やジブチル錫ジアセテート、
ジブチル錫オキサイドなどの有機錫化合物を酸化分解さ
せ、導電性の酸化錫膜を形成させることは公知である。Conventional technology Tin chloride such as stannic chloride, organic tin chloride, dibutyltin diacetate,
It is known to oxidatively decompose an organotin compound such as dibutyltin oxide to form a conductive tin oxide film.
発明が解決しようとする問題点
しかし錫塩化物を用いる方法では、塩素化合物のため膜
にくもりが発生し、まだ被膜と基体の間で高い電気抵抗
を示す。ジブチル錫ジアセテートを用いる方法では、造
膜速度が遅いため被膜が不均一となり透明性が損なわれ
、その被膜は高い電気抵抗を示す。ジブチル錫オキサイ
ドを用いる方法では、この化合物が如何なる溶剤にも不
溶のため、スプレー法やディピング法などの最も実用的
な造膜法に使用できない。上記有機錫化合物に各種フッ
化物をドーパントとして加え、被膜の電気抵抗をある程
度低下せしめる方法(特公昭53−25331号)も公
知であるが、この方法でも被膜の電気抵抗の低下は充分
で彦<、また造膜速度を改良できない。Problems to be Solved by the Invention However, in the method using tin chloride, cloudiness occurs in the film due to the chlorine compound, and high electrical resistance is still exhibited between the film and the substrate. In the method using dibutyltin diacetate, the film formation rate is slow, resulting in a non-uniform film, resulting in loss of transparency, and the film exhibits high electrical resistance. In the method using dibutyltin oxide, this compound is insoluble in any solvent, so it cannot be used in the most practical film forming methods such as spraying and dipping. There is also a known method (Japanese Patent Publication No. 53-25331) in which various fluorides are added as dopants to the above organic tin compound to reduce the electrical resistance of the coating to some extent, but even with this method, the electrical resistance of the coating is sufficiently reduced. , and the film formation rate cannot be improved.
本発明者等は種々の有機錫化合物を使用して導電性酸化
錫膜を形成させる研究を続けた結果、透明な被膜をすば
やく形成させ、かつ電気抵抗の小さい導電性酸化錫膜が
得られる化合物を見い出し本発明を完成した。As a result of continuing research on forming conductive tin oxide films using various organotin compounds, the present inventors have developed a compound that can quickly form a transparent film and provide a conductive tin oxide film with low electrical resistance. They discovered this and completed the present invention.
すなわち2本発明は、加熱したガラス等の基体表面に。In other words, the present invention applies to the surface of a substrate such as heated glass.
一般式
%式%
(式中Rはアルキル基又はアリール基f 、 R1は置
換又は非置換のアルキル基又はアリール基を、tnは○
又は1以上の整数をそれぞれ示す)で表わされるモノ有
機錫オキシカルボキシレート多量体の溶液を適用するこ
とを特徴とする基体に導電性酸化錫膜の形成方法である
。General formula % Formula % (In the formula, R is an alkyl group or an aryl group f, R1 is a substituted or unsubstituted alkyl group or an aryl group, tn is ○
A method for forming a conductive tin oxide film on a substrate, characterized by applying a solution of a monoorganotin oxycarboxylate polymer represented by (or an integer of 1 or more).
さらに2本発明は、加熱したガラス等の基体表面に、上
記一般式(II)で表わされるモノ有機錫オキシカルボ
キシレート多量体とドーパントの1種以上を含む溶液を
適用することを特徴とする基体に導電性酸化錫膜の形成
方法である。Furthermore, the present invention provides a substrate characterized in that a solution containing one or more of the monoorganic tin oxycarboxylate polymer represented by the above general formula (II) and a dopant is applied to the surface of a heated substrate such as glass. This is a method for forming a conductive tin oxide film.
本発明に使用するモノ有機錫オキシカルボキシレート多
量体は、上記一般式〔■〕において、 m−Qのときの
二量体1m−1の吉きの二量体、 m : 2のときの
四量体、−m−のごとき多量体として定義される化合物
を表わす。The monoorganotin oxycarboxylate polymer used in the present invention has the following general formula [■]: a positive dimer of 1 m-1 when m-Q, and a four-dimensional dimer when m: 2. mer, -m- represents a compound defined as a multimer.
一般式CI)において、Rはメチル基、エチル基。In general formula CI), R is a methyl group or an ethyl group.
プロピル基、ブチル基、アミル基、ヘキシル基。Propyl group, butyl group, amyl group, hexyl group.
オクチル基などのアルキル基を、R1はメチル基。An alkyl group such as an octyl group, and R1 is a methyl group.
エチル基、プロピル基、ブチル基、t−ブチル基1.1
−ジメチルプロピル基、ペンチル基、ヘキシル基、オク
チル基、ノニル基、デシル基、ウンデシル基、ドデシル
基、トリデシル基、ペンタデシル基、ヘプタデシル基な
どの置換又は非置換のアルキル基、フェニル基、トリル
基などのアリール基が挙げられる。Ethyl group, propyl group, butyl group, t-butyl group 1.1
- Substituted or unsubstituted alkyl groups such as dimethylpropyl group, pentyl group, hexyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, pentadecyl group, heptadecyl group, phenyl group, tolyl group, etc. The following aryl groups are mentioned.
もう一つの本発明に使用するドーパントとしては7例え
ばNH4F 、 HF 、 0F3COOH,05F7
000H。Another dopant used in the present invention is 7 such as NH4F, HF, 0F3COOH, 05F7
000H.
CF3CO2C2H5,CF2(COOC2H5)2.
cH2FcoNH2゜CBrFx + トリフルオロ無
水酢酸などのフッ素化合物、 5bce3.5b(oc
n3)3.5b(ococa3)3゜5b(oc4a9
)2y、 5b(003H,)2ce、5b(004H
9)3゜(C6H5)3Sbなどのアンチモン化合物が
挙げられる。CF3CO2C2H5, CF2(COOC2H5)2.
cH2FcoNH2゜CBrFx + Fluorine compounds such as trifluoroacetic anhydride, 5bce3.5b (oc
n3) 3.5b (ococa3) 3°5b (oc4a9
)2y, 5b(003H,)2ce, 5b(004H
9) Examples include antimony compounds such as 3°(C6H5)3Sb.
本発明において使用される溶媒は、上記一般式〇〕で表
わされるモノ有機錫オキシカルボキシレート多量体及び
ドーパントを溶解し、スプレーやデイビングしたとき揮
発しやすいもので1例えばメタノール、エタノール、イ
ソプロパツール、エチルセロソルブ、ブチルセロソルブ
などのアルコール類、メチルエチルケトン、アセトン、
メチルイソブチルケトンなどのケトン類、トルエン、キ
シレン、ソルベントナフサ、ヘキサン、ヘプタンなどの
炭化水素類、メチレンクロライド、 1.1.、1−ト
リフルオロエタン、トリフルオロトリクロロエタン、ト
リクロルエチレン、テトラクロロエチレンなどのハロゲ
ン化炭化水素類、酢酸エチル、酢酸プロピル、乳酸エチ
ルなどのエステル類、ジ−n−ブチルエーテル、ジエチ
レンクリコールジメチルエーテルなどのエーテル類が挙
げられる。The solvent used in the present invention is one that dissolves the monoorganotin oxycarboxylate polymer represented by the above general formula 〇〕 and the dopant, and easily evaporates when sprayed or dabbed, such as methanol, ethanol, isopropanol, etc. , alcohols such as ethyl cellosolve and butyl cellosolve, methyl ethyl ketone, acetone,
Ketones such as methyl isobutyl ketone, hydrocarbons such as toluene, xylene, solvent naphtha, hexane, heptane, methylene chloride, 1.1. , halogenated hydrocarbons such as 1-trifluoroethane, trifluorotrichloroethane, trichlorethylene, and tetrachloroethylene, esters such as ethyl acetate, propyl acetate, and ethyl lactate, and ethers such as di-n-butyl ether and diethylene glycol dimethyl ether. can be mentioned.
本発明は次のようにして実施される。The present invention is carried out as follows.
例えばガラスに対しては2表面を充分に脱脂洗浄し、ガ
ラスの軟化点以下400〜700cの温度に加熱保持し
た表面に2本発明の溶液をスプレー塗布し、そのまま加
熱炉(500〜60(lc)で熱分解を行ない、酸化錫
膜を形成させる。For example, for glass, the two surfaces are thoroughly degreased and cleaned, the solution of the present invention is spray applied to the surface heated and maintained at a temperature of 400 to 700 C below the softening point of the glass, and the solution is directly heated in a heating oven at 500 to 60 C (lc). ) to form a tin oxide film.
溶液中における本発明のモノ有機オキシヵルボ6一
キシレート多量体の含有量は、膜厚に応じて変えられる
が、10〜80重量係が適当である。The content of the monoorganic oxycarbo-6-xylate polymer of the present invention in the solution varies depending on the film thickness, but is suitably 10 to 80% by weight.
また本発明において酸化錫膜の導電性を高めるパ
ためドーーントと併用する場合は、膜の抵抗に応じて変
えられるが、ドーパントの使用量は本発明のモノ有機錫
オキシカルボキシレート多量体に対して10〜100重
量係が適当である。In addition, in the case of using a dopant to increase the conductivity of the tin oxide film in the present invention, the amount of the dopant to be used can be changed depending on the resistance of the film, but the amount of the dopant to be used is relative to the monoorganic tin oxycarboxylate polymer of the present invention. A weight ratio of 10 to 100 is appropriate.
作 用
本発明の方法によれば2分子中にSn −0−S nの
結合の存在が多く、酸化錫(S n O2)に近い構造
を示すため、高温での酸化錫の造膜が極めてすみやかに
行なわれ、均一透明な膜が形成される。Effect: According to the method of the present invention, there are many Sn-0-Sn bonds in two molecules, and the structure is similar to that of tin oxide (SnO2), so the formation of tin oxide films at high temperatures is extremely difficult. It is carried out quickly and a uniform transparent film is formed.
この現象はドーパントを併用した場合にも同様に認めら
れる。造膜が遅いと、膜がくもったり、不均一に結晶化
したりして、透明な均一膜が得られない。このような効
果は従来の有機錫化合物の使用では見い出すことはでき
ない。This phenomenon is similarly observed when a dopant is also used. If the film formation is slow, the film becomes cloudy or non-uniformly crystallized, making it impossible to obtain a transparent and uniform film. Such effects cannot be found with the use of conventional organotin compounds.
本発明によれは、ガラス、セラミックス、金属等の基体
表面に電気抵抗の低い導電性酸化錫を造膜させることが
できるので、自動車、飛行機等の窓やショーケースの防
曇ガラス、液晶セルの電極太陽電池用電極などに利用で
きる。According to the present invention, it is possible to form a film of conductive tin oxide with low electrical resistance on the surface of a substrate such as glass, ceramics, metal, etc., so it is possible to form a film of conductive tin oxide with low electrical resistance. It can be used for electrodes for solar cells, etc.
次に製造例と実施例を挙げて本発明を説明するが、製造
中の係は重量係を示す。Next, the present invention will be explained with reference to production examples and examples, where the term "during production" refers to weight.
製造例1
攪拌器2分液炉斗、温度計及び還流冷却器付き三
共沸脱水器を備えた11の中ツロフラスコにモノメチル
i酸166.7F(1モル)及びベンゼン200m1!
を仕込み、攪拌しながら、還流下に酢酸100り(1,
67モル)を30分間で滴下した。Production Example 1 166.7 F (1 mol) of monomethyl i acid and 200 ml of benzene were placed in an 11-sized medium-sized flask equipped with a stirrer, two-separating furnace, a thermometer, and a three-azeotropic dehydrator with a reflux condenser.
of acetic acid under reflux while stirring.
67 mol) was added dropwise over 30 minutes.
2時間還流脱水を続け、水を2371ne捕集した。Reflux dehydration was continued for 2 hours, and 2371ne of water was collected.
反応終了後溶液を濾過し、ろ液からベンゼンを留去して
・白色固体241り(収率99.3%)を得だ。このも
のを分析した結果。After the reaction was completed, the solution was filtered, and benzene was distilled off from the filtrate to obtain 241 white solids (yield: 99.3%). The result of analyzing this thing.
実測値 計算値
錫含量:487係 48.9係
酸 価 : 352 355赤外会
吸収スペクトル
以上からモノメチル錫オキシアセテート(三量体)であ
ることを確認した。Actual value Calculated value Tin content: 487 coefficient 48.9 coefficient Acid value: 352 It was confirmed from the 355 infrared absorption spectrum that it was monomethyl tin oxyacetate (trimer).
製造例2
製造例1と同じ反応容器に、モノ−n−ブチル錫酸20
8.8y(1モル)及びトルエン5oomeを仕込み、
攪拌しながら、還流下に酢酸9oy(1,5モル)を3
0分間で滴下した。2時間還流脱水を続け、水を22.
3mJ捕果した。反応終了後溶液を濾過し、炉液からト
ルエンを留去して、白色固体275y(99,5%)を
得だ。このものを分析した結果。Production Example 2 In the same reaction vessel as Production Example 1, 20% of mono-n-butylstannic acid was added.
Prepare 8.8y (1 mol) and 5oome of toluene,
While stirring, add 9 oy (1.5 mol) of acetic acid to 3 ml under reflux.
It was dropped in 0 minutes. Continue reflux dehydration for 2 hours, and remove water by 22.
3mJ was captured. After the reaction was completed, the solution was filtered and toluene was distilled off from the furnace solution to obtain white solid 275y (99.5%). The result of analyzing this thing.
実測値 計算値
錫 含 量 : 42.8 43.0
酸 価 : 303 305赤外吸収
スペクトル
以上からモノ−n−ブチル錫オキシアセテート(四量体
)であることを確認した。Actual value Calculated value Tin content: 42.8 43.0
Acid value: 303 305 It was confirmed from the infrared absorption spectrum that it was mono-n-butyltin oxyacetate (tetramer).
製造例3
製造例1と同じ反応容器に、モノ−n−モノオクチル錫
酸264.9y(1,0モル)及びベンゼン300tr
eを仕込み、攪拌しながら、還流下にオクチル酸288
.4f/(2モル)を30分間で滴下した。2時間還流
脱水を続け、水を26.8 ”g捕集した。反応終了後
溶液を濾過し、ろ液からベンゼンを留去して、白色固体
525.2y(99,8係)を得た。このものを分析し
た結果。Production Example 3 In the same reaction vessel as Production Example 1, 264.9y (1.0 mol) of mono-n-monooctylstannic acid and 300tr of benzene were added.
Add 288% of octylic acid under reflux while stirring.
.. 4f/(2 mol) was added dropwise over 30 minutes. Reflux dehydration was continued for 2 hours, and 26.8"g of water was collected. After the reaction was completed, the solution was filtered, and benzene was distilled off from the filtrate to obtain 525.2y of white solid (99.8 section). .The result of analyzing this thing.
実測値 計算値
錫 含 量 :22.3 係 226 %
酸 両 : 214 213赤
外吸収スペクトル
以上からモノーn−オクチル賜オキシオクトエート(二
量体)であることを確認した。Actual value Calculated value Tin content: 22.3% 226%
Acid: 214 213 From the infrared absorption spectrum, it was confirmed that it was mono n-octyl oxyoctoate (dimer).
製造例4〜7
製造例1と同じ反応容器に、下記第1表のモノ有機錫酸
と有機カルボン酸を各モル数反応させ。Production Examples 4 to 7 In the same reaction vessel as in Production Example 1, the monoorganic stannic acid and organic carboxylic acid shown in Table 1 below were reacted in respective moles.
製造例1と同様の反応操作と分析を行ない、モノ有機錫
オキシカルボキシレート多量体を得た。The same reaction operation and analysis as in Production Example 1 were carried out to obtain a monoorganotin oxycarboxylate polymer.
第 1 表
実施例1〜8及び比較例1〜3
ガラス板の表面を580°Cに加熱し2次いで下記箱2
−1表(実施例)及び第2−2表(比較例)の組成の溶
液を、空気圧25に7乙m2+ガラス板から40 cm
の距離で、3〜4秒間その表面にスプレー塗布し、酸化
錫膜を形成させた。得られた酸化錫膜について、被膜状
態を観察し、膜厚、可視光透過率及び電気抵抗値を測定
した。Table 1 Examples 1 to 8 and Comparative Examples 1 to 3 The surface of the glass plate was heated to 580°C, and then the following box 2 was heated.
A solution having the composition shown in Table 1 (Example) and Table 2-2 (Comparative Example) was heated to an air pressure of 25 m2 + 40 cm from a glass plate.
The tin oxide film was formed by spraying on the surface for 3-4 seconds at a distance of . The state of the obtained tin oxide film was observed, and the film thickness, visible light transmittance, and electrical resistance were measured.
結果を第2−1表及び第2−2表に示す。The results are shown in Tables 2-1 and 2-2.
Claims (2)
は非置換のアルキル基又はアリール基を、mは0又は1
以上の整数をそれぞれ示す)で表わされるモノ有機錫オ
キシカルボキシレート多量体の溶液を適用することを特
徴とする基体に導電性酸化錫膜の形成方法。(1) On the surface of a heated substrate such as glass, there is a general formula ▲ mathematical formula, chemical formula, table, etc. , m is 0 or 1
A method for forming a conductive tin oxide film on a substrate, the method comprising applying a solution of a monoorganotin oxycarboxylate polymer represented by the following integers.
は非置換のアルキル基又はアリール基を、mは0又は1
以上の整数をそれぞれ示す)で表わされるモノ有機錫オ
キシカルボキシレート多量体とドーパントの1種以上を
含む溶液を適用することを特徴とする基体に導電性酸化
錫膜の形成方法。(2) On the surface of a heated substrate such as glass, there is a general formula ▲ mathematical formula, chemical formula, table, etc. , m is 0 or 1
A method for forming a conductive tin oxide film on a substrate, the method comprising applying a solution containing one or more monoorganotin oxycarboxylate polymers represented by the above integers) and one or more dopants.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP20686884A JPS6184380A (en) | 1984-10-01 | 1984-10-01 | Formation of conductive oxide tin film on base body |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP20686884A JPS6184380A (en) | 1984-10-01 | 1984-10-01 | Formation of conductive oxide tin film on base body |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS6184380A true JPS6184380A (en) | 1986-04-28 |
Family
ID=16530365
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP20686884A Pending JPS6184380A (en) | 1984-10-01 | 1984-10-01 | Formation of conductive oxide tin film on base body |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6184380A (en) |
Citations (6)
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JPS4838319A (en) * | 1971-09-17 | 1973-06-06 | ||
JPS5456099A (en) * | 1977-10-13 | 1979-05-04 | Sumitomo Chem Co Ltd | Formation method for alumina or silica-alumina film |
JPS5515978A (en) * | 1978-07-24 | 1980-02-04 | Teijin Ltd | Production of titanium oxide film |
JPS56120543A (en) * | 1980-01-31 | 1981-09-21 | Bfg Glassgroup | Glass coating method and device |
JPS57161809A (en) * | 1981-03-31 | 1982-10-05 | Nippon Soda Co Ltd | Manufacture of multilayered film |
JPS58110427A (en) * | 1981-12-17 | 1983-07-01 | Matsumoto Seiyaku Kogyo Kk | Manufacture of transparent tin oxide film |
-
1984
- 1984-10-01 JP JP20686884A patent/JPS6184380A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4838319A (en) * | 1971-09-17 | 1973-06-06 | ||
JPS5456099A (en) * | 1977-10-13 | 1979-05-04 | Sumitomo Chem Co Ltd | Formation method for alumina or silica-alumina film |
JPS5515978A (en) * | 1978-07-24 | 1980-02-04 | Teijin Ltd | Production of titanium oxide film |
JPS56120543A (en) * | 1980-01-31 | 1981-09-21 | Bfg Glassgroup | Glass coating method and device |
JPS57161809A (en) * | 1981-03-31 | 1982-10-05 | Nippon Soda Co Ltd | Manufacture of multilayered film |
JPS58110427A (en) * | 1981-12-17 | 1983-07-01 | Matsumoto Seiyaku Kogyo Kk | Manufacture of transparent tin oxide film |
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