JPH03242351A - Production of water repellent glass - Google Patents
Production of water repellent glassInfo
- Publication number
- JPH03242351A JPH03242351A JP3672890A JP3672890A JPH03242351A JP H03242351 A JPH03242351 A JP H03242351A JP 3672890 A JP3672890 A JP 3672890A JP 3672890 A JP3672890 A JP 3672890A JP H03242351 A JPH03242351 A JP H03242351A
- Authority
- JP
- Japan
- Prior art keywords
- water repellent
- water
- repellent
- solution
- glass substrate
- 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
- 239000005871 repellent Substances 0.000 title claims abstract description 70
- 239000011521 glass Substances 0.000 title claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 230000002940 repellent Effects 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 43
- 238000000576 coating method Methods 0.000 claims abstract description 43
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 13
- 238000007598 dipping method Methods 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 abstract description 6
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 6
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 5
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- -1 polydimethylsiloxane Polymers 0.000 description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
Abstract
Description
【発明の詳細な説明】
U産業上の利用分野]
本発明は、車両など使用される撥水性ガラスの製造方法
に関する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Use] The present invention relates to a method for manufacturing water-repellent glass used in vehicles and the like.
[従来の技術]
従来、撥水剤のシリコーン系重合体をガラス基板に塗布
する方法として、撥水剤溶液にガラス基板を浸漬する方
法が塗布膜の膜厚を一定に制御しやすいため広くおこな
われている。たとえば、特開平1−126244号公報
には、ポリジメチルシロキサンを室温で液状の炭化水素
に溶解した溶液にガラス基板を浸漬し、引き上げた後、
熱処理により硬化させて撥水皮膜を形成する撥水性ガラ
スの製造方法が開示されている。[Prior Art] Conventionally, as a method for applying silicone-based water repellent polymers to glass substrates, the method of immersing the glass substrate in a water repellent solution has been widely used because it is easy to control the thickness of the coating film at a constant level. It is. For example, in Japanese Patent Application Laid-open No. 1-126244, a glass substrate is immersed in a solution of polydimethylsiloxane dissolved in a liquid hydrocarbon at room temperature, and then pulled up.
A method for producing water-repellent glass is disclosed, which is cured by heat treatment to form a water-repellent film.
しかしながら上記の方法では、炭化水素の溶液が疎水性
のため極性の高いガラスに対する濡れ性が悪くガラス基
板の表面に均一な塗布が困難な場合が多い。また、撥水
性を高めるために高重合度のシリコーン系重合体を用い
ると、重合体の粘度が高くこれを溶解した溶液では粘度
が上昇するため形成される塗布膜は膜厚が一層不均一に
なりやすい。したがって浸漬を繰返したり、また膜厚を
均一に形成するためにワイピングなどで調整しなければ
ならず、工程も煩雑となり好ましくない。However, in the above method, since the hydrocarbon solution is hydrophobic, it has poor wettability to highly polar glass, and it is often difficult to uniformly coat the surface of the glass substrate. Additionally, when a silicone-based polymer with a high degree of polymerization is used to increase water repellency, the viscosity of the polymer is high and the viscosity of a solution in which it is dissolved increases, making the coating film formed even more uneven in thickness. Prone. Therefore, it is necessary to repeat dipping or adjust the film thickness by wiping or the like in order to form a uniform film thickness, making the process complicated and undesirable.
一方、ガラス基板と濡れ性の良い極性の溶媒では撥水剤
が溶解しないため塗布用の溶媒として使用できない。On the other hand, polar solvents that have good wettability with glass substrates cannot be used as coating solvents because they do not dissolve the water repellent.
[発明が解決しようとする課題]
そこで本発明は炭化水素などの疎水性の溶媒に溶解され
たシリコーン系の撥水剤を、ガラス基板の表面に均一に
塗布することを目的とする。[Problems to be Solved by the Invention] Therefore, an object of the present invention is to uniformly apply a silicone-based water repellent dissolved in a hydrophobic solvent such as a hydrocarbon to the surface of a glass substrate.
[課題を解決するための手段]
本発明の撥水性ガラスの製造方法は、シリコーン系の撥
水剤を溶解した撥水剤溶液にガラス基板を浸漬させて表
面に撥水剤塗膜を形成し、次いで該撥水剤塗膜を加熱硬
化させて撥水皮膜をガラス基板上に形成する撥水性ガラ
スの製造方法において、該撥水剤塗膜の塗布時に該撥水
剤溶液に超音波振動を加えながら該ガラス基板を浸漬し
て撥水剤塗膜を形成することを特徴とする。[Means for Solving the Problems] The method for producing water-repellent glass of the present invention involves immersing a glass substrate in a water-repellent solution in which a silicone-based water repellent is dissolved to form a water-repellent coating on the surface. In a method for producing water-repellent glass, the water-repellent coating film is then heated and cured to form a water-repellent film on a glass substrate, in which ultrasonic vibration is applied to the water-repellent solution during application of the water-repellent coating film. The water repellent coating film is formed by immersing the glass substrate while adding water repellent.
本発明の特徴は、撥水剤を溶解した塗布溶液に超音波振
動を加えながら、その溶液中にガラス基板を浸漬するこ
とにより均一で接着性に優れた撥水皮膜をガラス基板上
に形成することにある。The feature of the present invention is to form a uniform and highly adhesive water-repellent film on a glass substrate by immersing the glass substrate in a coating solution containing a water-repellent agent while applying ultrasonic vibrations to the solution. There is a particular thing.
塗布溶液に超音波振動が加えられると、溶液が局部的に
高温、高圧になり大きなエネルギーが付与されて浸漬さ
れたガラス面に衝突するようになる。ガラス面ではこの
高エネルギー溶液の衝突により、溶液中に存在する撥水
剤がガラス面に付着固定され濡れ性の悪い溶液中でも均
一に塗布することができる。その結果、ガラス面には均
一な塗布膜が形成できる。When ultrasonic vibrations are applied to the coating solution, the solution locally becomes high temperature and high pressure, and a large amount of energy is applied to the solution, causing it to collide with the immersed glass surface. Due to the collision of this high-energy solution on the glass surface, the water repellent present in the solution is adhered and fixed to the glass surface, and even a solution with poor wettability can be uniformly applied. As a result, a uniform coating film can be formed on the glass surface.
塗布溶液に加える超音波振動は、10〜50KH7の範
囲であると短時間で均一な塗布膜が形成できるので好ま
しい。The ultrasonic vibration applied to the coating solution is preferably in the range of 10 to 50 KH7 because a uniform coating film can be formed in a short time.
撥水剤としてはシリコーン系のポリジメチルシロキサン
、ポリジフェニルシロキサン、ポリフェニルメチルシロ
キサンなどが使用できる。As the water repellent, silicone-based polydimethylsiloxane, polydiphenylsiloxane, polyphenylmethylsiloxane, etc. can be used.
この方法によれば粘度が10〜1000万CSの様な高
い重合度の撥水剤でも均一に塗布することができる。According to this method, even a water repellent having a high degree of polymerization such as a viscosity of 10 to 10 million CS can be uniformly applied.
溶媒としては撥水性剤が溶解できるものであれば利用で
きる。たとえば、炭化水素系のへキサン、ヘプタン、オ
クタン、トルエン、バンゼンなどが使用できる。撥水剤
は溶媒に、1〜10重量%の濃度に溶解されて使用する
のが好ましい。浸漬法では通常撥水剤の溶液濃度を調整
して塗布膜の膜厚をコントロールすることができる。し
たがって本発明においても膜厚の調整が容易である。Any solvent that can dissolve the water repellent agent can be used. For example, hydrocarbons such as hexane, heptane, octane, toluene, and banzene can be used. The water repellent is preferably used dissolved in a solvent at a concentration of 1 to 10% by weight. In the dipping method, the thickness of the coating film can usually be controlled by adjusting the concentration of the water repellent solution. Therefore, also in the present invention, the film thickness can be easily adjusted.
塗布後、浸漬溶液から引上げられたガラス基板は、乾燥
して溶媒を除去した後、加熱して塗布膜を硬化させる。After coating, the glass substrate is pulled up from the dipping solution, dried to remove the solvent, and then heated to harden the coating film.
この場合塗布膜はガラス面から硬化を始める。硬化後の
硬化皮膜の上面には、未硬化部分が残存している場合に
は、未硬化部分を前記の溶媒を用いて完全に拭き取り所
定の膜厚の撥水皮膜とすることができる。In this case, the coating film begins to harden from the glass surface. If an uncured portion remains on the upper surface of the cured film after curing, the uncured portion can be completely wiped off using the above-mentioned solvent to form a water-repellent film of a predetermined thickness.
[作用]
本発明の方法によれば、撥水剤の塗布溶液に超音波振動
を加えながらガラス基板が浸漬される。[Operation] According to the method of the present invention, a glass substrate is immersed in a water repellent coating solution while applying ultrasonic vibrations.
そのため塗布用液は超音波により振動しキャビテーショ
ンが起こると溶液が局部的に高温、高圧になり大きなエ
ネルギーをもってガラス面に衝突するようになる。また
ガラスへの衝突回数も増加するため溶液中に溶解してい
る撥水剤のガラス面への付着が容易になるとともに塗布
膜の接着性も高まり均一に塗布される。Therefore, when the coating liquid is vibrated by ultrasonic waves and cavitation occurs, the solution becomes locally high in temperature and pressure, and collides with the glass surface with a large amount of energy. Furthermore, since the number of collisions with the glass increases, the water repellent dissolved in the solution easily adheres to the glass surface, and the adhesion of the coating film increases, allowing it to be applied uniformly.
したがって炭化水素などのガラス面に対して濡れ性の悪
い塗布溶液や粘度の高い撥水剤を用いても均一に塗布す
ることができる。そのため得られる塗布膜を硬化して形
成される撥水皮膜も均一となり、むらのない撥水性ガラ
スとなる。さらにこの方法で形成した撥水皮膜は、従来
法の浸漬で形成した場合よりも接着性がよく硬化皮膜の
耐久性が高まり撥水性を向上させることができる。Therefore, it is possible to uniformly coat a glass surface using a coating solution made of hydrocarbon or the like having poor wettability or a water repellent having high viscosity. Therefore, the water-repellent film formed by curing the obtained coating film is also uniform, resulting in water-repellent glass with no unevenness. Furthermore, the water-repellent film formed by this method has better adhesion than that formed by conventional dipping, and the cured film has increased durability and water repellency can be improved.
[実施例] 以下、実施例により具体的に説明する。[Example] Hereinafter, this will be explained in detail using examples.
ガラス基板(70xl 50xt 3.1mm)の表面
を研磨用のコンパウンド入りクリーナで研磨、洗浄した
。The surface of a glass substrate (70xl 50xt 3.1 mm) was polished and cleaned using a cleaner containing a polishing compound.
撥水剤の塗布液は、粘度が10〜1000万C5のポリ
ジメチルシロキサンをn−ヘキサンで1〜10重量%に
稀釈して調整した。The water repellent coating solution was prepared by diluting polydimethylsiloxane having a viscosity of 10 to 10 million C5 with n-hexane to 1 to 10% by weight.
超音波発振装置としては、市販の超音波洗浄器の振動子
に外部の高周波発振機よりO〜50KH7の高周波を加
えられるように改良し、浸漬用容器内に配置して超音波
を塗布溶液に加えるようにした。As an ultrasonic oscillator, we modified the vibrator of a commercially available ultrasonic cleaner to be able to apply high frequencies of 0 to 50KH7 from an external high-frequency oscillator, and placed it in a dipping container to apply ultrasonic waves to the coating solution. I added it.
上記の1〜10重量%の濃度の塗布液の中に上記のガラ
ス基板を浸漬し、10〜50KH2の超音波振動を1分
間加えた。その俊、溶液の液面の振動がなくなるまで静
置してからガラス基板を引き上げた。このガラス基板を
乾燥炉にて70℃で15分間乾燥して溶媒を除去した。The above glass substrate was immersed in the above coating solution having a concentration of 1 to 10% by weight, and ultrasonic vibrations of 10 to 50 KH2 were applied for 1 minute. The glass substrate was then pulled up after the solution was allowed to stand until the vibrations on the surface of the solution stopped. This glass substrate was dried in a drying oven at 70° C. for 15 minutes to remove the solvent.
次いで300℃で20分間加熱して塗布皮膜を硬化させ
た。その後硬化皮膜の表面に残存する未硬化部分をヘキ
サンが含浸された布で拭き取った。The coated film was then cured by heating at 300° C. for 20 minutes. Thereafter, the uncured portion remaining on the surface of the cured film was wiped off with a cloth impregnated with hexane.
得られた撥水皮膜の接触角は、膜全面の平均で95〜1
00’で良好な撥水性を示した。The contact angle of the obtained water-repellent film was 95 to 1 on average over the entire surface of the film.
00' showed good water repellency.
一方、同じ塗布液を用いて超音波振動を加えないで浸漬
塗布した以外は同一の条件で硬化させた場合では、撥水
皮膜の接触角が60〜90’で小さく不均一でおった。On the other hand, when cured under the same conditions except that the same coating solution was used and dip coating was performed without applying ultrasonic vibration, the contact angle of the water-repellent film was small and non-uniform, ranging from 60 to 90'.
またワイピングにより濃度が1〜10重量%塗布液を擦
り込むようにガラス面に塗布した場合には、本発明と同
程度の撥水性をもつ撥水皮膜が形成される。Further, when a coating liquid having a concentration of 1 to 10% by weight is applied to a glass surface by wiping in a rubbing manner, a water-repellent film having water repellency comparable to that of the present invention is formed.
上記で得られた3種の撥水性ガラスについて、第1表
摩擦試験の前後の接触角を測定して塗布方法と撥水性と
の関係を調べた。For the three types of water-repellent glasses obtained above, the contact angles before and after the friction test shown in Table 1 were measured to investigate the relationship between the application method and water repellency.
接触角の測定は、協和界面科学■製 接触角計CA−A
型を用いて撥水性皮膜の水に対する接触角を測定した。The contact angle is measured using a contact angle meter CA-A manufactured by Kyowa Interface Science.
The contact angle of the water-repellent film with water was measured using a mold.
摩耗試験は、大栄科学精器製作所製 学振型平面摩耗試
験機を用い、摩擦子をネル布で覆い、荷重12009に
て1ooo回摩擦した。The abrasion test was carried out using a Gakushin type flat abrasion tester manufactured by Daiei Kagaku Seiki Seisakusho, the friction element was covered with flannel cloth, and the friction element was rubbed 100 times at a load of 12009.
第1表に摩耗試験前後の撥水皮膜の全面の接触角を調べ
その平均値を示す。Table 1 shows the average value of the contact angles of the entire surface of the water-repellent coating before and after the abrasion test.
従来の浸漬法により成膜した場合は、試験前の値が60
〜90”で低いが、摩擦試験後では5゜〜60”とさら
(低下している。一方、本発明の超音波を使用する方法
ではワイピングでガラス表面に擦り込む様に塗布した場
合と同じで試験前の初期値が95〜100”で摩擦後で
も90〜95°と低下が少なくガラス表面との接着性が
良く耐久性がよい撥水ガラスとなっている。When the film was formed using the conventional immersion method, the value before the test was 60.
90", which is low, but after the friction test, it has further decreased to 5° to 60". On the other hand, in the method using ultrasonic waves of the present invention, it is the same as when applied by rubbing it into the glass surface with wiping. The initial value before the test is 95 to 100'', and even after friction it is 90 to 95 degrees, which shows little deterioration, making it a water-repellent glass with good adhesion to the glass surface and good durability.
[効果]
本発明の製造方法によれば、ガラス面に対して濡れ性の
悪い塗布溶液であっても浸漬法によりガラス面に均一な
撥水皮膜を形成することができる。[Effects] According to the manufacturing method of the present invention, a uniform water-repellent film can be formed on the glass surface by the dipping method even if the coating solution has poor wettability on the glass surface.
このため浸漬法の特徴である濃度による塗布量のコント
ロールが容易にでき、塗布された塗膜を硬化して再現性
よく均一な撥水皮膜を形成することができる。また粘度
の高い撥水剤でもこの方法により撥水皮膜を形成するこ
とができる。得られる撥水性ガラスは従来のものに比べ
撥水性が向上できる。Therefore, the coating amount can be easily controlled by concentration, which is a feature of the dipping method, and the applied coating film can be cured to form a uniform water-repellent film with good reproducibility. Further, even with a highly viscous water repellent, a water repellent film can be formed by this method. The resulting water-repellent glass has improved water repellency compared to conventional glass.
Claims (1)
ラス基板を浸漬させて表面に撥水剤塗膜を形成し、次い
で該撥水剤塗膜を加熱硬化させて撥水皮膜をガラス基板
上に形成する撥水性ガラスの製造方法において、 該撥水剤塗膜の塗布時に該撥水剤溶液に超音波振動を加
えながら該ガラス基板を浸漬して撥水剤塗膜を形成する
ことを特徴とする撥水性ガラスの製造方法。(1) A glass substrate is immersed in a water repellent solution containing a silicone-based water repellent to form a water repellent coating on the surface, and then the water repellent coating is heated and cured to form a water repellent coating. In a method for manufacturing water-repellent glass formed on a glass substrate, the glass substrate is immersed in the water-repellent solution while applying ultrasonic vibration when applying the water-repellent coating film to form a water-repellent coating film. A method for producing water-repellent glass characterized by:
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3672890A JPH03242351A (en) | 1990-02-16 | 1990-02-16 | Production of water repellent glass |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3672890A JPH03242351A (en) | 1990-02-16 | 1990-02-16 | Production of water repellent glass |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH03242351A true JPH03242351A (en) | 1991-10-29 |
Family
ID=12477794
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3672890A Pending JPH03242351A (en) | 1990-02-16 | 1990-02-16 | Production of water repellent glass |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH03242351A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2013029685A (en) * | 2011-07-28 | 2013-02-07 | Marumi Koki Kk | Filter for digital camera with water-repellent function |
-
1990
- 1990-02-16 JP JP3672890A patent/JPH03242351A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2013029685A (en) * | 2011-07-28 | 2013-02-07 | Marumi Koki Kk | Filter for digital camera with water-repellent function |
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