JPH0225990B2 - - Google Patents
Info
- Publication number
- JPH0225990B2 JPH0225990B2 JP57149997A JP14999782A JPH0225990B2 JP H0225990 B2 JPH0225990 B2 JP H0225990B2 JP 57149997 A JP57149997 A JP 57149997A JP 14999782 A JP14999782 A JP 14999782A JP H0225990 B2 JPH0225990 B2 JP H0225990B2
- Authority
- JP
- Japan
- Prior art keywords
- compound
- nco
- substrate
- silicon oxide
- bond
- 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 - Lifetime
Links
- 238000000034 method Methods 0.000 claims description 25
- 150000001875 compounds Chemical class 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- -1 silane isocyanate compound Chemical class 0.000 claims description 15
- 229910000077 silane Inorganic materials 0.000 claims description 14
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 14
- 239000012948 isocyanate Substances 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 125000005842 heteroatom Chemical group 0.000 claims description 3
- 150000002736 metal compounds Chemical class 0.000 claims description 3
- 229910052755 nonmetal Inorganic materials 0.000 claims description 2
- 229910018557 Si O Inorganic materials 0.000 claims 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 150000003377 silicon compounds Chemical class 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- YASAKCUCGLMORW-UHFFFAOYSA-N Rosiglitazone Chemical compound C=1C=CC=NC=1N(C)CCOC(C=C1)=CC=C1CC1SC(=O)NC1=O YASAKCUCGLMORW-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 238000007611 bar coating method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000005647 linker group Chemical group 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000013008 moisture curing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Chemical group 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
Description
本発明は珪素酸化物被覆形成法、特に常温付近
の低温で任意に有機基を増減出来る基体表面の珪
素酸化物被覆形成法である。
電子部品用絶縁膜、プラスチツクやガラスの表
面安定化、金属メツキ、薄膜表面の保護や積層
板、液晶セル面配向膜の表面処理等の目的で基板
上に高純度な珪素酸化物被覆を形成して使用する
事は広く知られている。
これらの被覆形成はSiO2のスパツタ、真空蒸
着やシランのCVD法或は基体が珪素の場合には
熱酸化法での処理が行われている。更に最近は取
扱いが簡単で大面積処理に適するものとしてゾ
ル／ゲル法として分類される溶液法が注目されて
来ている。この溶液法は他の方法の如く特別な処
理装置を用いる事なく安全に広表面の処理が出来
る利点があり、この為の処理剤としてはハロゲン
化シランやアルキルシリケートを加水分解するか
又はアルコール−酸水溶液を加えて成る珪素化合
物の結合基の一部又は全てが加水分解されたゾ
ル／ゲルを用いるものであり特公昭52−16488、
特公昭52−20825、特開昭55−34276、特開昭57−
74370、特開昭57−105463、特開昭57−100940〜
44にその諸例が開示されている。
しかしこれらのゾル／ゲル法の場合も被膜形成
は通常200〜600℃の高温で焼成処理しないと酸化
物膜が形成されないので作業の連続性に欠け適用
材質にも制限が生じる為室温又は連続処理が可能
な低温域で珪素酸化物被覆処理をする方法の開発
が要請されていた。そこで室温付近の低温で珪素
酸化物被覆を形成する方法について研究した結果
分子中にSi−NCO結合を含むシランイソシアネ
ートで基体を処理する方法が有効である事を認め
本発明に至つた。
かくて本発明は分子中にSi−NCO結合を有す
るシランイソシアネート化合物で各種材質の基体
表面を処理することからなる珪素酸化物被覆形成
法を提供するものである。
本発明では、かかるシランイソシアネート化合
物とこの化合物と反応してSi−Ｏ−Ｍ結合（Ｍは
金属又は非金属元素）を形成し得る多価金属化合
物又はヘテロ元素化合物を併用して基体表面を処
理することによつて珪素酸化物被覆を形成するこ
ともできる。本発明では主として前記シランイソ
シアネート化合物として分子中にSiに直結する
NCO基を少くとも２個含有する化合物が用いら
れる。
本発明について更に詳細に説明すれば、ここで
用いられるシランイソシアネート化合物としては
式Si（NCO）4、RoSi（NCO）4-o、（RO）oSi−
（NCO）4-o（式中Ｒは置換基を有するか又は有し
ない炭化水素基、ｎ＝１、２又は３）の化合物、
又はこれらの化合物の縮合物があげられる。又無
水珪酸やポリシロキサン化合物と上記式の化合物
と縮合したSiに直結したNCO基を２個以上含む
化合物も同様に本発明に用いることができる。こ
のような珪素化合物は単独でまたは２種以上混合
して用いることができる。上記式中Ｒはメチル、
エチル、ビニル、フエニルその他の置換されない
又は置換された飽和又は不飽和の脂肪族又は芳香
族の炭化水素基であり希望する物性などに応じて
このような有機基を任意に選択、増減してこれら
を導入した珪素酸化物被覆を形成することができ
る。又上記式中ｎ＝１〜３の化合物中主としてｎ
＝１〜２の化合物が本発明で用いられるが、ｎ＝
３の化合物の場合は基板表面をアルキルシリル化
処理する効果がある。
これらの珪素化合物でプラスチツク、ガラス、
金属その他の各種材質の基体表面を処理するに当
つては、いわゆる流延法、スピンナー法、スプレ
ー法、バーコート法、蒸着法、CVD法等多数の
方法が用いられる。これらの方法で基体表面を処
理して前記珪素化合物を塗布、噴霧などするとき
は、上記のように分子中にSi−NCO結合を有す
る化合物中のSiに直結したNCO基は、特別な触
媒を用いることなく空気中の水分や基体表面の水
分或はOH基等と容易に室温で反応してシロキサ
ン結合を形成するので、単にかかるシランイソシ
アネートを含む化合物で常態雰囲気下に基体表面
を処理するだけで硬化して容易に基体表面に珪素
酸化物被覆を形成することができるのである。
このシランイソシアネート化合物は必要により
他の化合物を併用することができる。たとえば
NCO基と反応する活性水素を有しない化合物を
溶剤として併用することができる。溶剤として用
いることのできる化合物としては例えばｎ−ヘキ
サン、ベンゼン、トルエン、キシレン、塩化メチ
レン、トリクロルエチレン（トリクレン）、フツ
化炭化水素（フレオン）、ジメチルホルムアミド
（DMF）、ジメチルスルホキシド（DMSO）、ニ
トロベンゼン、酢酸メチル、酢酸エチル、酢酸ブ
チル等を挙げることができる。
又処理に際して密着性やアルカリ移行防止やそ
の他の機能を与えるために、処理時にシランイソ
シアネート化合物中のSiと反応してSi−Ｏ−Ｍ結
合（Ｍは下記の如き金属又は非金属元素）を形成
しうる多価金属化合物又はヘテロ元素化合物を併
用することができる。この目的に使用することが
できる化合物としては上記ＭとしてMg、Ca、
Zn、Ｂ、Al、Sn、Ti、Zr、Sb、In、Ｖ、Ta、
As、Ｐ、Fe、Co、Ni、Cr等の金属又は非金属元
素を含む化合物があげられる。而してこれらの化
合物はアルコキシド、キレート、アシレート、水
酸化物等種々の化合物で使用できるが、非水系で
シランイソシアネート化合物又はこれと前記の如
き溶剤とからなる溶液に溶解できるものでなけれ
ばならない。
本発明の方法は上述のように常態室温の雰囲気
下で処理して良好な珪素酸化物被覆が形成される
が必要により加温して処理することもできること
勿論でありこれによるときは被覆の安定化を促進
することができて好ましい。
かくして本発明の方法によれば室温又はその付
近の低温で湿気硬化法により基体の珪素酸化物被
覆が形成できるが、又希望する物性に応じて有機
基を任意に導入した珪素酸化物被覆が形成できる
ので工業上有用である。
以下に本発明の実施例を示す。例中部は重量部
を示す。
実施例 １−６
硬質スライドガラスを洗剤及びアルコールで充
分に洗浄して試片とした。この試片を10cm／min
の速度の浸漬引上げ法で下記各例の化合物を処理
し65％RH25℃の雰囲気で硬化させ形成させた被
覆の物性を測定した。
The present invention is a method for forming a silicon oxide coating, particularly a method for forming a silicon oxide coating on the surface of a substrate, in which organic groups can be arbitrarily increased or decreased at low temperatures around room temperature. We form high-purity silicon oxide coatings on substrates for purposes such as insulating films for electronic components, surface stabilization of plastics and glass, metal plating, protection of thin film surfaces, laminates, and surface treatment of liquid crystal cell surface alignment films. Its use is widely known. These coatings are formed by SiO 2 sputtering, vacuum evaporation, silane CVD, or when the substrate is silicon, thermal oxidation. Furthermore, recently, a solution method classified as a sol/gel method has been attracting attention because it is easy to handle and suitable for large area processing. This solution method has the advantage of being able to safely treat a wide surface area without using special treatment equipment like other methods, and the treatment agent used for this purpose is hydrolysis of halogenated silanes and alkyl silicates, or alcohol- It uses a sol/gel in which some or all of the bonding groups of a silicon compound are hydrolyzed by adding an acid aqueous solution.
Special Publication No. 52-20825, No. 55-34276, No. 57-
74370, JP-A-57-105463, JP-A-57-100940~
Examples are disclosed in 44. However, even in the case of these sol/gel methods, the oxide film cannot be formed unless the film is formed by firing at a high temperature of 200 to 600°C, so the work is not continuous, and there are restrictions on the materials that can be used, so it is necessary to process at room temperature or continuously. There was a demand for the development of a method for coating silicon oxide at low temperatures. Therefore, as a result of research into a method of forming a silicon oxide coating at a low temperature near room temperature, it was found that a method of treating a substrate with silane isocyanate containing a Si-NCO bond in the molecule was effective, leading to the present invention. Thus, the present invention provides a method for forming a silicon oxide coating, which comprises treating the surface of a substrate made of various materials with a silane isocyanate compound having a Si--NCO bond in the molecule. In the present invention, the substrate surface is treated using a combination of such a silane isocyanate compound and a polyvalent metal compound or a hetero element compound that can react with this compound to form a Si-O-M bond (M is a metal or a non-metal element). A silicon oxide coating can also be formed by doing this. In the present invention, mainly the silane isocyanate compound is directly bonded to Si in the molecule.
Compounds containing at least two NCO groups are used. To explain the present invention in more detail, the silane isocyanate compounds used herein include formulas Si(NCO) 4 , RoSi (NCO) 4-o , (RO) oSi-
(NCO) 4-o (wherein R is a hydrocarbon group with or without a substituent, n = 1, 2 or 3),
Or condensates of these compounds can be mentioned. Further, a compound containing two or more NCO groups directly bonded to Si, which is condensed with a silicic anhydride or a polysiloxane compound and a compound of the above formula, can also be used in the present invention. Such silicon compounds can be used alone or in combination of two or more. In the above formula, R is methyl,
Ethyl, vinyl, phenyl, and other unsubstituted or substituted saturated or unsaturated aliphatic or aromatic hydrocarbon groups, and such organic groups can be arbitrarily selected and increased or decreased depending on the desired physical properties. A silicon oxide coating can be formed. In the above formula, n=1 to 3, mainly n
=1 to 2 compounds are used in the present invention, but n=
In the case of compound No. 3, there is an effect of alkylsilylation treatment on the substrate surface. These silicon compounds can be used to make plastics, glass,
In treating the surface of a substrate made of metal or other various materials, a number of methods are used, such as the so-called casting method, spinner method, spray method, bar coating method, vapor deposition method, and CVD method. When treating the surface of a substrate using these methods and coating or spraying the silicon compound, the NCO group directly bonded to Si in the compound having an Si-NCO bond in the molecule as described above must be treated with a special catalyst. It easily reacts at room temperature with moisture in the air, moisture on the surface of the substrate, or OH groups, etc. to form siloxane bonds without using silane isocyanate, so simply treat the surface of the substrate with a compound containing such silane isocyanate in a normal atmosphere. It is possible to easily form a silicon oxide coating on the substrate surface by curing the silicon oxide coating. This silane isocyanate compound can be used in combination with other compounds if necessary. for example
A compound having no active hydrogen that reacts with the NCO group can be used in combination as a solvent. Examples of compounds that can be used as solvents include n-hexane, benzene, toluene, xylene, methylene chloride, trichlorethylene (triclene), fluorinated hydrocarbons (freon), dimethylformamide (DMF), dimethylsulfoxide (DMSO), and nitrobenzene. , methyl acetate, ethyl acetate, butyl acetate, and the like. Also, in order to provide adhesion, prevent alkali migration, and other functions during processing, it reacts with Si in the silane isocyanate compound to form a Si-O-M bond (M is a metal or nonmetallic element as shown below). A polyvalent metal compound or a hetero element compound that can be used may be used in combination. Compounds that can be used for this purpose include Mg, Ca,
Zn, B, Al, Sn, Ti, Zr, Sb, In, V, Ta,
Compounds containing metal or nonmetallic elements such as As, P, Fe, Co, Ni, and Cr can be mentioned. Therefore, these compounds can be used in various forms such as alkoxides, chelates, acylates, and hydroxides, but they must be non-aqueous and soluble in a solution consisting of a silane isocyanate compound or the above-mentioned solvent. . In the method of the present invention, as described above, a good silicon oxide coating is formed by processing in an atmosphere at normal room temperature, but it is of course possible to perform the treatment under heating if necessary, and when this is used, the coating is stabilized. This is preferable because it can promote the Thus, according to the method of the present invention, a silicon oxide coating can be formed on a substrate by a moisture curing method at room temperature or a low temperature in the vicinity thereof, but a silicon oxide coating can also be formed into which organic groups are optionally introduced depending on the desired physical properties. It is industrially useful. Examples of the present invention are shown below. The middle part of the example shows parts by weight. Example 1-6 A hard glass slide was thoroughly washed with detergent and alcohol to prepare a specimen. 10cm/min of this specimen
The physical properties of the coatings formed by treating the compounds of the following examples with a dipping/pulling method at a speed of 25% and curing them in an atmosphere of 65% RH and 25°C were measured.
【表】
実施例 ７
液中ガス導入管と気化ガス導出管を設けた密閉
ガラスフラスコにSi（NCO）4を入れ充分に乾燥し
たN2ガスを通しつつフラスコ温度を80℃に昇温
させた。この状態で導出管から出るSi（NCO）4気
化物を含むN2ガスを各種基体表面に吹き付けて
処理し65％RH、25℃の雰囲気で硬化させた。得
られた被覆は良好な物性を示した。[Table] Example 7 Si(NCO) 4 was placed in a sealed glass flask equipped with a submerged gas inlet pipe and a vaporized gas outlet pipe, and the flask temperature was raised to 80°C while sufficiently dry N 2 gas was passed through. . In this state, N 2 gas containing Si(NCO) 4 vapor released from the outlet tube was sprayed onto the surfaces of various substrates to cure them in an atmosphere of 65% RH and 25°C. The resulting coating showed good physical properties.
【表】
イルム
実施例 ８
CH3Si（NCO）310部、Si（NCO）490部の混合物
をシリコン単結晶板に2000rpmでスピンナー塗布
して25℃65％RHで20分間放置後赤外線ランプで
160℃に５分間加熱して均一膜を得た。
この処理膜の表面抵抗1015Ω／cm2であり煮沸テ
ストは25時間であつた。[Table] Illum Example 8 A mixture of 10 parts of CH 3 Si (NCO) 3 and 90 parts of Si (NCO) 4 was applied to a silicon single crystal plate using a spinner at 2000 rpm, left at 25°C, 65% RH for 20 minutes, and then exposed to an infrared lamp. in
A uniform film was obtained by heating to 160°C for 5 minutes. The surface resistance of this treated membrane was 10 15 Ω/cm 2 and the boiling test was for 25 hours.
Claims (1)
アネート化合物で基体表面を処理することからな
る珪素酸化物被覆形成法。 ２ シランイソシアネート化合物が分子中にSiに
直結するNCO基を少くとも２個含有する化合物
を含むものである特許請求の範囲第１項記載の方
法。 ３ 分子中にSi−NCO結合を含むシランイソシ
アネート化合物と、この化合物と反応してSi−Ｏ
−Ｍ結合（Ｍは金属又は非金属元素）を形成し得
る多価金属化合物又はヘテロ元素化合物を併用し
て基体表面を処理することからなる特許請求の範
囲第１項記載の方法。[Scope of Claims] 1. A method for forming a silicon oxide coating, which comprises treating the surface of a substrate with a silane isocyanate compound containing a Si-NCO bond in its molecule. 2. The method according to claim 1, wherein the silane isocyanate compound contains a compound containing at least two NCO groups directly bonded to Si in the molecule. 3 A silane isocyanate compound containing a Si-NCO bond in the molecule reacts with this compound to form Si-O
2. The method according to claim 1, which comprises treating the surface of the substrate using a polyvalent metal compound or a hetero element compound capable of forming a -M bond (M is a metal or a non-metal element).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57149997A JPS5939714A (en) | 1982-08-31 | 1982-08-31 | Formation of silicon oxide coat |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57149997A JPS5939714A (en) | 1982-08-31 | 1982-08-31 | Formation of silicon oxide coat |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5939714A JPS5939714A (en) | 1984-03-05 |
| JPH0225990B2 true JPH0225990B2 (en) | 1990-06-06 |
Family
ID=15487205
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57149997A Granted JPS5939714A (en) | 1982-08-31 | 1982-08-31 | Formation of silicon oxide coat |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5939714A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0891953A1 (en) * | 1997-07-15 | 1999-01-20 | Central Glass Company, Limited | Glass plate with water-repellent film and method for producing same |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2598520B1 (en) * | 1986-01-21 | 1994-01-28 | Seiko Epson Corp | MINERAL PROTECTIVE FILM |
| JP2812121B2 (en) * | 1986-01-21 | 1998-10-22 | セイコーエプソン株式会社 | Optical article manufacturing method |
| JP2655036B2 (en) * | 1986-01-21 | 1997-09-17 | セイコーエプソン株式会社 | Optical article manufacturing method |
| US5783299A (en) * | 1986-01-21 | 1998-07-21 | Seiko Epson Corporation | Polarizer plate with anti-stain layer |
| US5759643A (en) * | 1987-01-16 | 1998-06-02 | Seiko Epson Corporation | Polarizing plate and method of production |
| JPH07113683B2 (en) * | 1987-04-02 | 1995-12-06 | セイコーエプソン株式会社 | Optical article having inorganic coating film and method for producing the same |
| JPH062833B2 (en) * | 1988-06-03 | 1994-01-12 | 帝人株式会社 | Release film |
| JPH05341108A (en) * | 1993-01-20 | 1993-12-24 | Seiko Epson Corp | Method for reforming surface of inorganic coat film |
| JPH0682603A (en) * | 1993-02-03 | 1994-03-25 | Seiko Epson Corp | Antireflective optical article and its surface reforming method |
| JPH0688902A (en) * | 1993-02-03 | 1994-03-29 | Seiko Epson Corp | Optical article having inorganic coating film and modifying method for its surface |
| JPH0682605A (en) * | 1993-04-08 | 1994-03-25 | Seiko Epson Corp | Optical article having inorganic coating film and its surface reforming method |
| US6942924B2 (en) | 2001-10-31 | 2005-09-13 | Chemat Technology, Inc. | Radiation-curable anti-reflective coating system |
| JP3915054B2 (en) * | 2002-03-05 | 2007-05-16 | 株式会社トリケミカル研究所 | Film forming material, film forming method, and element |
| JP4353379B2 (en) * | 2006-12-19 | 2009-10-28 | 株式会社トリケミカル研究所 | Film forming material, film forming method, and element |
-
1982
- 1982-08-31 JP JP57149997A patent/JPS5939714A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0891953A1 (en) * | 1997-07-15 | 1999-01-20 | Central Glass Company, Limited | Glass plate with water-repellent film and method for producing same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5939714A (en) | 1984-03-05 |
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