A kind of preparation method of antimony sulfide film

An antimony sulfide and thin film technology, applied in metal material coating process, vacuum evaporation plating, coating and other directions, can solve the problems of long and complicated preparation process, waste of raw materials, high cost, etc. Environmental pollution problems, the effect of reducing production costs

Active Publication Date: 2021-11-30
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems of these preparation methods are as follows: 1) The preparation process is lengthy and complex, with many influencing factors and poor repeatability; 2) The antimony sulfide film composition segregation is serious, and it needs to be further passed through excessive sulfur powder or poisonous hydrogen sulfide gas Annealing treatment will inevitably cause environmental pollution and waste of raw materials; 3) high-purity antimony sulfide (≥99.99%) material preparation is required, and the cost is expensive
However, the conventional vacuum coating has a high degree of vacuum, it is difficult to control the doping concentration of impurity elements, and it is often over-doped, which is not conducive to the coating of stibnite. Due to the problems of impurities and low sulfur in stibnite, no suitable simple one has been found. Preparation process Directly prepare good antimony sulfide thin films from minerals

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Cut the copper foil used in batteries such as sodium-ion batteries, lithium-ion batteries, and solid-state thin-film batteries into a rectangular substrate of 10mm*20mm. At the same time, pre-cut a piece of white glass into a rectangle of 10mm*20mm (for detection). The rectangular white glass slices were ultrasonically cleaned with deionized water, glass cleaner, acetone, alcohol, and deionized water for 15 minutes, and then dried with an air compressor.

[0035] (2) Weigh 0.40 g of stibnite powder into a porcelain boat, and then put the porcelain boat and the stibnite powder into the middle of the temperature zone of the tubular annealing furnace.

[0036] (3) Put the required deposition film copper foil substrate and white glass into the suction end of the glass tube in the dual temperature zone tube furnace, and place it at the furnace mouth of the dual temperature zone tube furnace. Connect the glass tube and the mechanical pump with a flange, and turn on the m...

Embodiment 2

[0045] (1) The thickness is 1.1mm, resistance ≤ 14Ω / m 2 1. ITO conductive glass with a light transmittance ≥ 90% (Wuhan Jingge Solar Technology Co., Ltd.), pre-cut into 2 pieces of square substrate sheets of 50mm*50mm. The square slices were ultrasonically cleaned with deionized water, glass cleaner, acetone, alcohol, and deionized water for 15 minutes, and then dried with an air compressor for use.

[0046] (2) A 50nm CdS electron transport layer was deposited on the ITO conductive glass sheet to be used by a chemical water bath method.

[0047] Specifically, 160 milliliters of deionized water was added to a 250 milliliter beaker, and then 0.03 mol / liter of cadmium sulfide solution, 1.5 mol / liter of thiourea and 14.5 milliliters of 25% ammonia were added to the beaker, Then put the beaker with the ITO conductive glass sheet into a heat-collecting constant temperature heating magnetic stirrer and conduct a water bath at 80°C. After 3-6 minutes, the solution turns orange, and ...

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Abstract

The invention discloses a method for preparing an antimony sulfide thin film, wherein the raw material for preparing the antimony sulfide thin film is antimony mineral which has been simply screened. The present invention utilizes the difference in melting point between antimony sulfide and other impurities in antimony minerals, and combines the one-step treatment of coating and annealing in a tubular annealing furnace to prepare a film with properties comparable to those prepared by using high-purity antimony sulfide (≥99.999%) as a raw material. film. In the process of preparing antimony sulfide film, the present invention can not only avoid the environmental pollution problem produced in the process of preparing high-purity antimony sulfide raw material, but also solve the problem of impurities and less sulfur in the preparation of antimony sulfide film from stibnite, and the process The process is simple and efficient, greatly reduces the preparation cost, is stable and reliable, and has a wide range of applications. It is suitable for most substrates that need to be coated with antimony sulfide. It is an energy-saving, efficient, green and environmentally friendly method.

Description

technical field [0001] The invention relates to the technical field of battery thin film manufacturing, in particular to a preparation method of an antimony sulfide thin film battery material. Background technique [0002] China is a country with large antimony resources in the world. There are more than 120 kinds of antimony minerals identified at present, and 70 kinds are more common, but only more than 10 kinds have industrial utilization value. antimony ore. China is the world's most important antimony-producing country, with reserves ranking first in the world. There are 111 antimony producing areas, especially the tin mines in Hunan, known as the "world's antimony capital". In addition, there are antimony deposits in Guizhou, Guangxi, Guangdong, Yunnan and other provinces. [0003] The main component of stibnite is antimony sulfide (Sb 2 S 3 ). Antimony sulfide is a V-VI group sulfide semiconductor, which belongs to the orthorhombic crystal system, and the space g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/06C23C14/24C23C14/58
CPCC23C14/0623C23C14/24C23C14/5806
Inventor 刘芳洋吴杰韩璐曾溢宇孙振陈佳蒋良兴贾明刘业翔
Owner CENT SOUTH UNIV
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