JPH05856A - Method for calcining thin-film forming material - Google Patents

Abstract

(57) [Abstract] [Purpose] The baking temperature for forming a metal or metal oxide thin film by coating a thin film forming material on a substrate with a low softening point such as soda lime glass, drying, and baking as much as possible It is to provide a method that can be performed at low temperatures. [Structure] The baking temperature when baking the thin film forming material is 50
When the temperature is 0 to 600 ° C, the oxygen concentration in the gas is 75 vol%
In the above atmosphere, the firing temperature exceeds 600 ° C and 700 ° C
In the following cases, the object can be achieved by firing in an atmosphere in which the oxygen concentration in the gas is 50 vol% or more.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for firing a thin film forming material used for forming a thin film of metal or metal oxide on a substrate having a low softening point.

[0002]

2. Description of the Related Art In the conventional method, a thin film forming material is printed by a screen printing machine, dried at 120 ° C. for about 5 minutes, and then heated to 700 to 850 ° C. in the atmosphere to obtain a thin film forming material. An organic substance as a component is decomposed and oxidized to form a metal or metal oxide thin film on the substrate. However, for low softening point substrates such as soda lime glass, 700
At a firing temperature of ˜850 ° C., the substrate was softened and it was impossible to form a circuit using the thin film forming material. In order to form a thin film of metal or metal oxide using a thin film forming material, it is necessary to burn a large amount of organic substances contained in the thin film forming material in the atmosphere to cause thermal decomposition and oxidation. At this time, most of the organic substances are decomposed into carbon and further oxidized into carbon dioxide, which is discharged to the outside air. If this reaction does not occur quickly, some carbon will remain in the deposited metal thin film, and the surface of the metal thin film thus formed will discolor or become a film with poor surface roughness. At a high temperature of 700 to 850 ° C., organic substances are completely converted to carbon dioxide and gasified so that carbon does not remain in the film. However, for forming a thin film on a low softening point substrate such as soda lime glass, a substrate The softening occurred and the thin film forming material could not be used.

[0003]

SUMMARY OF THE INVENTION The present invention is directed to a low softening point substrate such as soda lime glass having a low softening point, which has hitherto been impossible, by using a thin film forming material and using a metal or metal oxide free of organic decomposition products or carbon. The object is to provide a firing method for forming a thin film of a product.

[0004]

According to the present invention, when firing a thin film forming material, when the firing temperature is 500 to 600 ° C., the oxygen concentration in the gas is set to an atmosphere of 75 vol% or more, and the firing temperature exceeds 600 ° C. This is a method for baking a thin film forming material, which is characterized in that, when the temperature is 700 ° C. or less, the gas is baked in an atmosphere having an oxygen concentration of 50 vol% or more.

When the thin film forming material is fired, it will be 7
It has been found that even with a thin film forming material that requires a firing temperature of 00 to 850 ° C., the firing temperature is lowered by 100 to 350 ° C. by firing in an atmosphere with an increased oxygen concentration. When the firing temperature is 500 to 600 ° C., the oxygen concentration in the gas is set to an atmosphere of 75 vol% or more. Even in a 100% oxygen atmosphere, a large amount of organic substances in the thin film forming material are completely decomposed at a temperature of less than 500 ° C. 75vo due to lack of speed
This is because in an atmosphere containing 1% or more oxygen, the firing rate does not change even if the temperature is raised to 600 ° C. or more. Further, when the firing temperature is 600 to 700 ° C., firing is performed in an atmosphere in which the oxygen concentration in the gas is 50 vol% or more, because when the oxygen concentration is 50 vol% to 75 vol%, the decomposition rate of organic substances is unsatisfactory when the firing temperature is less than 600 ° C. This is because the decomposition rate is sufficient, and the decomposition rate of organic substances does not change even at a firing temperature of 700 ° C. or higher. Hereinafter, details of the present invention will be described with reference to examples.

[0006]

Example 1 A gold metalloorganic (AP-222CA manufactured by Tanaka Kikinzoku Kogyo) was solid-printed on a glass glaze substrate (200 × 300 × thickness 1.1 mm) with a # 325 mesh screen at 120 ° C. It was dried with warm air in a clean oven for 5 minutes. Then 500, 6
At a firing temperature of 00 and 700 ° C., a mixed gas of nitrogen and oxygen is mixed in a tubular furnace at a ratio of oxygen of 25 to 100 v in the mixed gas.
The content was changed to ol% and baked. The firing conditions at this time are
The temperature was raised at 40 ° C./min, and after reaching each temperature, the temperature was maintained for 10 minutes. The flow rate of the mixed gas of nitrogen and oxygen flowing in the tubular furnace was 2 liters per minute. The surface of the gold thin film thus formed was observed with a stereoscopic microscope, the same substrate was used as a glass glaze substrate, and the heating rate was 40 ° C /
Table 1 shows the results of comparison with the surface of the gold thin film formed by holding the film at 830 ° C. for 10 minutes.

[0007]

[Table 1]

[0008]

For comparison, a gold metalloorganic (AP222CA manufactured by Tanaka Kikinzoku Kogyo Co., Ltd.) was screen-printed on the same glass glaze substrate as in the above example, and the temperature was raised to 40 ° C./min at 700 ° C. in the atmosphere. And held for 10 minutes for firing. As a result, the reddish brown color was stronger than that of the gold thin film when fired at 830 ° C.

[0009]

[Example 2] A soda lime glass substrate which is a low softening point substrate was used as a substrate, and gold metalloorganic was screen-printed in the same manner as in Example 1, and in an atmosphere having an oxygen concentration of 75 vol%, a heating rate of 40 ° C / Min, and baked at 500 ° C. for 10 minutes. The gold thin film formed as a result was obtained in Example 1.
It had a golden luster similar to the case of using the glass glaze substrate.

[0010]

Example 3 Screen printing was performed on a soda-lime glass substrate in the same manner as in Example 2 except that the gold metalloorganic was changed to platinum metalloorganic (ES-16 manufactured by Tanaka Kikinzoku Kogyo Co., Ltd.), the oxygen concentration was raised to 75 vol%, and the temperature was raised. Speed 30 ℃
/ Min, the temperature was kept at 500 ° C. for 10 minutes for firing. As a result, the platinum thin film thus formed had a silver glossy surface.

[0011]

As is apparent from the above description, in order to form a thin film using a thin film forming material on a substrate having a low softening point such as soda lime glass, conventional firing in air is expensive. Although it was not possible to form a thin film by softening the substrate due to the need for temperature, according to the method of the present invention, a thin film that can be fired at a low temperature and formed,
This is a method capable of solving the conventional problem of being able to obtain the same material as that formed at a high temperature.

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Claims (1)

Claims: 1. When firing a thin film forming material, the oxygen concentration in the gas is 75 vo when the firing temperature is 500 to 600 ° C.
When the firing temperature is higher than 600 ° C and lower than 700 ° C, the oxygen concentration in the gas is 50 vol%.
A method for firing a thin film-forming material, comprising firing in the above atmosphere.