JPS62169102A - Method for modifying surface of inorganic coating film - Google Patents
Method for modifying surface of inorganic coating filmInfo
- Publication number
- JPS62169102A JPS62169102A JP61010468A JP1046886A JPS62169102A JP S62169102 A JPS62169102 A JP S62169102A JP 61010468 A JP61010468 A JP 61010468A JP 1046886 A JP1046886 A JP 1046886A JP S62169102 A JPS62169102 A JP S62169102A
- Authority
- JP
- Japan
- Prior art keywords
- film
- coating film
- water
- inorganic
- lens
- 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.)
- Granted
Links
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- 238000000576 coating method Methods 0.000 title abstract description 25
- 239000011248 coating agent Substances 0.000 title abstract description 23
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- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
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- 230000002209 hydrophobic effect Effects 0.000 abstract description 5
- 230000007423 decrease Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
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- 238000011282 treatment Methods 0.000 description 14
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
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- BYLOHCRAPOSXLY-UHFFFAOYSA-N dichloro(diethyl)silane Chemical compound CC[Si](Cl)(Cl)CC BYLOHCRAPOSXLY-UHFFFAOYSA-N 0.000 description 6
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- 125000001424 substituent group Chemical group 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
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- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
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- JHQVCQDWGSXTFE-UHFFFAOYSA-N 2-(2-prop-2-enoxycarbonyloxyethoxy)ethyl prop-2-enyl carbonate Chemical compound C=CCOC(=O)OCCOCCOC(=O)OCC=C JHQVCQDWGSXTFE-UHFFFAOYSA-N 0.000 description 2
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 239000005331 crown glasses (windows) Substances 0.000 description 2
- MAYIDWCWWMOISO-UHFFFAOYSA-N dichloro-bis(ethenyl)silane Chemical compound C=C[Si](Cl)(Cl)C=C MAYIDWCWWMOISO-UHFFFAOYSA-N 0.000 description 2
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- 230000003068 static effect Effects 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
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- 238000007738 vacuum evaporation Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
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- QFLWZFQWSBQYPS-AWRAUJHKSA-N (3S)-3-[[(2S)-2-[[(2S)-2-[5-[(3aS,6aR)-2-oxo-1,3,3a,4,6,6a-hexahydrothieno[3,4-d]imidazol-4-yl]pentanoylamino]-3-methylbutanoyl]amino]-3-(4-hydroxyphenyl)propanoyl]amino]-4-[1-bis(4-chlorophenoxy)phosphorylbutylamino]-4-oxobutanoic acid Chemical compound CCCC(NC(=O)[C@H](CC(O)=O)NC(=O)[C@H](Cc1ccc(O)cc1)NC(=O)[C@@H](NC(=O)CCCCC1SC[C@@H]2NC(=O)N[C@H]12)C(C)C)P(=O)(Oc1ccc(Cl)cc1)Oc1ccc(Cl)cc1 QFLWZFQWSBQYPS-AWRAUJHKSA-N 0.000 description 1
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
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- QXKMQBOTKLTKOE-UHFFFAOYSA-N 3-[dichloro(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC[Si](C)(Cl)Cl QXKMQBOTKLTKOE-UHFFFAOYSA-N 0.000 description 1
- UUNGBOQAZQUJMZ-UHFFFAOYSA-N 3-bromopropyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CCCBr UUNGBOQAZQUJMZ-UHFFFAOYSA-N 0.000 description 1
- OLBGECWYBGXCNV-UHFFFAOYSA-N 3-trichlorosilylpropanenitrile Chemical compound Cl[Si](Cl)(Cl)CCC#N OLBGECWYBGXCNV-UHFFFAOYSA-N 0.000 description 1
- UIFBMBZYGZSWQE-UHFFFAOYSA-N 4-[dichloro(methyl)silyl]butanenitrile Chemical compound C[Si](Cl)(Cl)CCCC#N UIFBMBZYGZSWQE-UHFFFAOYSA-N 0.000 description 1
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- 239000005047 Allyltrichlorosilane Substances 0.000 description 1
- 241000501754 Astronotus ocellatus Species 0.000 description 1
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- 244000005687 Poranopsis paniculata Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FYTPGBJPTDQJCG-UHFFFAOYSA-N Trichloro(chloromethyl)silane Chemical compound ClC[Si](Cl)(Cl)Cl FYTPGBJPTDQJCG-UHFFFAOYSA-N 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- ABHNFDUSOVXXOA-UHFFFAOYSA-N benzyl-chloro-dimethylsilane Chemical compound C[Si](C)(Cl)CC1=CC=CC=C1 ABHNFDUSOVXXOA-UHFFFAOYSA-N 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- BNCXNUWGWUZTCN-UHFFFAOYSA-N trichloro(dodecyl)silane Chemical compound CCCCCCCCCCCC[Si](Cl)(Cl)Cl BNCXNUWGWUZTCN-UHFFFAOYSA-N 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- ZOYFEXPFPVDYIS-UHFFFAOYSA-N trichloro(ethyl)silane Chemical compound CC[Si](Cl)(Cl)Cl ZOYFEXPFPVDYIS-UHFFFAOYSA-N 0.000 description 1
- SRQHGWJPIZXDTA-UHFFFAOYSA-N trichloro(heptyl)silane Chemical compound CCCCCCC[Si](Cl)(Cl)Cl SRQHGWJPIZXDTA-UHFFFAOYSA-N 0.000 description 1
- LFXJGGDONSCPOF-UHFFFAOYSA-N trichloro(hexyl)silane Chemical compound CCCCCC[Si](Cl)(Cl)Cl LFXJGGDONSCPOF-UHFFFAOYSA-N 0.000 description 1
- JIWLOZPAQDZWQN-UHFFFAOYSA-N trichloro(icosyl)silane Chemical compound CCCCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl JIWLOZPAQDZWQN-UHFFFAOYSA-N 0.000 description 1
- SSBOTKQTCWQWMG-UHFFFAOYSA-N trichloro(nonyl)silane Chemical compound CCCCCCCCC[Si](Cl)(Cl)Cl SSBOTKQTCWQWMG-UHFFFAOYSA-N 0.000 description 1
- RCHUVCPBWWSUMC-UHFFFAOYSA-N trichloro(octyl)silane Chemical compound CCCCCCCC[Si](Cl)(Cl)Cl RCHUVCPBWWSUMC-UHFFFAOYSA-N 0.000 description 1
- KWDQAHIRKOXFAV-UHFFFAOYSA-N trichloro(pentyl)silane Chemical compound CCCCC[Si](Cl)(Cl)Cl KWDQAHIRKOXFAV-UHFFFAOYSA-N 0.000 description 1
- HZFOTCWMVIXGCN-UHFFFAOYSA-N trichloro(phenoxy)silane Chemical compound Cl[Si](Cl)(Cl)OC1=CC=CC=C1 HZFOTCWMVIXGCN-UHFFFAOYSA-N 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- HKFSBKQQYCMCKO-UHFFFAOYSA-N trichloro(prop-2-enyl)silane Chemical compound Cl[Si](Cl)(Cl)CC=C HKFSBKQQYCMCKO-UHFFFAOYSA-N 0.000 description 1
- DOEHJNBEOVLHGL-UHFFFAOYSA-N trichloro(propyl)silane Chemical compound CCC[Si](Cl)(Cl)Cl DOEHJNBEOVLHGL-UHFFFAOYSA-N 0.000 description 1
- LPMVYGAHBSNGHP-UHFFFAOYSA-N trichloro(tetradecyl)silane Chemical compound CCCCCCCCCCCCCC[Si](Cl)(Cl)Cl LPMVYGAHBSNGHP-UHFFFAOYSA-N 0.000 description 1
- CPYKRKMVWIPNFZ-UHFFFAOYSA-N trichloro-(3-chloro-2-phenylpropyl)silane Chemical compound Cl[Si](Cl)(Cl)CC(CCl)C1=CC=CC=C1 CPYKRKMVWIPNFZ-UHFFFAOYSA-N 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、無機コート膜の表面状態の改ｉ法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for modifying the surface state of an inorganic coat film.
本発明は、無機コート膜の表面改質法において、無機コ
ート膜に各種の機能を持つ九ノ・ロゲン化シラン化合物
を反応させることにより、無機コート膜に槙々の機能を
付与し友ものである。In the surface modification method of an inorganic coat film, the present invention is a method for imparting various functions to the inorganic coat film by reacting the inorganic coat film with a silane compound having various functions. be.
真空蒸着法、イオンブレーティング法、スノくツタリン
グ＠などによって得られる無機コート膜は、眼鏡、レン
ズ等元学材料の反射防止膜、ハードコート膜、各種機能
性膜などに広く用いられている。Inorganic coating films obtained by vacuum evaporation, ion blating, snow vine coating, etc. are widely used as antireflection films, hard coat films, and various functional films for materials such as glasses and lenses.
特にＳｉｎ、農は、その基板との付着力、硬度、取扱い
易さなどの点で幅広く使用されている。In particular, Sin (N) is widely used because of its adhesion to substrates, hardness, ease of handling, and the like.
しかし、１３１０．等の無機コート膜は、８１．Ｎａ。 However, 1310. Inorganic coated films such as 81. Na.
Ｃａ、 等の不純物を含む水滴が付着した場合、乾燥
する過程に於いて不純物が無機コート膜表面に残り、い
わゆるヤク現象金起こす。When water droplets containing impurities such as Ca, etc. adhere, the impurities remain on the surface of the inorganic coat film during the drying process, causing a so-called yak phenomenon.
ま友、蒸着による膜はバルクに比べ一般に密度が小さく
、膜内での水分子、気体分子等の移動も容易であると考
えられる。その為、水分子等が膜の表面に吸着、その後
拡散によＶ膜と基材の界面に達し、膜の密着性に悪影響
を及ぼすなど、耐久性の低下を招いていた。さらに環境
の温度差により光学材料上のコート膜表面に水滴が細か
く付着して生ずる曇りにより、材料の透過率が低下する
という問題もあった。その他、表面帯電によりホコリが
つきやすいなど表面状態から生じる樵々の問題がある。Well, a film formed by vapor deposition generally has a lower density than a bulk film, and it is thought that water molecules, gas molecules, etc. can easily move within the film. Therefore, water molecules and the like are adsorbed on the surface of the film and then diffused to reach the interface between the V film and the base material, adversely affecting the adhesion of the film and causing a decrease in durability. Furthermore, due to environmental temperature differences, fine water droplets adhere to the surface of the coating film on the optical material, resulting in clouding, which reduces the transmittance of the material. In addition, woodcutter problems arise from the surface condition, such as the tendency for dust to accumulate on the surface due to electrostatic charge.
そこで本発明は、このような問題点全解決するもので、
その目的とするところは、無機コート膜の表面状態を改
質し、上記にあげ友様な種々の問題１ｉ−１つまたに２
つ以上解消できうる機能全表面に持たせるところにある
。Therefore, the present invention aims to solve all of these problems.
The purpose of this is to modify the surface condition of the inorganic coated film and to solve various problems listed above.
The problem lies in the fact that the entire surface has functions that can eliminate more than one problem.
本発明の無機コート膜の表面改質法に、無機コート膜に
、ハロゲン化シラン化合物を反応させ次ことを特徴とす
る。The method for surface modification of an inorganic coated film according to the present invention is characterized in that the inorganic coated film is reacted with a halogenated silane compound.
無機コート膜に処理上行なうには、すでに基材上に存在
しているコート膜の性質、密着性、耐久性を低下させず
に処理を行う必豊かある。その為には、密着性、耐久性
上低下させない温Ｋ及び環境で、かつ反射防止膜等の分
光特性に影響を与えないなど、層全体に影響を与えない
程度の表面付近で反応上行なう処理が望ましい。本発明
で用いるハロゲン化シラン化合物は、水酸基の存在下で
、たとえばＳ１０．膜表面付近に対して下に示すような
脱塩酸反応が起こり、水酸基の存在する表面の反応に非
常に有効である。In order to carry out further processing on an inorganic coated film, it is necessary to carry out the processing without reducing the properties, adhesion, and durability of the coated film already present on the substrate. To achieve this, it is necessary to perform reactive treatment near the surface at a temperature that does not reduce adhesion and durability, and at a temperature that does not affect the spectral characteristics of anti-reflection coatings, etc., and at a level that does not affect the entire layer. is desirable. The halogenated silane compound used in the present invention can be used in the presence of a hydroxyl group, for example, S10. The dehydrochlorination reaction shown below occurs near the membrane surface, and is very effective for reactions on the surface where hydroxyl groups are present.
バ
（Ｒは任意の置換基）
ハロゲン化シラン化合物の反応に関与するハロゲンとは
別の８１に対する残りの置換基に種々の機能を持次せる
ことができる。コート膜の表面に持たせる機能としては
、疎水性、親水性、導電性、ぬれ性、耐摩耗性１分離性
、バリヤー性、吸着機能など用途に応じて多彩に選択で
きる。本発明では、用途に応じた機能を持つ基會有する
ハロゲン化シラン化合物を用いることによって表面の改
質を行なう。(R is an arbitrary substituent) The remaining substituents for 81 other than the halogen involved in the reaction of the halogenated silane compound can have various functions. Functions to be imparted to the surface of the coated film can be selected from a variety of options depending on the application, such as hydrophobicity, hydrophilicity, conductivity, wettability, abrasion resistance, separability, barrier properties, and adsorption function. In the present invention, the surface is modified by using a halogenated silane compound having a group having functions depending on the intended use.
本発明で用いるハロゲン化シラン化合物としてハ、トリ
メチルクロロシラン、ジメチルジクロロシラン、メチル
トリクロロシラン、ジエチルジクロロシラン、トリクロ
ロシラン、クロロメチルトリクロロシラン、メチルジク
ロロシ９ｙ、１．２−ジブロモエチルトリクロロシラン
、ビニルトリクロロシラン、１．２−ジクロロエチルト
リクロロクラン、１−／ロロエテルトリクロロシラン、
２−クロロエチルトリクロロシラン、クロロメチルメチ
ルジクロロシラン、エチルトリクロロシラン、エチルジ
クロロシラン、ジメチルクロロシラン、へ４３トリフル
オロクロピルトリクロロシラン、２−シアノエチルトリ
クロロシラン、アリルトリクロロシラン、３−ブロモプ
ロピルトリクロロシラン、メチルビニルジクロロシラン
、３クロロ７０ピルトリクロロシラン、ジクロロメチル
ジメチルクロロシラン、ｎ−プロピルトリクロロシラン
、クロロメチルジメチルクロロシラン、エチルメチルジ
クロロシラン、ニドキシメチルジクロロシラン、ジメト
キシメチルクロロシラン、ジビニルジクロロシラン、３
−シアノプロピルトリクロロシラン、メチル−４４３−
トリフルオロクロロビルジクロロシラン、アリルメチル
ジクロロシラン、ジメチルビニルクロロシラン、ｎ−ブ
チルトリクロロシラン、５−クロロクロビルメチルジク
ロロシラン、インブチルトリクロロシラン、メチルクロ
ビルジクロロシラン、ジェトキシジクロロシラン、３−
シアノプロピルメチルジクロロシラン、アリルジメチル
クロロシラン、ペンチルトリクロロシラン、３−クロロ
プロピルジメチルクロロシラン、ブチルメチルジクロロ
シラン、ジメチルフ”ロビル／ ｏ ｏ ｙ ５ン、ジ
メテルイソグロビルクロロシラン、４へ４．４．５．５
．６．４６−ノナフルオロヘキジルトリクロロシランｓ
’−／クロフェニルトリクロロシラン、フェニルトリク
ロロシラン、フェノキジトリクロロシラン、フェニルジ
クロロシラン、ジアリルジクロロシラン、シクロヘキシ
ルトリクロロシラン、３−シアノクロビルジメチルクロ
ロシラン、ヘキシルトリクロロシラン、メチルペンチル
ジクロロシラン、ｔａｒｔ−ブチルジメチルクロロシラ
ン、トリエチルクロロシラン、３，４４，４゜５、５．
４６．６−ノナフルオロヘキジルメチルジクロロシラン
、ベンジルトリクロロシランｓ ｐ−ト’）ルトリク
ロロ７ラン、メチルフェニルジクロロシラン、メチルフ
ェニルクロロシラン、６−ドリクロロシリルー２−ノル
ボルネンｓ２−ト’）／クロシリルノルボル不ン、シク
ロヘキシルメチルジクロロシラン、ヘプチルトリクロロ
シラン、ヘキシルメチルジクロロシラン、フェニルビニ
ルジクロロシラン、β−７エネテルトリクロロシラン、
ジメチルフェニルクロロシラン、２−（４−シクロヘキ
セニルエチル）トリクロロシラン、２−メチルジクロロ
シリルノルボルネン、３−メタクリルオキシプロピルメ
チルジクロロシラン、オクチルトリクロロシラン、ヘプ
チルメチルジクロロシラン、シフチルジクロロシラン、
アリルフェールジクロロシラン、クロロメチルフェニル
エチルトリクロロシラン、メチルフェニルビニルクロロ
シラン、３−クロロプロピルフェニルジクロロシラン、
２−フェニルプロピルトリクロロシラン、メチル−β−
７エネテルジクロロシラン、ベンジルジメチルクロロシ
ラン、ノニルトリクロロシラン、メチルオクチルジクロ
ロシラン、トリプロヒルクロロシラン、ｔｅｒｔ−ブチ
ルフェニルジクロロシラン、デシルトリクロロシラン、
ジメチルオクチルクロロシラン、デシルメチルジクロロ
シラン、ジフェニルジクロロシラン、ジフェニルジフル
オロ７ラン、ジフェニルクロロシラン、ドデシルトリク
ロロシラン、ジヘキシルジクロロシラン、トリブチルク
ロロシラン、ジフェニルメチルクロロシラン、ドデシル
メチルジクロロシラン、ジフェニルビニルクロロシラン
、テトラデシルトリクロロシラン、トリフェニルクロロ
シラン、トリヘキシルクロロシラン、メチルオクタデシ
ルジクロロシラン、エイコシルトリクロロシラン、ジメ
チルオクタデシルクロロシラン、トリベンジルクロロシ
ラン、トコジルトリクロロシラン、トコシルメチルジク
ロロシラン、１．２−ビス（） ＩＪジクロロリル）エ
タン、１．２−ビス（メチルジクロロシリル）エタン、
１，１．４４−テトラメチル−１，３−ジクロロジシロ
キサン、１．２−ビス（ジメチルクロロシリル）エタン
、１．４−ビス（ジメチルクロロシリル）ベンゼン、１
．３−ジクロロテトラインプロピルジシロキサン、１ｉ
、Ａ４５．５−ヘキサメチル−１、ｓ −ジクロロトリ
シロキサン、１．７−ジクロロオクタメチルテトラシロ
キサン、などがあげられる。Halogenated silane compounds used in the present invention include trimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, diethyldichlorosilane, trichlorosilane, chloromethyltrichlorosilane, methyldichlorosilane, 1,2-dibromoethyltrichlorosilane, vinyltrichlorosilane, Chlorosilane, 1,2-dichloroethyltrichlorosilane, 1-/loloetheltrichlorosilane,
2-chloroethyltrichlorosilane, chloromethylmethyldichlorosilane, ethyltrichlorosilane, ethyldichlorosilane, dimethylchlorosilane, trifluorocropyltrichlorosilane, 2-cyanoethyltrichlorosilane, allyltrichlorosilane, 3-bromopropyltrichlorosilane, methyl Vinyldichlorosilane, 3chloro70pyltrichlorosilane, dichloromethyldimethylchlorosilane, n-propyltrichlorosilane, chloromethyldimethylchlorosilane, ethylmethyldichlorosilane, nidoxymethyldichlorosilane, dimethoxymethylchlorosilane, divinyldichlorosilane, 3
-cyanopropyltrichlorosilane, methyl-443-
Trifluorochlorovirdichlorosilane, allylmethyldichlorosilane, dimethylvinylchlorosilane, n-butyltrichlorosilane, 5-chlorochlorovirmethyldichlorosilane, inbutyltrichlorosilane, methylchlorovirdichlorosilane, jetoxydichlorosilane, 3-
Cyanopropylmethyldichlorosilane, allyldimethylchlorosilane, pentyltrichlorosilane, 3-chloropropyldimethylchlorosilane, butylmethyldichlorosilane, dimethylfluoroyl/o-o-y-5, dimethelisoglobylchlorosilane, 4 to 4.4.5 .5
．． 6.46-nonafluorohexyltrichlorosilane s
'-/Clophenyltrichlorosilane, phenyltrichlorosilane, phenoxytrichlorosilane, phenyldichlorosilane, diallyldichlorosilane, cyclohexyltrichlorosilane, 3-cyanoclovirdimethylchlorosilane, hexyltrichlorosilane, methylpentyldichlorosilane, tart-butyldimethylchlorosilane , triethylchlorosilane, 3,44,4°5,5.
46.6-nonafluorohexylmethyldichlorosilane, benzyltrichlorosilanesp-t')-trichloro7-rane, methylphenyldichlorosilane, methylphenylchlorosilane, 6-dolychlorosilyl-2-norbornene-s2-t')/ Crosilylnorborane, cyclohexylmethyldichlorosilane, heptyltrichlorosilane, hexylmethyldichlorosilane, phenylvinyldichlorosilane, β-7enethertrichlorosilane,
Dimethylphenylchlorosilane, 2-(4-cyclohexenylethyl)trichlorosilane, 2-methyldichlorosilylnorbornene, 3-methacryloxypropylmethyldichlorosilane, octyltrichlorosilane, heptylmethyldichlorosilane, cyphthyldichlorosilane,
Allylferdichlorosilane, chloromethylphenylethyltrichlorosilane, methylphenylvinylchlorosilane, 3-chloropropylphenyldichlorosilane,
2-phenylpropyltrichlorosilane, methyl-β-
7eneterdichlorosilane, benzyldimethylchlorosilane, nonyltrichlorosilane, methyloctyldichlorosilane, triproylchlorosilane, tert-butylphenyldichlorosilane, decyltrichlorosilane,
Dimethyloctylchlorosilane, decylmethyldichlorosilane, diphenyldichlorosilane, diphenyldifluoro7rane, diphenylchlorosilane, dodecyltrichlorosilane, dihexyldichlorosilane, tributylchlorosilane, diphenylmethylchlorosilane, dodecylmethyldichlorosilane, diphenylvinylchlorosilane, tetradecyltrichlorosilane, Triphenylchlorosilane, trihexylchlorosilane, methyloctadecyldichlorosilane, eicosyltrichlorosilane, dimethyloctadecylchlorosilane, tribenzylchlorosilane, tocodyltrichlorosilane, tocosylmethyldichlorosilane, 1,2-bis()IJdichlorolyl)ethane, 1 .2-bis(methyldichlorosilyl)ethane,
1,1.44-tetramethyl-1,3-dichlorodisiloxane, 1,2-bis(dimethylchlorosilyl)ethane, 1,4-bis(dimethylchlorosilyl)benzene, 1
．． 3-dichlorotetranepropyldisiloxane, 1i
, A45.5-hexamethyl-1,s-dichlorotrisiloxane, 1,7-dichlorooctamethyltetrasiloxane, and the like.
例えば、疎水性の基′？ｌ−有するノ・ロゲン化シラン
化合物金用いることによＶ％水によるヤケの防止、膜の
耐水性の向上、水による密着性の低下防止が期待できる
。さらに摩擦係数の低下が伴なえば、膜の耐摩耗性の同
上が期待できる。For example, a hydrophobic group'? By using a silane compound having l-V% water, it can be expected to prevent discoloration due to water, improve the water resistance of the film, and prevent deterioration in adhesion due to water. Furthermore, if this is accompanied by a decrease in the coefficient of friction, the wear resistance of the film can be expected to improve as well.
さらに後処理によって親水性の基に変換さｎるようなＷ
ｔ置換基持つノ・ロゲン化シラン化合物、あるいは後処
理によって親水性の基に変換されるような置換基と疎水
基を合わせ持ったノ・ロゲン化シラン化合物を無機コー
ト膜に反応させたのち、後処理である観水性処！七行な
えば、コート膜表面に親水性、あるいは親水性と疎水性
上台わせ持つ様な機能を持たせることも可能である。後
処理として、別の物質をコート膜と反応しｔハロゲン化
シラン化合物に反応させてもよい。後処理により親水性
上最表面に持たせ、疎水性の基がコート膜と親水性基の
間に配置していれば、ぬｎ性によくても水分子を透過さ
せないなどの複合機能ｔコート膜に持たせることができ
る。このように後処理により相反する機能を同時にコー
ト膜に持たせることが可能である。Furthermore, W that is converted into a hydrophilic group by post-treatment
After reacting the inorganic coated film with a rosogenated silane compound having a t substituent, or a rosogenated silane compound having both a substituent and a hydrophobic group that can be converted into a hydrophilic group by post-treatment, A water-viewing place for post-processing! By performing seven lines, it is possible to make the surface of the coating film hydrophilic or have a function of having both hydrophilic and hydrophobic properties. As a post-treatment, another substance may be reacted with the coat film to react with the halogenated silane compound. If a hydrophilic group is placed on the outermost surface through post-treatment, and a hydrophobic group is placed between the coating film and the hydrophilic group, a multi-functional t-coat that has good wettability but does not allow water molecules to pass through. It can be attached to a membrane. In this way, it is possible to simultaneously provide the coat film with contradictory functions through post-treatment.
ハロゲン化シラン化合物を無機コート膜に反応させるに
は５Ｄｉｐ伝、スピナー法、スプレー法等により表面に
ハロゲン化シラン化合物を塗布（反応させる方法、まｆ
ｃは、真空雰囲気中あるいに大気中でハロゲン化シラン
化合物ガス全無機コート膜と反応させる方＠など用いる
ことができる。前者の場合、塗布中の雰囲気、友とえば
湿度、温既’４１退にコントロールすることにより、ニ
ジ反応が促進されるし、又漬時間も反応が十分終了する
時間が望ましい。また、塗布後コート膜の特性に影響を
与えない程度の熱を加えることにより反応紫促進すｎば
より効果的である。後者の場合、真空槽内で無機コート
膜全形成後、）・ロゲン化シラン化合物ガスを導入し反
応させてもよい。また、無機コート膜形成後、Ａｒガス
等のプラズマ雰囲気中にハロゲン化シラン化合物ガスを
導入し、反応性蒸着、反応性イオンプレーテインク等を
行うことも可が目である。To make the halogenated silane compound react with the inorganic coating film, apply the halogenated silane compound to the surface using 5Dip method, spinner method, spray method, etc.
c can be reacted with a halogenated silane compound gas and an all-inorganic coating film in a vacuum atmosphere or in the air. In the former case, the reaction is promoted by controlling the atmosphere during coating, such as humidity and temperature, and the soaking time is preferably a time sufficient to complete the reaction. Further, it is more effective to accelerate the reaction by applying heat to an extent that does not affect the properties of the coated film after application. In the latter case, after the inorganic coat film is completely formed in a vacuum chamber, a rogensated silane compound gas may be introduced and reacted. Further, after forming the inorganic coat film, it is also possible to introduce a halogenated silane compound gas into a plasma atmosphere such as Ar gas and perform reactive vapor deposition, reactive ion plate ink, etc.
ハロゲン化シラン化合物との反応性Ｆａ％める為に前処
理として、無機コート膜表面に、洗浄、薬品処理、１ラ
ズマ処理を行なうとより効果的である。In order to reduce the reactivity Fa% with the halogenated silane compound, it is more effective to perform cleaning, chemical treatment, and 1-laser treatment on the surface of the inorganic coated film as a pretreatment.
反応に用いるハロゲン化シラン化合物は単体で用いても
よいし、溶媒で希釈して用いることも可能であるが、こ
の場合、水ｆＲ基に１１ない溶媒を用いることが、液寿
命の点で好ましい。例えば、溶媒として、トルエン、塩
化メチレン、１．４４−トリフロロトリクロロエタン、
トリクロロエチレン、テトラヒドロフラン等を用いるこ
とができる。The halogenated silane compound used in the reaction may be used alone or diluted with a solvent, but in this case, it is preferable to use a solvent that does not have 11 in the water fR group in terms of liquid life. . For example, as a solvent, toluene, methylene chloride, 1,44-trifluorotrichloroethane,
Trichlorethylene, tetrahydrofuran, etc. can be used.
反応が終了後、大気中の水分子と反応しｔノ１０ゲン化
シラン化合物、；−ト膜表面との反応に寄与できなかつ
次ハロゲン化シラン化合物を洗浄により洗い流すことに
よジ、処理前と反射防止特性などの外観が変わらない処
理上行うことができる。After the reaction is completed, the halogenated silane compounds that react with water molecules in the atmosphere, and the halogenated silane compounds that cannot contribute to the reaction with the membrane surface are washed away. It is possible to carry out treatments that do not change the appearance, such as anti-reflection properties.
洗浄方法としては、反応終了後、純水などで洗浄して反
応に寄与できなかったハロゲン化シラン化合′＠全処理
し、その後、トルエン、塩化メチレン、１．３．４−）
＋７７０ロトリクロロエタン、トリクロロエチレン、テ
トラヒドロフラン等の溶媒で洗浄するとよｔ）５ＩｙＪ
来的である。As for the cleaning method, after the reaction is complete, wash with pure water etc. to completely process the halogenated silane compounds that could not contribute to the reaction, and then use toluene, methylene chloride, etc.
+770 Wash with a solvent such as trichloroethane, trichloroethylene, or tetrahydrofuran.t)5IyJ
It is conventional.
今まで述べｔ処理ニ８１０！、Ａｔ、０３．ｚｒＯｌ。The processing described so far is 810! , At, 03. zrOl.
Ｔａ１０ｇ 、 ＭｇＦ’ｌ 、 ＣｏＯ２等あらゆる
無機コート膜表面に可能であるが１反応性の点などから
特に８１０！膜、ＳｉＯ膜、 ５ｉＯ（１＋ｚ） （
０＜１＜ １ ）で表わさｎ；ｂ襖に対して有効である
。It is possible to coat the surface of any inorganic film such as Ta10g, MgF'l, CoO2, etc., but 810! film, SiO film, 5iO(1+z) (
It is valid for n; b fusuma expressed as 0<1<1).
無機コート膜に目的に応じた機能を持つハロゲン化シラ
ン化合１１反応させたことにより、無機コート膜表面の
物性が変化し、コート膜の特性全署しく変化させること
ができる。たとえば、疎水性全表面に持たせれば、水や
その中に含まれる不純物とコート膜表面の結合性が弱ま
り、ヤケ現象の防止につながる。また表面が疎水性であ
る為に、水分に対し表面がレイルターの役目をは比し、
水分子によるコート膜全体の耐久性劣化金防ぐことがで
きる。さらに表面の摩擦係数が低下することにより、付
着したゴミなどのすベジがよくなり耐摩耗性が向上する
。By reacting the inorganic coat film with a halogenated silane compound 11 having a function according to the purpose, the physical properties of the surface of the inorganic coat film change, and the characteristics of the coat film can be completely changed. For example, if the entire surface is made hydrophobic, the bond between water and impurities contained therein and the coating film surface will be weakened, leading to the prevention of discoloration. In addition, since the surface is hydrophobic, the surface acts as a layer against moisture.
The durability of the entire coated film due to water molecules can be prevented from deteriorating. Furthermore, by lowering the coefficient of friction on the surface, adhering dirt and other particles are better removed and wear resistance is improved.
ま友、親水性を表面に持たし次場合、水の接触角が低下
することにより、細かい水滴が発生しにくくなり元の乱
反射による曇りの現象が防げ、表面の電気伝導度が上る
ことにより、表面の帯電防止となり、コート膜表面にホ
コリ等がつきにくくなる。When the surface has hydrophilic properties, the contact angle of water decreases, making it difficult for fine water droplets to form, preventing the clouding phenomenon caused by diffused reflection, and increasing the electrical conductivity of the surface. It prevents the surface from becoming static, making it difficult for dust to adhere to the surface of the coated film.
以下実施例に基づき本発明の詳細な説明するが本発明は
これらに限定されるものでにない。The present invention will be described in detail below based on Examples, but the present invention is not limited thereto.
〔実施例１〕
ジエチレングリコールビス（アリルカーボネート）製樹
脂からなる合成樹脂製レンズをアセトンで洗浄し、その
後真空蒸着法によジ基板温度５０℃で合成樹脂製レンズ
表面に反射防止処理を行なった。膜構成にレンズ側から
８１０！がλｏ／４゜Ｚｒ０ｕＢ：５ｉＯｅの合計膜厚
がλ６／ ４ 、 ＺｒＯ，Ｉｌｌがλｏ／４．最上
／１１のＳｉＯ，ｉｌがλｏ／ ４とした。次にこのレ
ンズ七インクロビルアルコールで洗浄し、十分乾燥させ
次後、液温１５℃のジメチルジクロルシラン９８％溶液
に、１分間浸漬した。浸漬後、湿度６０％、温度２５℃
の雰囲気中で、１ｃＷＩ／秒の速度でレンズを引き上げ
た。引き上げ後、６０℃の雰囲気中に３０分間放置し、
その後トリクロロエチレンにより洗浄上行なった。洗浄
後のレンズの外観、反射防止特性に、大きな変化にみら
れなかった。[Example 1] A synthetic resin lens made of diethylene glycol bis(allyl carbonate) resin was cleaned with acetone, and then an antireflection treatment was applied to the surface of the synthetic resin lens by vacuum evaporation at a substrate temperature of 50°C. 810 from the lens side to the film configuration! is λo/4°, the total film thickness of Zr0uB:5iOe is λ6/4, and ZrO, Ill is λo/4. Mogami/11 SiO,il was set to λo/4. Next, this lens was washed with 7-inclovir alcohol, thoroughly dried, and then immersed for 1 minute in a 98% solution of dimethyldichlorosilane at a temperature of 15°C. After soaking, humidity 60%, temperature 25℃
The lens was pulled up at a speed of 1 cWI/sec in an atmosphere of . After pulling it up, it was left in an atmosphere at 60°C for 30 minutes,
Thereafter, washing was performed with trichlorethylene. No major changes were observed in the appearance or antireflection properties of the lenses after cleaning.
得られ几コート膜の評価方法は以下に示す方法を用い友
。The obtained coating film was evaluated using the method shown below.
■ ヤケ性：水道水に：２−ト膜表面に次らし乾燥させ
たのち、布で残留物に払き取った。残留物が残れｒｌ’
Ｃ、完全に払きとれればＡ、一部残ればＢと評価した
。■ Stain resistance: Added to tap water. After drying, the residue was wiped off with a cloth. Residue remains rl'
It was rated C, if it was completely removed, it was rated A, and if some remained, it was rated B.
■ 耐摩耗性：コート膜表面を布で１ ｋｆの荷重をか
け１０００回摩擦し次。傷のついた置台を以下の３段階
に分けて評価し友。■ Abrasion resistance: Rub the surface of the coated film 1000 times with a cloth under a load of 1 kf. We evaluated the scratched stand by dividing it into the following three levels.
Ａ：全く傷がつかない。A: No scratches at all.
Ｂ：１〜１０本、細かい傷がつく。B: 1 to 10 fine scratches.
Ｃ：＃かく無数に傷がつく。C: #There will be countless scratches.
■ 密着性：３０℃の純水に１週間浸漬した後、コート
膜の密着性を調べた。コート膜の密層性な、ＪＩＳＤ−
０２ｔ１２に準じてクロスカットテープ試験によって行
った。即ち、ナイフ上用い、レンズ表面に１１１１間隔
に切れ目を入れ％１１１１１”のマス目？１００個形成
させる。■ Adhesion: The adhesion of the coated film was examined after being immersed in pure water at 30°C for one week. Dense coating film, JISD-
A cross-cut tape test was conducted in accordance with 02t12. That is, using a knife, incisions are made on the lens surface at 1111 intervals to form 100 squares of %11111''.
次に、その上へセロファン粘漕テープ（日東化学（帽「
セロテープ″）を強くおしつけ友後、表面から９００万
同へ、急に引つばジ剥離したのち、コート被膜の残って
いるマス目ｔもって＠滑性指標とし次。Next, apply cellophane adhesive tape (Nitto Chemical) on top of it.
After strongly applying cellophane tape ("Cellotape"), it suddenly peeled off from the surface to 9,000,000 yen, and then the remaining squares of the coating film were used as an index of lubricity.
■ 接触角：接触角計（協和科学株式会社展ＣＡ−Ｄ型
）を用いて液滴法により測足し友。■ Contact angle: Measured by the droplet method using a contact angle meter (Kyowa Scientific Co., Ltd. Exhibition CA-D model).
■防曇性：試料を湿度２０チ、温度５℃の雰囲気中に５
０分間放置後、湿度８０％、温度３０℃の雰囲気に堰９
出し、曇りの消失する時間ヶ測定した。■Anti-fogging property: Place the sample in an atmosphere with a humidity of 20 degrees and a temperature of 5 degrees Celsius.
After leaving it for 0 minutes, weir 9 was placed in an atmosphere with a humidity of 80% and a temperature of 30°C.
The time required for the cloudiness to disappear was measured.
■ 防塵性：スタティックオネストメーター（宍戸商会
製）による帯電圧の半減期全測定した。（測定条件：温
度２５℃、相対湿度６０％）
〔実施例２〕
クラウンガラスからなるレンズ表面に、レンズ側から屈
折率１．６０の償化アルミニウムを１μｍ厚にアルゴン
プラズマ申でイオンブレーティングした後、Ｃｒ１ＬＬ
ＣＩ０２μｍ真空蒸溜し、その上ＶＣＭｇＦ、 ｆｏ、
１２ μｍアルゴンプラズマ中でイオンブレーティン
グして反射防止層全形成し次。この様にして得られ之し
ンズ葡、純水で洗浄後、十分に水ｗｖＪｖ乾燥させた。■ Dust resistance: The entire half-life of the electrostatic voltage was measured using a static honest meter (manufactured by Shishido Shokai). (Measurement conditions: temperature 25°C, relative humidity 60%) [Example 2] On the surface of a lens made of crown glass, a 1 μm thick layer of compensated aluminum with a refractive index of 1.60 was ion-blated with argon plasma from the lens side. After, Cr1LL
CI02μm vacuum distilled, and VCMgF, fo,
The entire anti-reflection layer was formed by ion blasting in a 12 μm argon plasma. The grapes thus obtained were washed with pure water and thoroughly dried with water.
その後塩化メチレンにＬ９１０％に希釈されたジエチル
ジクロロシラン層液にレンズを１分間浸漬した。浸漬後
、湿度８０％、温度２５℃中で、１０儒／分の割合でレ
ンズ全引き上げ、塩化メチレン９９．９％浴推により洗
浄した。洗浄後の外観は処理ｉｔＪとほとんど変化がな
かった。Thereafter, the lens was immersed for 1 minute in a diethyldichlorosilane layer solution diluted with L910% in methylene chloride. After immersion, the lens was completely lifted out at a rate of 10 F/min at a humidity of 80% and a temperature of 25° C., and washed in a 99.9% methylene chloride bath. The appearance after washing was almost unchanged from that of treated itJ.
〔実施例３〕
実施例１で最上階のＳｉｎ、／傍七形成後、８１０１表
面ヲアルゴンガスプラズマで１分間懺面処理を行なった
後にメチル−ｈｓ、ｓ−トリフロロプロビルジクロロシ
ラン２５ｃｃフ分の割合で真空槽内へ２分間導入し友。[Example 3] After the formation of the topmost layer of Sin, /S, in Example 1, the surface of 8101 was treated with argon gas plasma for 1 minute, and then 25 cc of methyl-hs, s-trifluoropropyldichlorosilane was applied. Introduce the sample into the vacuum chamber for 2 minutes at a rate of 2 minutes.
その時の表面温度は５５℃であった。その後レンズを大
気中に取り出し、テトラヒドロフランにより洗浄を行な
つ之。洗浄後の外観は処理前とほとんど変化がなかった
。The surface temperature at that time was 55°C. The lens was then taken out into the atmosphere and cleaned with tetrahydrofuran. The appearance after washing was almost unchanged from before treatment.
〔実施例４〕
実施例１で得られた処理前の反射防止膜つき合成樹脂製
レンズ上１真空槽内にセットし、アルゴンと水の比が１
００：５の混合ガスを真空槽内に真空度が０．ＩＴｏｒ
ｒｌ／Ｃなる株専入し、１ｉ５６ＭＨｚの高周波電場に
より雰囲気ｔプラズマ化した。プラズマ出力１３００Ｗ
とし３０秒処ＩＭｔ行なった。その後真空槽よりレンズ
ｔと９だし、スプレー法により、１−７ジクロロオクタ
メチルテトラシロキサン９９．９％溶液″ｆｔ塗布した
。その仮、１．４５−トリフロロトリクロロエタン勿用
いて洗浄を行なった。洗浄上りのレンズは外観上例の変
化もなかつｔｏ
〔実施例５〕
インクロビルアルコールで洗浄さｆしたジエチレングリ
コールビス（アリルカーボネート）ＭレンズＩＩ−室温
で５分間、５％水酸化ナトリウム水溶液で処理上行い、
以下に述べるコーテイング液を、ディッピング法により
、液温５℃、引き上げ速度４０ Ｃ１ｎ／ ｍｉｎ
の条件で塗布し次。次に熱風乾燥炉中で８０℃で３０分
、１３０℃で２時間加熱硬化させた。[Example 4] The synthetic resin lens with the anti-reflection film before treatment obtained in Example 1 was placed in a vacuum chamber, and the ratio of argon to water was 1.
A mixed gas of 0:5 is placed in a vacuum chamber at a vacuum degree of 0:5. ITor
A strain called rl/C was used, and the atmosphere was made into plasma using a high frequency electric field of 1i56 MHz. Plasma output 1300W
Then, I performed IMt for 30 seconds. Thereafter, the lenses T and 9 were taken out from the vacuum chamber, and a 99.9% solution of 1-7 dichlorooctamethyltetrasiloxane was applied by a spray method.Temporary cleaning was performed using 1,45-trifluorotrichloroethane. [Example 5] Diethylene glycol bis(allyl carbonate) M lens II cleaned with Inclovir alcohol - treated with 5% aqueous sodium hydroxide solution for 5 minutes at room temperature. conduct,
The coating liquid described below was applied using a dipping method at a liquid temperature of 5°C and a pulling rate of 40 C1n/min.
Apply under the following conditions. Next, it was heated and cured in a hot air drying oven at 80°C for 30 minutes and at 130°C for 2 hours.
コーテイング液は次の様にして作成し友。The coating liquid is prepared as follows.
攪拌装置を備え九反応容器中にエタノール２０６部、エ
タノール分散コロイダルシリカ３９６部（触媒化成工業
株式会社製”オスカル１２３２”固形分５０％）、ｒ−
グリシドキシクロビルトリメトキシシランの部分加水分
解物 ３１２９．フローコントロール剤α２部（日本ユ
ニカー（切要″Ｌ−７６０４”）及びα０５Ｎ酢酸水溶
ｐｓｂ部を加え、罠温で３時間攪拌γし、コーテイング
液とした。In a nine reaction vessel equipped with a stirring device, 206 parts of ethanol, 396 parts of ethanol-dispersed colloidal silica (“Oscar 1232” manufactured by Catalysts & Chemicals Co., Ltd. solid content 50%), r-
Partial hydrolyzate of glycidoxyclobyltrimethoxysilane 3129. 2 parts of a flow control agent α (Nippon Unicar (Kiwaki "L-7604")) and 5 parts of α05N acetic acid aqueous solution PSB were added, and the mixture was stirred at trap temperature for 3 hours to obtain a coating liquid.
上記の似にして得ら九たレンズに実施例１と同様に反射
防止処理を行ない、その後同様にジメチルジクロルシラ
ン金柑いて処理した。洗浄上りの外貌に特に変化はみら
ｎなかった。A lens obtained in the same manner as above was subjected to antireflection treatment in the same manner as in Example 1, and then treated with dimethyldichlorosilane citrate in the same manner. No particular change was observed in the appearance after washing.
〔実施例６〕
実施例１で得られた処理前の反射防止膜つきレンズ七塩
化メチレンで洗浄し、ジビニルジクロロシラン９９．９
％溶液に２分間浸漬した。浸漬後、湿度６υチ、温度１
５℃中で５６ｎ／分の＠盆でレンズを引き上げ、塩化メ
チレン９９９％浴液により洗浄した。欠に洗浄されｔレ
ンズｉ ２ Ｎ Ｈ，Ｓｏ。[Example 6] The untreated lens with antireflection film obtained in Example 1 was washed with methylene heptachloride, and divinyldichlorosilane 99.9
% solution for 2 minutes. After soaking, humidity 6υ, temperature 1
The lens was pulled up in a tray at 56 n/min at 5°C and washed with a 999% methylene chloride bath. The lens i 2 NH, So was washed frequently.
中で６ｕ℃、１時間加熱処理し、ビニル基をヒドロキシ
エチル赫に変化させ友。処理後外観に変化はみられなか
った。Heat treatment was carried out at 6u℃ for 1 hour in a vacuum chamber to convert the vinyl group to hydroxyethyl chloride. No change in appearance was observed after treatment.
〔実施例７〕
実施例５で得られ九ジメチルジクロルシラン処理を行う
前の反射防止膜つきレンズｉアセトンで洗浄して真空槽
内にセットし、真空度αＩ Ｔｏｒｒ。[Example 7] The lens with the antireflection film obtained in Example 5 and before being treated with 9-dimethyldichlorosilane was cleaned with acetone and set in a vacuum chamber at a vacuum degree of αI Torr.
基＆温度５０℃となる様排気、加熱した。その後真空槽
内にジフェニルビニルクロロシランを、１ （Ｉ ｃｃ
／分の割合で真空槽内へ１分間導入し友。It was evacuated and heated to a temperature of 50°C. After that, diphenylvinylchlorosilane was added to the vacuum chamber at 1 (I cc
Introduce the sample into the vacuum chamber for 1 minute at a rate of 1 minute.
その後レンズを大気中に取り出し、テトラヒドロフラン
により洗浄上行なった。洗浄後のレンズを２Ｎ Ｈ，
Ｓｏ、中で５０℃、３０分間力Ω熱処理をし。Thereafter, the lens was taken out into the atmosphere and washed with tetrahydrofuran. Wash the lens with 2N H,
Heat treated in SO for 30 minutes at 50°C.
ビニル基七ヒドロキシエチル基に変化させ次。処理後の
レンズの外観に特別な異常は見られながった。Next, the vinyl group is changed to a heptahydroxyethyl group. No particular abnormality was observed in the appearance of the lens after treatment.
〔比較例１〕
実施例１で得られ比ジメチルジクロルシラン処理前の反
射防止つき合成樹脂製レンズを比較例１とし友。[Comparative Example 1] The antireflection synthetic resin lens obtained in Example 1 and before being treated with dimethyldichlorosilane was used as Comparative Example 1.
〔比較例２〕
実施例２で得られ次ジエチルジクロロシラン処理前の反
射防止膜つきクラウンガラスレンズを比較例２とした。[Comparative Example 2] Comparative Example 2 was a crown glass lens with an antireflection film obtained in Example 2 and before being treated with diethyldichlorosilane.
〔比較例３〕
実施例５で得ら九たジメチルジクロルシラン処理勿行う
前の反射防止膜っき合成樹脂製レンズを比較例５とし友
。[Comparative Example 3] Comparative Example 5 was an antireflection coated synthetic resin lens obtained in Example 5 before being treated with dimethyldichlorosilane.
実施例と比較例の評価結果はまとめて表１に示した。The evaluation results of Examples and Comparative Examples are summarized in Table 1.
無機コート膜に、ハロゲン化７ラン化合？！７を反応さ
せ比為に、無機コート、膜及び表面の親水性、疎水性な
どの特性が変化し、従って、ヤク現象の防止、膜の耐水
性、耐久性の同上、耐摩耗性の同上、曇りの防止など膜
特性が者しく向上するという効果が得られ比。A 7-ranium halide compound in the inorganic coating film? ! By reacting 7, the properties such as hydrophilicity and hydrophobicity of the inorganic coat, membrane and surface change, thus preventing the yak phenomenon, improving the water resistance and durability of the membrane, and improving the abrasion resistance. This has the effect of significantly improving film properties such as preventing fogging.
不発明は、合成樹脂製及びガラス製眼鏡レンズ、カメラ
レンズ、表示用パネル、時計用カバーガラス、窓ガラス
等無機コート膜を便角した製品に適用できる。The invention is applicable to products coated with inorganic coatings, such as synthetic resin and glass eyeglass lenses, camera lenses, display panels, watch cover glasses, and window glasses.
Claims (1)
ことを特徴とする無機コート膜の表面改質法。A method for surface modification of an inorganic coat film, characterized by reacting the inorganic coat film with a halogenated silane compound.
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61010468A JP2622541B2 (en) | 1986-01-21 | 1986-01-21 | Optical article manufacturing method |
| FR8700257A FR2598520B1 (en) | 1986-01-21 | 1987-01-13 | MINERAL PROTECTIVE FILM |
| DE19873701654 DE3701654A1 (en) | 1986-01-21 | 1987-01-21 | METHOD FOR TREATING INORGANIC COATINGS |
| JP5007901A JP2655036B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
| JP5007902A JP2812121B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
| US08/183,105 US5622784A (en) | 1986-01-21 | 1994-01-18 | Synthetic resin ophthalmic lens having an inorganic coating |
| US08/324,066 US5783299A (en) | 1986-01-21 | 1994-10-14 | Polarizer plate with anti-stain layer |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61010468A JP2622541B2 (en) | 1986-01-21 | 1986-01-21 | Optical article manufacturing method |
| JP5007901A JP2655036B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
| JP5007902A JP2812121B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
Related Child Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5007903A Division JPH05341108A (en) | 1993-01-20 | 1993-01-20 | Method for reforming surface of inorganic coat film |
| JP5007902A Division JP2812121B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
| JP5007901A Division JP2655036B2 (en) | 1986-01-21 | 1993-01-20 | Optical article manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62169102A true JPS62169102A (en) | 1987-07-25 |
| JP2622541B2 JP2622541B2 (en) | 1997-06-18 |
Family
ID=27277794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61010468A Expired - Lifetime JP2622541B2 (en) | 1986-01-21 | 1986-01-21 | Optical article manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2622541B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63240504A (en) * | 1987-03-27 | 1988-10-06 | Sharp Corp | Preparation of thin dielectric optical film |
| JPH05341108A (en) * | 1993-01-20 | 1993-12-24 | Seiko Epson Corp | Method for reforming surface of inorganic coat film |
| JPH05341107A (en) * | 1986-01-21 | 1993-12-24 | Seiko Epson Corp | Optical material having inorganic coat film |
| US5759643A (en) * | 1987-01-16 | 1998-06-02 | Seiko Epson Corporation | Polarizing plate and method of production |
| WO2019189071A1 (en) * | 2018-03-26 | 2019-10-03 | 日本電気硝子株式会社 | Substrate with anti-glare film, laminate, and laminate production method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS511387A (en) * | 1974-05-23 | 1976-01-08 | Canon Kk | |
| JPS58172245A (en) * | 1982-04-02 | 1983-10-11 | Asahi Glass Co Ltd | Surface treating agent for glass |
| JPS61130902A (en) * | 1984-11-30 | 1986-06-18 | Asahi Glass Co Ltd | Plastic lens with antireflective film and capable of easy removal of stain |
-
1986
- 1986-01-21 JP JP61010468A patent/JP2622541B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS511387A (en) * | 1974-05-23 | 1976-01-08 | Canon Kk | |
| JPS58172245A (en) * | 1982-04-02 | 1983-10-11 | Asahi Glass Co Ltd | Surface treating agent for glass |
| JPS61130902A (en) * | 1984-11-30 | 1986-06-18 | Asahi Glass Co Ltd | Plastic lens with antireflective film and capable of easy removal of stain |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05341107A (en) * | 1986-01-21 | 1993-12-24 | Seiko Epson Corp | Optical material having inorganic coat film |
| US5759643A (en) * | 1987-01-16 | 1998-06-02 | Seiko Epson Corporation | Polarizing plate and method of production |
| JPS63240504A (en) * | 1987-03-27 | 1988-10-06 | Sharp Corp | Preparation of thin dielectric optical film |
| JPH0529083B2 (en) * | 1987-03-27 | 1993-04-28 | Sharp Kk | |
| JPH05341108A (en) * | 1993-01-20 | 1993-12-24 | Seiko Epson Corp | Method for reforming surface of inorganic coat film |
| WO2019189071A1 (en) * | 2018-03-26 | 2019-10-03 | 日本電気硝子株式会社 | Substrate with anti-glare film, laminate, and laminate production method |
| JPWO2019189071A1 (en) * | 2018-03-26 | 2021-04-01 | 日本電気硝子株式会社 | Substrate with anti-glare film, laminate, and method for manufacturing laminate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2622541B2 (en) | 1997-06-18 |
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| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |