A kind of preparation method of antimony oxide film

An antimony oxide film and transparent electrode technology, applied in the field of preparation of inorganic functional films, can solve problems such as temperature rise, coarse grains, complex sputtering equipment, etc., and achieve the advantages of avoiding blocking effect, simple preparation method and good application prospect. Effect

Inactive Publication Date: 2018-01-23
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods all have its weak point, for example: the sputtering equipment is complicated, and temperature rises during the sputtering process; Expensive vacuum equipment is required, so the cost is relatively high; chemical vapor deposition method is easy to cause deformation, coarse grains, reduced strength, especially excessive thermal stress and other problems

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Conductive glass (ITO) was ultrasonically cleaned in acetone and ethanol solutions for 15 minutes, and then rinsed with deionized water; 0.03gSb 2 S 3 Add to 10ml ethylenediamine and 1ml 1,2-ethanedithiol mixed solvent, stir and dissolve at room temperature to prepare electrodeposition solution; figure 1 As shown, two pieces of conductive glass 2 are used as cathode and anode electrodes, vertically arranged in the electrolytic tank 1 equipped with the above-mentioned electrodeposition solution 3, the electrode surfaces are parallel to each other, and the cathode constant potential electrodeposition is carried out, the voltage is 4V, and the plating time is After the electrodeposition is completed, a layer of uniform and dense film is deposited on the conductive glass. The electrodeposited film is soaked in pure water for 24 hours, then heat-treated at 400°C for 1 minute under nitrogen, and naturally cooled to room temperature to obtain antimony oxide membrane.

[0025...

Embodiment 2

[0028] Conductive glass (FTO) was ultrasonically cleaned in acetone and ethanol solutions for 15 minutes, and then rinsed with deionized water; 0.02gSb 2 S 3 Add it to a mixed solvent of 10ml ethylenediamine and 1ml 1,2-ethanedithiol, stir and dissolve at room temperature to obtain an electrodeposition solution; use two pieces of conductive glass as cathode and anode electrodes, and put them in a vertical arrangement with the above electrodes In the electrolytic tank of the deposition solution, the electrode surfaces are parallel to each other, and the cathode constant potential electrodeposition is carried out, the voltage is 8V, and the electroplating time is 20min. After the electrodeposition is completed, a uniform and dense film is deposited on the conductive glass, and the electrodeposited film Soak in pure water for 10 hours, then heat-treat at 350° C. for 5 minutes under nitrogen, and cool naturally to room temperature to obtain an antimony oxide film.

Embodiment 3

[0030] Conductive glass (AZO) was ultrasonically cleaned in acetone and ethanol solutions for 15 minutes, and then rinsed with deionized water; 0.01gSb 2 S 3 Add it to a mixed solvent of 10ml ethylenediamine and 1ml 1,2-ethanedithiol, stir and dissolve at room temperature to obtain an electrodeposition solution; use two pieces of conductive glass as cathode and anode electrodes, and put them in a vertical arrangement with the above electrodes In the electrolytic tank of the deposition solution, the electrode surfaces are parallel to each other, and the cathode constant potential electrodeposition is carried out, the voltage is 2V, and the electroplating time is 10min. After the electrodeposition is completed, a layer of uniform and dense film is deposited on the conductive glass. The electrodeposited film Soak in pure water for 8 hours, then heat-treat at 300° C. for 10 minutes under nitrogen gas, and cool naturally to room temperature to obtain an antimony oxide film.

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Abstract

The invention discloses a preparation method for an antimony oxide membrane. The preparation method mainly comprises the following steps: an antimony sulfide is dissolved in a mixed solution of ethidene diamine and 1,2-dithioglycol according to a rate that 0.01-0.03g of the antimony sulfide is added into every 11ml of the mixed solution of ethidene diamine and 1,2-dithioglycol, so that electrodeposition liquid is prepared; then two transparent electrodes are vertically arranged in an electrolytic cell containing the electrodeposition liquid for cathode constant-potential electrodeposition, wherein the voltage is 1.5 V-8V, and the electroplating time is 5-30 min; after the electrodeposition is finished, a uniform and compact membrane is deposited on a cathode; and the membrane electrode is soaked in water for 1-24 h, is subjected to thermal treatment for 1-10 min at 300-400 DEG C in a nitrogen atmosphere, and is naturally cooled to room temperature, so that the antimony oxide membrane is obtained on a conductive substrate. The manufacture method is simple, short in reaction time and high in productivity and is applicable to large-scale production of factories; the practicability is high; and the preparation method has good application prospect.

Description

technical field [0001] The invention relates to a preparation method of an inorganic functional film, in particular to a preparation method of an antimony oxide film. Background technique [0002] Antimony trioxide is an important group V–VI compound that has been widely used in industry over the past century. It is often used as a flame retardant synergist for flame retardant of various polymer materials; as a defoamer for melting glass, clearing air bubbles, and as a catalyst in polyester fibers, especially with vanadium, uranium, molybdenum and iron oxide It is used in the ammoxidation reaction of acetone and the oxidation or ammoxidation reaction of propylene; as a passivator in heavy oil, residual oil, catalytic cracking, and catalytic reforming in petroleum; as a covering agent in the enamel industry, as a It is a kind of white pigment, which can be used in paint and other industries, and can prepare various antimonides. There are two crystal forms of antimony trioxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D9/08C01G30/00
CPCC01G30/005C25D9/08
Inventor 张海全侯文龙梁波王海龙郭慧云赵乐乐程才红彭飞杨越冬
Owner YANSHAN UNIV
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