JPS5927961A - Paste for forming transparent film and transparent film - Google Patents

Abstract

PURPOSE:To provide a paste for forming transparent film, which has excellent mass-productivity, consisting of an organolead compd., an organo-silicon compd., a thickening agent and an org. solvent, as well as a transparent film having a high film strength and relatively high insulating properties, by coating a substrate with said paste an firing it. CONSTITUTION:A paste for forming transparent film is prepd. from an organolead compd. such as lead caprylate, an organosilicon compd. such as vinyl-tris (2-methoxyethoxy) silane, a thickening agent such as cellulose compd. and an org. solvent (e.g. butylcarbinol) capable of dissolving said organolead compd., said organosilicon compd. and said thickening agent. The combined amount of said organolead compd. and said organosilicon compd. in the paste is pref. 2- 10wt%. A substrate such as glass or ceramic is screen-printed with said paste and fired at 400 deg.C or above the form a transparent lead oxide/silicon oxide film having the desired pattern.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a transparent metal oxide film formed on a substrate such as glass or ceramic, and more specifically, the present invention relates to a transparent metal oxide film formed on a substrate such as glass or ceramic. j
It is related to Ig.

6; Transparent metal oxide coating 1 made from lead dioxide-silicon oxide
;・:°(formation methods include vacuum evaporation method, chemical spray method, and immersion method), and (. There were problems with this, and processing such as etching was required to support patterning.

On the other hand, the chemical spray method and the dipping method are relatively suitable for actual production, but the patterning response is similar to the former: 1'α. As you can see, the conventional method has advantages and disadvantages, and it cannot necessarily be said that it is a superior method.

The purpose of the present invention is to eliminate the drawbacks of such conventional collisions [2]
, screen printing with excellent M productivity is possible, and the coating l[l
Paste for forming a transparent film with good I' property and its paste) Dilutive film formed using Pi;/Provided-
It's all over the place.

To achieve this objective, the present invention provides a compound which forms a film of lead-silicon oxide (by calcination) in an organic solvent.
A paste for forming a transparent film is produced by mixing a soluble organic lead compound and an organic silicon compound with a stiff organic lead compound, an organic silicon compound, and a soluble organic solvent such as a thickener. be.

In order to achieve the above-mentioned object, the present invention further provides a method for forming a lead oxide-silicon oxide glue by calcination. A paste made by kneading a stiff organic lead compound, an organic silicon compound, and a soluble organic solvent such as a thickener is applied to a substrate and fired to form a lead oxide-silicon oxide selection film. 2).

As the organic lead compound used in the present invention, lead octylate is preferable.

Furthermore, as the organosilicon compound used in the present invention, vinyltris(2-methoxyethoxy)silane is preferred 2).

Furthermore, as the first filter thickener used in the present invention, cellulose compounds such as nitrocellulose and ethylcellulose are preferred.

Examples of organic solvents that can dissolve the above-mentioned lead compound, organosilicon compound, and thickener include terpineol, 2-ethylhexanol, and benzyl alcohol. High boiling point alcohol-A/s, high boiling point esters such as verzyl acetate and dimethyl tucrate, and high boiling point alcohol ethers such as carpitol, butyl carpitol and butyl cellosolve are used.

A 1m lead compound, an organosilicon compound, a thickener, and a hot solvent are mixed in a predetermined ratio to make a paste, patterned into the desired shape, and using a seventh screen plate, the paste is made of glass. Screen printing is performed on a nine board such as ceramic.By pre-drying this and firing it at a temperature of about 400°C or higher, a transparent film of lead oxide-silicon oxide is formed in the desired pattern. Not only is it transparent, it has a strength of 116 and has relatively high insulation properties.

However, it is important to appropriately control the total amount of organic lead compounds and organic silicon compounds in the paste (from τ, 4
A coating of 000'A or less can be freely formed.

Next, examples of the present invention will be described.

Using lead octylate (lead content 20%) as an organic lead compound and vinyltris(2-methoxyethoxy)silane as an organic silicon compound, pastes with the following compositions were made by varying the mixing ratio of the organic compounds. It was created.

[Organic compound] 5% by weight (X+Y=1
00) [Thickener] 14 weight - nitrocellulose 144 weight% organic solvent] 81 Shigesato Typtyl Cellosolve 405 Butyl Calpitol 4
05% by weight Also, for comparison, an organic compound and 12 lead octylate and vinyltris(2-methoxyethoxy)silane were used individually and pastes were made in the same way. Created.

For each paste, resist thickness is 250 mesh.
A screen version made of Oμn1 stainless steel net? to print on a soda glass substrate.

Then, they were pre-dried at 50"C for 15 minutes and then fired at 500C for 30 minutes to form transparent metal oxide films.

The results of examining the film properties of each of these transparent films are shown in the following table.

Note that in the table, ○ marks are good and △ marks are slightly bad.

An X mark indicates something that has been judged to be bad. The film strength was examined using a pencil scratch test, and the light transmittance indicates the minimum light transmittance in the visible region.

Table As is clear from this table, the transparent metal oxide film formed using the paste of the present invention containing an organic lead compound and an organosilicon compound that are soluble in an organic solvent has a relatively thick film. Even though it is thick, it has a high minimum light transmittance in the visible region and has high electrical insulation properties. Furthermore, those using the paste of the present invention have good one-screen printability and the printed surface is very hard.

As a result of examining the total content of organolead compounds and organosilicon compounds in the paste and the presence or absence of cracks in the formed coating, it was found that the total content was 10% by weight - 1% 'k t'BY, which means that no cracks occurred. There is an outbreak. On the other hand, if the total content is less than 2 M%, the amount is too small and it is almost impossible to form a film. Therefore, if the total content of organolead compounds and organosilicon compounds in the paste is controlled to be within the range of approximately 2 to 10% by weight, a beautiful transparent metal oxide coating with a film thickness of 500'' to 4000'A will be formed. is formed.

The present invention has the above-mentioned structure, and can be screen printed suitable for 48cm, has a transparent film forming paste that is easy to pattern, and has light transmittance and insulation properties even if the film thickness is relatively jν. A highly transparent coating can be formed.

Claims (1)

[Scope of Claims] (1) an organic lead compound and an organic silicon compound which are compounds that form a lead oxide-silicon oxide film upon firing; a thickener; A paste for forming a transparent film characterized by comprising a silicon compound and an organic solvent that dissolves a thickener. (2. A paste for forming a transparent film characterized in that the organic lead compound is lead octylate in claim (1). (3) Claim (1) In the description, the paste for forming a transparent film is characterized in that the organosilicon compound is vinyltris(2-methoxyethoxy)silane. (4) In the description in claim (1), the thickening agent A paste for forming a transparent film, characterized in that the agent is a cellulose compound. (5) In claim (1), the total content of the organolead compound and the organosilicon compound in the paste is about A paste for forming a transparent film, characterized in that the weight is regulated in the range of 2 to 10. (6) Organic lead, which is a compound that forms a lead oxide-silicon oxide film by firing and is soluble in organic solvents. compound, an organosilicon compound, a thickener, and an organic solvent that dissolves the organolead compound, the organosilicon compound yz, and the thickener?
The kneaded paste is applied onto the substrate and fired to form lead oxide.
Silicon oxide god np + formed is characterized by 1
Bright film. (7) In claim (6), the total content of the organic lead compound and the silicon compound in the paste is regulated to a range of about 2 to 10 times the content. Transparent coating.