A kind of preparation method of tin oxide film

A tin oxide and thin film technology, applied in tin oxide and other directions, can solve the problems of incomplete reaction, turbulent airflow, affecting the quality of the film layer, etc., and achieve the effects of good thickness consistency, smooth aerosol movement, and superior electrical conductivity.

Active Publication Date: 2015-08-26
YANGZHOU MINGSHENG NEW TECH
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AI Technical Summary

Problems solved by technology

[0003] At present, conventional spray pyrolysis usually uses high-pressure liquid flow and high-pressure airflow to mix and spray to form high-speed moving atomized droplets, which hit and deposit on high-temperature substrates for thermal decomposition to form thin film deposition. , solvent vaporization, and thermal decomposition reactions lead to significant heat absorption and cooling, which are likely to cause problems such as uneven deposition on the substrate surface, sudden drop in temperature, cracking of the substrate, incomplete reaction, etc. Usually, the solvent usually uses a low molecular weight flammable organic solvent, Periodic, intermittent spraying is also required
It not only affects the quality of the film layer, but also reduces the production efficiency. In addition, a large amount of waste gas emission and environmental pollution are also problems that it must face
[0004] There are four problems in spray pyrolysis technology: 1. Antimony halides, hydrofluoric acid and ammonium fluoride are used for doping, especially the fluorides are easy to volatilize and the doping efficiency is extremely low, resulting in serious fluoride pollution and emission 2. The spray method of pressure liquid atomization leads to large atomized droplet size (5 μm ~ 20 μm), the atomization amount is too large and difficult to control, the substrate cooling is serious, and there are many internal and surface defects in the film. At the same time, Objectively requires intermittent and periodic repeated spraying, which leads to a decrease in production efficiency; 3. Using an organic solvent system, the concentration of sol (solution) is low, and the pollution discharge is serious during the thermal decomposition process, and the coating deposition cycle is long and the production efficiency is low; 4 , The impact of the gas flow on the substrate leads to gas flow disorder, uneven deposition and low deposition efficiency
[0005] In addition, the usual means of atomization is ultrasonic atomization, which uses ultrasonic energy to atomize the solution into tiny mist particles. The formed aerosol is warm and gentle, but it is limited by the following four aspects: 1. Ultrasonic chips are not easy to work in acidic , Alkaline and other corrosive media environment; 2. Due to the limitation of ultrasonic energy, it cannot fog high-concentration solutions; 3. It needs fan blowing to complete the aerosol transportation, and the working mechanism is complicated; 4. Due to the heating of the chip during the working process , resulting in unstable solution system and precipitation, not suitable for industrial production of thin film preparation

Method used

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  • A kind of preparation method of tin oxide film
  • A kind of preparation method of tin oxide film
  • A kind of preparation method of tin oxide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Under room temperature, normal pressure, and dry environment, use antimony trifluoride as raw material and deionized water as solvent, and mix and stir to form a doping solution. Using tin tetrachloride (SnCl 4 ) as the raw material and deionized water as the solvent, mixed and stirred to form a tin salt solution. Then the doping solution is added dropwise to the tin salt solution under stirring conditions to form a mixed solution. The doping ratio in the mixed solution is: fluorine is 18 mol%, antimony is 6 mol%, and the molar concentration of tin is 3.5 mol / L , and then use hydrochloric acid to adjust the pH of the solution to about 2-3, and after airtight aging for 6 hours, a precursor coating solution is obtained.

[0029] The precursor coating solution is then added to the gas compression atomizer.

[0030] 2. Select one of the high-temperature-resistant materials such as high-transmission glass (low-Fe glass), quartz glass, Corning glass, and high-alumina til...

Embodiment 2

[0037] 1. Under room temperature, normal pressure, and dry environment, use antimony trifluoride as raw material and deionized water as solvent, and mix and stir to form a doping solution. Using tin tetrachloride (SnCl 4 ) as the raw material and deionized water as the solvent, mixed and stirred to form a tin salt solution. Then the doping solution is added dropwise to the tin salt solution under stirring conditions to form a mixed solution, and the doping ratio in the mixed solution is controlled: the fluorine is 24 mol%, the antimony is 8 mol%, and the tin molar concentration is 3.5 mol / L. The pH value of the mixed solution is adjusted to 2-3 with trifluoroacetic acid, and sealed and aged for 10 hours to obtain a precursor coating solution.

[0038] The precursor coating solution is then added to the gas compression atomizer.

[0039] 2. Select one of the high-temperature-resistant materials such as high-transmission glass (low-Fe glass), quartz glass, Corning glass, and h...

Embodiment 3

[0046] 1. Under room temperature, normal pressure, and dry environment, use antimony pentafluoride as raw material and deionized water as solvent, and mix and stir to form a doping solution. Using tin tetrachloride (SnCl 4 ·5H 2 O) as the raw material and deionized water as the solvent, mixed and stirred to form a tin salt solution. Then the doping solution is added dropwise to the tin salt solution under stirring conditions to form a mixed solution, and the doping ratio in the mixed solution is controlled: fluorine is 24 mol%, antimony is 4.8 mol%, tin is 2.5 mol / L, and hydrochloric acid is used adjust the mixed solution p The H value reaches 2-3, and after airtight aging for 10 hours, a precursor coating solution is obtained.

[0047] The precursor coating solution is then added to the gas compression atomizer.

[0048] 2. Select one of the high-temperature-resistant materials such as high-transmission glass (low-Fe glass), quartz glass, Corning glass, and high-alumina t...

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Abstract

The invention discloses a preparation method of a tin oxide film, and belongs to the technical field of film preparation. The preparation method is as follows: a fluoride of antimony is used as a doping source, a chloride of tin is used as a starting raw material, after mixed atomization, the fluoride of antimony and the chloride of tin are deposited on the surface of a high temperature resistant substrate to from a transparent fluorine-antimony co-doping tin oxide thin film with good functions. According to the method, in a SnO2 crystal structure, fluoride ions replace part of oxygen ion positions, antimony ions replace part of tin ion positions for doping, and higher carrier density is obtained, so that the tin oxide film is better in electrical conductivity, atmosphere sensitivity, transmittance and the like than single fluorine or single antimony doping film, and is a very advanced and potential semiconductor functional thin film material.

Description

technical field [0001] The invention belongs to the technical field of film preparation, and relates to a water system atomization heat deposition preparation method of a fluorine-antimony co-doped tin oxide film. Background technique [0002] The current preparation methods of different ion-doped tin oxide films mainly include sputtering deposition (PVD), chemical vapor deposition (CVD), and spray pyrolysis (SP) technology coating. Compared with PVD and CVD methods, the equipment and process of spray pyrolysis SP method are relatively simple, not only can prepare high-quality films, but also easy to dope, it is an economical, high-efficiency, large-scale, industrial film preparation method . [0003] At present, conventional spray pyrolysis usually uses high-pressure liquid flow and high-pressure airflow to mix and spray to form high-speed moving atomized droplets, which hit and deposit on high-temperature substrates for thermal decomposition to form thin film deposition. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C17/23C01G19/02C04B41/85
Inventor 张卫华高中明陈源清
Owner YANGZHOU MINGSHENG NEW TECH
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