JPS5927964A - 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 organocerium compd., an organosilicon compd., a thickening agent and an org. solvent, as well as a transparent film having good film characteristics, by coating a substrate with said paste and firing it. CONSTITUTION:A paste for forming transparent film is prepd. from an organocerium compd. such as triacetylacetonato cerium, an organosilicon compd. such as vinyl tris (2-methoxyethoxy)silane, a thickening agent such as cellulose compd. and an org. solvent (e.g. butyl cellosolve) capable of dissolving the above three components. The combined amount of said organocerium compd. and said organosilicon compd. in the paste is pref. 2-30wt%. A substrate such as glass or ceramic is screen-printed with said paste and fired at 400 deg.C or above to form a transparent cerium 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 particularly to a transparent film made of cerium oxide-silicon oxide. .

Methods for forming a transparent metal oxide film made of cerium oxide-silicon oxide include a vacuum deposition method, a chemical spray method, and a dipping method. By the way, although the properties of the film formed by the vacuum evaporation method are excellent, there is a problem in mass production, and processing such as etching is required in order to correspond to the formation of a pattern. On the other hand, the chemical spray method and the dipping method are relatively suitable for mass production, but they have the same problems as the former when it comes to patterning.As described above, the conventional methods have advantages and disadvantages, and are not necessarily considered superior or superior methods. It's difficult.

The object of the present invention is to overcome the drawbacks of the prior art.
An object of the present invention is to provide a paste for forming a transparent film that can be screen printed with excellent mass productivity and has good film properties, and a transparent film formed using the paste.

To achieve this objective, the present invention comprises an organic cerium compound which forms a cerium oxide-silicon oxide film by firing, an organic solvent-soluble organic cerium compound, an organic silicon compound, a thickener, and a stiff organic cerium compound. The present invention is characterized in that an organosilicon compound and an organic solvent that dissolves a thickener are kneaded to form a paste for forming a transparent film.

In order to achieve the above object, the present invention further provides an organic cerium compound and an organic silicon compound which are compounds that form a cerium oxide-silicon oxide film by firing, and which are soluble in an organic solvent, a thickener, and a stiff organic cerium compound. The compound, an organosilicon compound, and a soluble organic solvent such as a thickener are kneaded and coated on a paste substrate, which is then baked to form a transparent film of cerium oxide-silicon oxide.

The organic cerium compound used in the present invention includes:
Cerium trisacetylacetonate is preferred.

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

Further, as the thickener used in the present invention, cellulose compounds such as nitrocellulose and ethylcellulose are suitable.

Examples of the organic solvent that dissolves the organic cerium compound, the organic silicon compound, and the thickener include terhineol, 2
- High boiling point alcohols such as ethylhexanol and benzyl alcohol, high boiling point esters such as verzyl acetate and dimethyl phthalate, calpitol and butyl carpitol.

High boiling point alcohol ethers such as butyl cellosolve are used.

A paste is made by mixing an organocerium compound, an organosilicon compound, a thickener, and an organic solvent in a predetermined ratio, and a screen plate patterned into a desired shape is also used to make the paste into glass, ceramic, etc. Screen print onto the board. By baking at a temperature of about 400°C or higher after pre-drying, a cerium oxide-silicon oxide transparent film h'' is formed in the desired turn.This film is not only transparent but also has a high film strength. It has relatively poor insulation properties.Furthermore, by appropriately controlling the total amount of organic cerium compounds and organic silicon compounds in the paste, it is possible to freely form a film of 20,006 or less. .

Next, examples of the present invention will be described.

The following compositions were prepared by using triacetylacetonate and cerium as the organic cerium compound, vinyltris(2-methoxyethoxy)silane as the organic silicon compound, and varying the mixing ratio of the organic compounds.

[Organic compounds] 15-layered Hif, □) Squirrel (2-meth4'c) -+7) □ 58
Ding 3. Amount Tisilane (X+Y=100) [Thickener] 14ili! ? 3'tinitrocellulose 14-fold organic solvent [Organic solvent] 71% by weight Butyl cellosolve 355% by weight Butylcarpitol 355% by weight Also, for comparison, organic compounds such as cerium triacetylacetonate and vinyltris (2-methoxy A paste was made using the same O8β using ethoxysilane Sowazowa alone.

Each stiff paste? 250 meshes and a screen plate made of stainless steel net with a resist thickness of 10 μm was used to print on a soda glass substrate.

Pre-dry at 150°C for 15 minutes, then dry at 50°C.
After firing at 0° C. for 30 minutes, a clear metal oxide film was formed on the J7 teeth.

The film characteristics of each transparent film were investigated and the results are shown in the following table.

Note that in the table, O marks indicate good R, and △ marks indicate somewhat poor results.

An X mark indicates something that has been judged to be bad. The film strength was examined using a pencil-type 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 containing an organic cerium compound and an organosilicon compound soluble in an organic solvent as in the present invention has a relatively thick film thickness. Even if the visible part has only a small amount of light transmittance, it also has high military insulation. ). Furthermore, the paste used in the present invention has good screen printability and the printed surface is very sharp.

As a result of examining the total content of organic cerium compounds and organic silicon compounds in the paste and the occurrence of cracks in the formed film, it was found that cracks occur when the total content exceeds 30% by weight. On the other hand, if the total content is less than 2% by weight, the amount is too small and it is almost impossible to form a film. Therefore, the total content of organocerium compounds and organosilicon compounds in the paste is regulated to a range of about 2 to 30% by weight, which means that the film thickness is 500%.
Beautiful transparent metal oxide coatings are formed from °A to 2000°.

The present invention has the above-mentioned structure, and can be screen printed suitable for production, and has a transparent film forming paste that can be easily patterned, as well as a paste that has good light transmittance and insulation properties even if the film is relatively thick. A highly transparent film can be formed.

Claims (1)

[Scope of Claims] (1) An organic cerium compound and an organic silicon compound which are compounds that form a cerium oxide-silicon oxide film by firing, a thickener, the organic cerium compound, an organic 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 according to claim (1), characterized in that the organic cerium compound is cerium triacetylacetonate. (3) Claim (1) ), wherein the organosilicon compound is vinyltris(2-methoxyethoxy)silane. (4) In claim (1), the paste A paste for forming a transparent film, characterized in that the thickener is a cellulose compound. (5) In claim (1), the total content of the organic cerium compound and the organic silicon compound in the paste. A paste for forming a transparent film, characterized in that the particle size is regulated to a range of about 2 to 30 times. An organic cerium compound, an organic silicon compound, a thickener, and an organic solvent that dissolves the organic cerium compound, the organic silicon compound, and the thickener are kneaded together and then applied onto a paste substrate and fired. A transparent coating characterized by forming a cerium oxide-silicon oxide coating. (7) In claim (6), the total content of the organic cerium compound and the organic silicon compound in the paste is A transparent film characterized by being regulated within a range of approximately 2 to 30 times.