KR20070013712A - Method for manufacture of coating glass with improved anti-fogging - Google Patents

Abstract

A process of manufacturing a coated glass with improved anti-fogging property is provided to produce the glass having expression of transition metal oxides by UV ray and improved anti-fogging property by fabricating a coating layer with transition metal oxides such as titanium dioxide, zinc oxide, tin dioxide through vacuum coating mode and applying silica solution to the coating layer. The process comprises the steps of: preparing a coating layer from transition metal oxide such as titanium dioxide, zinc oxide, tin dioxide through vacuum coating way; and applying a silica solution to the coating layer by any one selected from flow coating, spin coating and dip coating to form the resulting coating layer. The process further includes addition of pore generating agent to the silica solution to form the porous silica layer. The process includes additional step of heat treating the silica layer under oxidation atmosphere at 100 to 350deg.C for 30 minutes to 2 hours to enhance adhesion between the silica layer and the transition metal oxide layer.

Description

Method for manufacture of coating glass with improved anti-fogging}

1 is a schematic view showing the structure of a conventional hydrophilic coating glass.

Figure 2 is a schematic diagram showing the structure of the hydrophilic coating glass by the conventional reaction sputtering method.

Figure 3 is a schematic diagram showing the structure of the coated glass improved anti-fog holding force according to the present invention.

<Description of the symbols for the main parts of the drawings>

10 silica particles 12 transition metal oxides such as titanium dioxide

The present invention relates to a method for manufacturing coated glass having improved antifogging property, and more particularly, to manufacturing an improved antifogging holding glass that improves anti-fogging holding force in which semiconductive transition metal oxide is exposed to ultraviolet rays. It is about a method.

Generally, it is advantageous for automotive glass to have hydrophilicity by ultraviolet rays or the like.

Conventional hydrophilic coated glass forms a structure of porous silica particles 10 on the transition metal oxide (12) layer, such as titanium dioxide, in order to maintain the hydrophilicity expressed by irradiation of ultraviolet light on the surface of titanium dioxide. do.

In forming the optical functional hydrophilic coating glass there are two methods as follows.

1. A method of forming two layers by reaction sputtering in a vacuum coating method as shown in FIG.

2. There is a method of mixing the titanium dioxide forming liquid and silica forming liquid by wet coating and then heat treatment after coating.

However, the conventional optically functional hydrophilic coated glass has a high durability in the silica layer.

1. In the case of reaction sputtering, there is a problem that the bonding force between silica layer and titanium dioxide layer is insufficient, so that it is easily separated by boiling test or alkaline solution.

2. In the case of the wet coating, there is a problem that the anti-fogging force is easily lowered due to the high temperature heat treatment (over 500 ° C.) after the mixed coating of the silica and the transition metal oxide.

The present invention has been made in view of the above point, and the light-excited anti-fogging properties of the coating layer surface caused by the photoexcited semiconducting properties of transition metal oxides such as TiO ₂ , ZnO, SnO _2, etc. The object of the present invention is to provide a method of manufacturing coated glass with improved anti-fog holding ability, which can be maintained for a long time even in the absence of (ultraviolet rays).

The present invention for achieving the above object in the coated glass having a titanium dioxide layer and a porous silica structure,

After preparing a coating layer of a transition metal oxide such as titanium dioxide, zinc oxide, tin dioxide, etc. by vacuum coating method, the coating layer is prepared by any one method selected from flow, spin, and dip coating on the coating layer. do.

In a preferred embodiment, the silica layer is porous by adding a pore-forming agent to the silica solution.

In a more preferred embodiment, the silica layer is heat-treated at an temperature of 100 to 350 ° C. for 30 minutes to 2 hours in an oxidizing atmosphere to improve the bonding strength between the silica layer and the transition metal oxide layer.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

3 is a schematic view showing the structure of the coated glass with improved anti-fogging force according to the present invention.

The present invention can maintain the anti-fogging properties of the surface of the coating layer caused by the photoexcited semiconducting properties of transition metal oxides such as TiO ₂ , ZnO, SnO ₂ even in the absence of light irradiation (ultraviolet). One point is to make it possible.

Example 1

A thin silica solution prepared by hydrolysis from a silane solution or the like on the glass surface is thinly coated on the transition metal oxide layer produced by the reaction sputtering method by spin, flow, or dip coating method, and then firmly adhered to the transition metal oxide layer. By carrying out the heat treatment in order to improve the durability, the durability of the porous silica layer that influences the antifogging property can be improved.

In the case of the reaction sputtering method, the degree of vacuum is 10 ^-2 to 10 ^-3 torr, the reaction gas ratio and the supply amount are Ar: 0 ₂ = 1: 4,20.0 sccm, the target input power is made under the conditions of 4KW or more.

In the case of the wet coating and heat treatment, the silica layer coating solution is a pore forming polymer (PEG; pore forming agent) is added to the hydrolysis solution of Tetra Ethoxy Ortho Silicate solution, the concentration of the coating solution is 0.001 Mole / liter. At this time, the coating speed is 1 cm / min (lift speed, dip coating), the heat treatment is made for 30 hours at 100 ~ 350 ℃ for 2 hours.

Comparative Example 1

Coating glass which forms a titanium dioxide layer and a porous silica layer by reaction sputtering.

Comparative Example 2

Coated glass that is heat-treated after coating once after mixing titanium dioxide forming liquid and silica forming liquid by wet coating.

Test Example: Evaluation

The boiling test of the glass of Example 1, Comparative Example 1 and Comparative Example 2 thus prepared and the result of the immersion test of NaOH aqueous solution of 1 normal concentration are as follows.

1. Boiling test: Soak three kinds of glass in boiling water of 100 ℃ and heat it for 30 minutes.

2. Alkali test: Three kinds of glass are immersed in 1N NaOH aqueous solution for 2 hours.

The specimens tested according to the boiling test and the alkali resistance test were thoroughly dried with distilled water, and the dried specimens were allowed to stand for 12 hours under a BLB (Black light Blue) lamp having a dose of 1 mW / cm 2, and then the water droplets on the surface of the specimens. The contact angle is measured by dropping the sample, and the contact angle is measured after storage in a dark place for 168 hours.

As a result of the measurement, the glass produced by Example 1 according to the present invention maintained a contact angle of 7 degrees even after about 7 days in the dark, whereas in the same conditions for Comparative Example 1 and Comparative Example 2 The contact angle rose to 30 degrees and 35 degrees.

Therefore, when the silica solution is thinly coated on the transition metal oxide produced by the reaction sputtering method by wet coating, the contact angle of 10 degrees or less can be maintained to maintain the antifogging property for a long time even in the absence of light irradiation (ultraviolet ray).

As described above, according to the manufacturing method of the coating glass with improved anti-fog holding force according to the present invention, when the silica solution is thinly coated by the wet coating on the transition metal oxide produced by the reaction sputtering method to maintain a contact angle of 10 degrees or less Therefore, antifogging property can be maintained for a long time even in the absence of light irradiation (ultraviolet ray).

Claims (3)

In the coated glass having a titanium dioxide layer and a porous silica structure, After preparing a coating layer of a transition metal oxide such as titanium dioxide, zinc oxide, tin dioxide, etc. by vacuum coating method, the coating layer is prepared by any one method selected from flow, spin, and dip coating on the coating layer. Method of manufacturing a coated glass with improved anti-fogging force. The method according to claim 1, A method of manufacturing coated glass having improved antifogging property, characterized in that the silica layer is made porous by adding a pore-forming agent to the silica solution. The method according to claim 1 or 2, The silica layer is heat-treated for 30 minutes to 2 hours at a temperature of 100 to 350 ℃ in an oxidizing atmosphere to improve the adhesion between the silica layer and the transition metal oxide layer characterized in that the anti-fogging retention improved coating glass manufacturing method.

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