JP3597213B2 - Method of forming water-repellent coating - Google Patents
Method of forming water-repellent coating Download PDFInfo
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- JP3597213B2 JP3597213B2 JP30782293A JP30782293A JP3597213B2 JP 3597213 B2 JP3597213 B2 JP 3597213B2 JP 30782293 A JP30782293 A JP 30782293A JP 30782293 A JP30782293 A JP 30782293A JP 3597213 B2 JP3597213 B2 JP 3597213B2
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Description
【０００１】
【産業上の利用分野】
本発明は自動車ガラスなどの透明基板の表面に撥水被膜を形成する方法に関する。
【０００２】
【従来の技術】
ポリジメチルシロキサンやポリフルオロアルキル基を含有した溶液をガラス板の表面に塗布し、これを乾燥した後に焼成することで付着した水滴の接触角を大きくする撥水被膜とすることが従来から行われており、斯かる撥水被膜に関する先行技術として、特開平４−３３８１３７号公報、特開平４−３５９０８６号公報、特開平５−２４８８５号公報或いは特開平５−２４８８６号公報に開示されるものが知られている。
【０００３】
特開平４−３３８１３７号公報にはシリコーン系撥水被膜に代るものとして、ＳiＯ２を主成分とするセラミックスの非金属原子の一部をフルオロアルキル基で置換したものが開示され、、特開平４−３５９０８６号公報には金属アルコキシドを含むビヒクルに所定量のフルオロアルキルシラン或いはアルキルシランを混合したものが開示され、特開平５−２４８８５号公報にはガラス表面と撥水被膜との間に透明金属皮膜を介在させたものが開示され、特開平５−２４８８６号公報にはガラス表面にＳiＯ２膜を形成し、このＳiＯ２膜の表面に凹凸を形成し、その上に撥水被膜を形成することが開示されている。
【０００４】
そして、上述した先行技術にあっては、撥水被膜形成用の塗布溶液をガラス表面に塗布した後に乾燥し、その後焼成することで撥水被膜としており、塗布方法としてはディッピング法、スプレー法、スピンコート法が開示されている。
【０００５】
ディッピング法は撥水被膜形成用の塗布溶液中にガラス基板を浸漬して塗布する方法であり、この方法では多量の塗布溶液が必要になり、塗布溶液が汚れた場合には多量の塗布溶液を交換しなければならず、片面のみ撥水加工が必要でも両面に撥水被膜が形成されてしまい、これを避けるべく片面にマスクを被せた状態でディッピングしてもガラス板が湾曲しているとマスクにシワがより、シワの部分から塗布液が滲み込んでしまう。
【０００６】
スプレー法は塗布ガンを用い雰霧状にしてガラス板に塗布する方法であり、この方法による場合には、膜厚分布が不均一になる不利がある。また、スピンコート法はガラス板上に塗布液を滴下するとともにガラス板を高速で回転させ、遠心力でガラス板表面に塗布液を均一に拡散せしめる方法であるが、自動車用ガラス等は大型で、高速で回転せしめることはできず、膜厚も不均一でしかも薄くできない。
【０００７】
また上記のディッピング法、スプレー法及びスピンコート法の欠点を解消できる方法として、図２に示すように上下方向に保持したガラス基板１の上縁にノズル２を用いて塗布溶液３を流し出すフロー法がある。
【０００８】
【発明が解決しようとする課題】
フロー法によると、使用する塗布液の量も比較的少なくて済み、且つ膜厚も均一にできるのであるが、図２にも示すようにガラス板１の非塗布面側の下縁に塗布液の廻り込み部４が生じる。そして、この廻り込み部４と非塗布部との境界部が目立つ不利がある。
【０００９】
【課題を解決するための手段】
上記課題を解決すべく本発明は、請求項１は、ガラス板などの透明基板を上下方向に保持し、この透明基板の一面の上縁にノズルを用いて撥水被膜となる塗布溶液を流し出し、次いで塗布溶液を乾燥せしめ、この後焼成することで撥水被膜を形成する方法において、前記透明基板の塗布溶液が塗布される面と反対側の面の下縁には塗布に先立って予め別の撥水被膜が形成され、前記透明基板の下縁に予め形成する撥水被膜の幅は２０ｍｍ以上６０ｍｍ以下とすることを特徴とする。
撥水皮膜の幅が２０ｍｍ未満であると、完全に廻り込みをカバーできず、６０ｍｍを超えて設けても無駄になるからである。また６０ｍｍを超えて設けるとこの部分は従来シール等を貼着していた部分であり、撥水被膜はシール等を貼着しにくくする不利もある。請求項１では撥水被膜の幅は２０ｍｍ以上６０ｍｍ以下としたので、透明基板の下縁に予め形成する撥水被膜の境界部が目立つおそれもあるが、これにより目立つのを防止できる。
【００１０】
請求項２は、ガラス板などの透明基板を上下方向に保持し、この透明基板の一面の上縁にノズルを用いて撥水被膜となる塗布溶液を流し出し、次いで塗布溶液を乾燥せしめ、この後焼成することで撥水被膜を形成する方法において、前記透明基板の塗布溶液が塗布される面と反対側の面の下縁には塗布に先立って予め別の撥水被膜が形成され、前記透明基板の下縁に予め形成する撥水被膜は非塗布部との境界部においてその厚みが連続的に変化していることを特徴とする。
撥水皮膜は、非塗布部との境界部においてその厚みが連続的に変化しているので、撥水被膜と非塗布部との境界部が目立たなくすることができる。
【００１１】
請求項３は、請求項１又は請求項２において、前記透明基板の下縁に予め形成する撥水被膜の厚さは１５０Å以上３００Å以下とすることを特徴とする。
撥水皮膜の厚さが１５０Å未満であると撥水機能が十分に発揮されず、３００Åを超えると、干渉領域の厚みになり非塗布部との境界部が目立つ。
尚、膜厚の調整は塗布液の濃度を希釈することで行う。つまり、溶媒の量を増やすと形成される膜厚は薄くなる。
【００１２】
請求項４は、請求項１に記載の撥水被膜の形成方法において、前記透明基板の下縁に予め形成する撥水被膜は非塗布部との境界部においてその厚みが連続的に変化していることを特徴とする。
請求項１の作用、効果とともに、撥水被膜の厚みが連続的に変化するので、撥水被膜と非塗布部との境界部を目立たない。
【００１３】
請求項５は、請求項１乃至請求項４の何れかに記載の撥水被膜の形成方法において、前記撥水被膜形成用の塗布溶液はテトラエトキシシラン及びフルオロアルキルシランを含むことを特徴とする。
本発明の撥水被膜形成用の塗布液は、Ｓ i Ｏ ２ を５０％以上含むセラミックスの非金属原子の一部がフルオロアルキル基に置換されたものである。更にガラス基板としては、珪酸ガラス、珪酸アルカリガラス、鉛アルカリガラス、ソーダ石灰ガラス、カリ石灰ガラス、バリウムガラス等の珪酸塩ガラス、Ｂ ２ Ｏ ３ 及びＳ i Ｏ ２ を含有するほう珪酸ガラス、Ｐ ２ Ｏ ５ を含有するリン酸塩ガラスなどから選択することができる。またガラス板の代りに透明樹脂板を用いることも可能である。
【００１４】
【作用】
塗布液の廻り込みが生じる部分に予め別の撥水被膜を形成しておくことで、廻り込みがなくなる。
【００１５】
【実施例】
本発明に係る撥水被膜の形成方法は塗布溶液の調製工程、廻り込み防止処理工程、塗布工程及び焼成工程に大別される。以下に各工程毎に説明する。
【００１６】
（調製工程）
以下の（ａ）〜（ｃ）を２０分間攪拌する。
【００１７】
（廻り込み防止処理工程）
上記によって調製した塗布溶液を更にエタノールで４倍に希釈（５％溶液）し、この希釈溶液を図１に示すようにガラス板１の非塗布面の下縁に３０ｍｍ幅で塗布した。塗布方法は布を用いた手塗りとした。
この後、Ｃe２Ｏ３（セリコ）で洗浄した後、純水でリンスし、エアーナイフにて乾燥させて撥水被膜５を形成した。
【００１８】
（塗布工程）
上記で得られた塗布溶液をフロー法にてガラス板の片面に塗布する。フロー法はガラス板１を上下方向に保持した状態で、ガラス板１の上縁部にノズル２を用いて塗布溶液３を２００ｃｃ／ｍｉｎの供給量で流し出すことで行う。
塗布液を塗布したら、乾燥室の条件を温度２１℃、湿度１８％、風速分布０．３ｍ／ｍｉｎ〜０．５ｍ／ｍｉｎとして乾燥せしめた。これによりガラス板表面にウェット膜が形成される。
【００１９】
（焼成工程）
上記のウェット膜を形成したガラス板を大気中で１２０℃、２０分間保持して水及びエタノールを蒸発させ、更に２５０℃に昇温し、１時間保持することで撥水被膜を形成した。
【００２０】
【発明の効果】
以上に説明したように本発明によれば、フロー法にて撥水被膜形成用の塗布液をガラス板等の透明基板に塗布するにあたり、前記透明基板の塗布溶液が塗布される面と反対側の面の下縁に塗布に先立って予め別の撥水被膜を形成しておき、透明基板の下縁に予め形成する撥水被膜の幅を２０ｍｍ以上６０ｍｍ以下とし、或いは透明基板の下縁に予め形成する撥水被膜は非塗布部との境界部においてその厚みが連続的に変化させるようにしたので、廻り込みがなくなり、廻り込んだ塗布液の境界部が目立つことがなくなる。
【００２１】
また、透明基板の下縁に予め形成する撥水被膜の境界部が目立つおそれもあるが、これは予め形成する撥水被膜の厚さを１５０Å以上３００Å以下とするか、幅を２０ｍｍ〜６０ｍｍとするか、境界部における撥水被膜の厚さを連続的に変化させることで防止できる。
【図面の簡単な説明】
【図１】本発明方法を説明する図
【図２】従来方法を説明する図
【符号の説明】
１…ガラス板、２…ノズル、３…塗布液、４…廻り込み部、５…予め形成する撥水被膜。[0001]
[Industrial applications]
The present invention relates to a method for forming a water-repellent coating on a surface of a transparent substrate such as an automobile glass.
[0002]
[Prior art]
Conventionally, a solution containing polydimethylsiloxane or a polyfluoroalkyl group is applied to the surface of a glass plate, dried, and then fired to form a water-repellent coating that increases the contact angle of attached water droplets. As a prior art relating to such a water-repellent coating, those disclosed in JP-A-4-338137, JP-A-4-359086, JP-A-5-24885 or JP-A-5-24886 are disclosed. Are known.
[0003]
Japanese Patent Application Laid-Open No. 4-338137 discloses a ceramic having SiO 2 as a main component in which some nonmetallic atoms are substituted with a fluoroalkyl group as an alternative to the silicone-based water-repellent coating. JP-A-4-359086 discloses a mixture containing a predetermined amount of fluoroalkylsilane or alkylsilane in a vehicle containing a metal alkoxide, and JP-A-5-24885 discloses a transparent material between a glass surface and a water-repellent coating. Japanese Patent Application Laid-Open No. Hei 5-24886 discloses a technique in which a metal film is interposed. An SiO 2 film is formed on a glass surface, irregularities are formed on the surface of the SiO 2 film, and a water-repellent film is formed thereon. Is disclosed.
[0004]
And, in the above-mentioned prior art, a coating solution for forming a water-repellent film is applied to a glass surface, then dried, and then baked to form a water-repellent film. As a coating method, a dipping method, a spray method, A spin coating method is disclosed.
[0005]
The dipping method is a method in which a glass substrate is immersed in a coating solution for forming a water-repellent film and coating is performed.In this method, a large amount of the coating solution is required. It is necessary to replace it, and even if water repellent processing is necessary only on one side, a water repellent coating is formed on both sides, and if the glass plate is curved even if dipping with a mask on one side to avoid this The coating liquid oozes from the wrinkled portion of the mask.
[0006]
The spraying method is a method of applying an atmosphere to a glass plate using a coating gun, and has a disadvantage that the film thickness distribution is not uniform. The spin coating method is a method in which a coating liquid is dropped onto a glass plate and the glass plate is rotated at a high speed so that the coating liquid is uniformly diffused on the surface of the glass plate by centrifugal force. , Cannot be rotated at high speed, and the film thickness is not uniform and cannot be reduced.
[0007]
As a method for solving the drawbacks of the dipping method, the spraying method and the spin coating method, as shown in FIG. 2, a flow in which a coating solution 3 is poured using a nozzle 2 to the upper edge of a
[0008]
[Problems to be solved by the invention]
According to the flow method, the amount of the coating liquid to be used can be relatively small and the film thickness can be made uniform. However, as shown in FIG. Wraparound
[0009]
[Means for Solving the Problems]
In order to solve the above-mentioned problems, the present invention is directed to claim 1, wherein a transparent substrate such as a glass plate is vertically held, and a coating solution to be a water-repellent film is flowed on an upper edge of one surface of the transparent substrate using a nozzle. In the method of forming a water-repellent film by drying the coating solution and then baking it, the lower edge of the transparent substrate opposite to the surface on which the coating solution is coated is preliminarily coated before coating. Another water-repellent coating is formed, and the width of the water-repellent coating formed in advance on the lower edge of the transparent substrate is 20 mm or more and 60 mm or less.
If the width of the water-repellent film is less than 20 mm, it is impossible to completely cover the wraparound, and even if the width exceeds 60 mm, it is useless. Further, if it is provided over 60 mm, this portion is a portion to which a seal or the like has been pasted, and the water-repellent coating has a disadvantage that it is difficult to stick the seal or the like. In the first aspect, since the width of the water-repellent film is set to 20 mm or more and 60 mm or less, the boundary of the water-repellent film formed in advance on the lower edge of the transparent substrate may be conspicuous, but this can be prevented.
[0010]
Claim 2 holds a transparent substrate such as a glass plate in the up and down direction, flows out a coating solution to be a water-repellent film using a nozzle on the upper edge of one surface of the transparent substrate, and then dries the coating solution. In the method of forming a water-repellent film by post-baking, another water-repellent film is formed in advance on the lower edge of the surface opposite to the surface of the transparent substrate on which the coating solution is applied, prior to application, The water-repellent film formed in advance on the lower edge of the transparent substrate is characterized in that its thickness continuously changes at the boundary with the non-coated portion.
Since the thickness of the water-repellent film continuously changes at the boundary with the non-coated portion, the boundary between the water-repellent coating and the non-coated portion can be made inconspicuous.
[0011]
Claim 3, in
If the thickness of the water-repellent film is less than 150 °, the water-repellent function is not sufficiently exhibited, and if it exceeds 300 °, the thickness of the interference region becomes large and the boundary with the non-coated portion is conspicuous.
The thickness is adjusted by diluting the concentration of the coating solution. That is, when the amount of the solvent is increased, the formed film thickness is reduced.
[0012]
According to a fourth aspect of the present invention, in the method for forming a water-repellent coating according to the first aspect, the thickness of the water-repellent coating formed in advance on the lower edge of the transparent substrate changes continuously at a boundary with the non-coated portion. It is characterized by having.
Since the thickness of the water-repellent coating changes continuously with the operation and effect of the first aspect, the boundary between the water-repellent coating and the non-coated portion is not noticeable.
[0013]
According to a fifth aspect of the present invention, in the method for forming a water-repellent film according to any one of the first to fourth aspects, the coating solution for forming the water-repellent film includes tetraethoxysilane and fluoroalkylsilane. You.
Coating solution for water repellent coating formed of the present invention, a portion of non-metallic atoms of ceramics containing S i O 2 50% or more is replaced with a fluoroalkyl group. Furthermore as the glass substrate is silicate glass, silicate alkali glass, lead alkali glass, soda lime glass, potash lime glass, silicate glass such as barium glass, B 2 O 3 and silicate glasses should contain S i O 2, P It can be selected from phosphate glass containing 2 O 5 and the like. It is also possible to use a transparent resin plate instead of a glass plate.
[0014]
[Action]
By forming another water-repellent coating in advance on the portion where the coating liquid is sneaked, the sneaking is eliminated.
[0015]
【Example】
The method for forming a water-repellent film according to the present invention is roughly classified into a coating solution preparation step, a wraparound prevention step, a coating step, and a baking step. Hereinafter, each step will be described.
[0016]
(Preparation process)
The following (a) to (c) are stirred for 20 minutes.
[0017]
(Wrap-around prevention process)
The coating solution prepared as described above was further diluted 4-fold with ethanol (5% solution), and this diluted solution was applied to the lower edge of the non-coated surface of the
Thereafter, the substrate was washed with Ce 2 O 3 (celico), rinsed with pure water, and dried with an air knife to form a water-repellent coating 5.
[0018]
(Coating process)
The coating solution obtained above is applied to one surface of a glass plate by a flow method. The flow method is performed by flowing the coating solution 3 at a supply rate of 200 cc / min to the upper edge of the
After the application of the coating solution, drying was performed under the conditions of a drying chamber at a temperature of 21 ° C., a humidity of 18%, and a wind speed distribution of 0.3 to 0.5 m / min. Thereby, a wet film is formed on the surface of the glass plate.
[0019]
(Baking process)
The glass plate on which the above-mentioned wet film was formed was kept at 120 ° C. for 20 minutes in the atmosphere to evaporate water and ethanol. The temperature was further raised to 250 ° C., and kept for 1 hour to form a water-repellent coating.
[0020]
【The invention's effect】
As described above, according to the present invention, when a coating solution for forming a water-repellent film is applied to a transparent substrate such as a glass plate by a flow method, the side opposite to the surface of the transparent substrate to which the coating solution is applied. Prior to application, another water-repellent coating is formed in advance on the lower edge of the surface, and the width of the water-repellent coating previously formed on the lower edge of the transparent substrate is set to 20 mm or more and 60 mm or less, or to the lower edge of the transparent substrate. Since the thickness of the previously formed water-repellent coating is continuously changed at the boundary with the non-coated portion, the coating does not wrap around, and the boundary of the coating liquid that has wrapped around does not stand out.
[0021]
In addition, the boundary of the water-repellent coating formed in advance on the lower edge of the transparent substrate may be conspicuous. This is because the thickness of the water-repellent coating formed in advance is set to be 150 to 300 mm, or the width is set to 20 mm to 60 mm. Alternatively, it can be prevented by continuously changing the thickness of the water-repellent coating at the boundary.
[Brief description of the drawings]
FIG. 1 is a diagram for explaining a method of the present invention. FIG. 2 is a diagram for explaining a conventional method.
DESCRIPTION OF
Claims (5)
前記透明基板の塗布溶液が塗布される面と反対側の面の下縁には塗布に先立って予め別の撥水被膜が形成され、
前記透明基板の下縁に予め形成する撥水被膜の幅は２０ｍｍ以上６０ｍｍ以下とする、
ことを特徴とする撥水被膜の形成方法。A transparent substrate such as a glass plate is held up and down, a coating solution to be a water-repellent coating is poured out using a nozzle on the upper edge of one surface of the transparent substrate, and then the coating solution is dried and then fired. In the method of forming a water-repellent coating ,
Another water repellent film advance prior to coating is formed on the lower edge side of the surface where the coating solution before Symbol transparent substrate is applied the opposite side,
The width of the water-repellent coating formed in advance on the lower edge of the transparent substrate is 20 mm or more and 60 mm or less,
Method of forming a water-repellent coating, characterized in and this.
前記透明基板の塗布溶液が塗布される面と反対側の面の下縁には塗布に先立って予め別の撥水被膜が形成され、
前記透明基板の下縁に予め形成する撥水被膜は非塗布部との境界部においてその厚みが連続的に変化している、
ことを特徴とする撥水被膜の形成方法。 A transparent substrate such as a glass plate is held up and down, a coating solution to be a water-repellent coating is poured out using a nozzle on the upper edge of one surface of the transparent substrate, and then the coating solution is dried and then fired. In the method of forming a water-repellent coating,
Another water-repellent coating is formed in advance on the lower edge of the surface opposite to the surface on which the coating solution of the transparent substrate is applied, prior to application,
The water-repellent coating formed in advance on the lower edge of the transparent substrate has its thickness continuously changed at the boundary with the non-coated portion,
Method of forming a water-repellent coating, characterized in and this.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30782293A JP3597213B2 (en) | 1993-12-08 | 1993-12-08 | Method of forming water-repellent coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30782293A JP3597213B2 (en) | 1993-12-08 | 1993-12-08 | Method of forming water-repellent coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07157749A JPH07157749A (en) | 1995-06-20 |
| JP3597213B2 true JP3597213B2 (en) | 2004-12-02 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30782293A Expired - Fee Related JP3597213B2 (en) | 1993-12-08 | 1993-12-08 | Method of forming water-repellent coating |
Country Status (1)
| Country | Link |
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| JP (1) | JP3597213B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007176443A (en) * | 2005-12-28 | 2007-07-12 | Nippon Sheet Glass Co Ltd | Vehicular window glass and manufacturing method thereof |
| JP4933780B2 (en) | 2006-01-17 | 2012-05-16 | 日本板硝子株式会社 | WINDOW GLASS AND MANUFACTURING METHOD THEREOF |
| JP5494254B2 (en) * | 2010-06-07 | 2014-05-14 | 旭硝子株式会社 | Manufacturing method of automotive window glass with coating |
| JP2015085215A (en) * | 2013-10-28 | 2015-05-07 | 株式会社イーコートジャパン | Coating method of light transmitting plate |
-
1993
- 1993-12-08 JP JP30782293A patent/JP3597213B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07157749A (en) | 1995-06-20 |
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