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Preparation method of fine indium sulfide powder and target material

A technology of indium sulfide and powder, which is applied in the field of solar cell materials, can solve the problems of unfavorable grain size, large powder particle size, and small density, and achieve uniform resistivity, high density, and reduced grain size. Effect

Active Publication Date: 2021-08-06
先导薄膜材料(安徽)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, although the synthesis method of indium sulfide powder has been reported, the particle size of these powders is relatively large, which is not conducive to obtaining small grain size and high density target

Method used

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  • Preparation method of fine indium sulfide powder and target material
  • Preparation method of fine indium sulfide powder and target material
  • Preparation method of fine indium sulfide powder and target material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method of preparing a fine sulfide oxide powder, steps below:

[0032] Be in 3+ IN in the concentration of 100 g / L 2 (SO4) 3 The solution was added to the glass reaction kettle, and the stirring paddle was opened, and the mixing paddle rate was controlled at 200 rpm. Then, will h 2 The S gas is entry in the flow of 2 L / min. 2 (SO4) 3 In the solution until the reaction is completed. Then, the pure water is rinsed, and the cycle is filtered multiple times until the liquid in the reactor is not turbid. Take the sulfurized indium moisture in the filter bag, place in a clean quartz booon, then add the calcination in the quartz force, the calcination temperature is 450 ° C, heat insulation 120min, cool to room temperature, discharge. The material was placed in the ball grinding 10 min, and then sieved with a 325 mesh stainless steel screen to give indium oxide powder. Sampling, XRD and SEM analysis of sulfide sulfide powder, analysis results figure 1 and figure 2 .

[0033]...

Embodiment 2

[0036] A method of preparation of indium sulfide targets, as follows:

[0037] The fine sulfide produced in Example 1 was laid into the graphite mold, and then the graphite mold was placed in a vacuum hot press. First, the preload is performed at 2T / min to 10 MPa to exclude the air in the graphite mold, and the pressure is charged for 3 minutes to obtain an indium oxide billet. Then, when the furnace door is closed, the vacuum is vacumed to a vacuum to 5PA, start heating, warming up at 5 ° C / min to 700 ° C, heat insulation 120min; wherein the holding is 20 min, pressurize, pressurized to 30 MPa After 40 min, after the insulation is complete, slow down to 10 MPa until the insulation is over. Finally, the burner door is opened, the fireplace door is opened, and the indium sulfide blank target is obtained. The sulfide indium blank target is processed into the desired size to obtain an indium oxide target.

[0038] Density, resistivity, and crystal particle size detection of indiu...

Embodiment 3

[0040] A method of preparing a fine sulfide oxide powder, steps below:

[0041] Be in 3+ Ins with a concentration of 200g / L 2 (SO4) 3 The solution was added to the glass reaction kettle, and the stirring paddle was opened, and the stirring paddle rate was controlled at 300 rpm. Then, will h 2 S gas is entry in 3L / min 2 (SO4) 3 In the solution until the reaction is completed. Then, the pure water is rinsed, and the cycle is filtered multiple times until the liquid in the reactor is not turbid. Take the sulfurized indium moisture in the filter bag, place in a clean quartz booon, then add the calcination in the quartz force, the calcination temperature is 450 ° C, heat insulation 120min, cool to room temperature, discharge. The material was placed in the ball grinding 10 min, and then sieved with a 325 mesh stainless steel screen to give indium oxide powder. Sampling, XRD and SEM analysis of the sulfide oxide powder, analysis results are analyzed as the analysis result of the ind...

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Abstract

The invention discloses a preparation method of fine indium sulfide powder and a target material, and the preparation method of the fine indium sulfide powder comprises the following steps: introducing H2S gas into an In2 (SO4) 3 solution, reacting under stirring to synthesize indium sulfide, and after the reaction is finished, rinsing, filtering, calcining, ball-milling and sieving the synthesized product to obtain indium sulfide powder with the particle size D90 of 20-40 [mu] m; and allowing the indium sulfide powder to be subjected to airflow crushing, wherein the feeding pressure and crushing pressure of airflow crushing are 8-12 kg, the feeding speed is 3-5 kg / h, and continuing ventilation for 3-5 min after feeding is finished to obtain the fine indium sulfide powder with D90 smaller than 5 micrometers. The prepared indium sulfide powder is beta-In2S3 of a tetragonal structure, the particle size D90 is smaller than 5 microns, the indium sulfide powder is used for preparing the target material, the quality of the target material is improved, the average grain size of the target material is smaller than 5 microns, the resistivity is smaller than 0.5 K omega / cm, the relative density is larger than or equal to 97%, the impurity content is low, and a film formed through sputtering is good in stability, uniform in thickness distribution and consistent in grain size.

Description

Technical field [0001] The present invention relates to the technical field of solar cell material, and more particularly to a method of preparing a fine sulfide oxide powder and a target. Background technique [0002] With the growing population of the world and the continuous development of the economy, human society is increasingly demanding energy. Among them, the supply of traditional energy represented by oil and coal, etc. has increasingly difficult to meet the growing energy consumption. To this end, the development of new energy such as solar energy, wind energy, geothermal energy, biomass, and tidal energy is imminent. [0003] Indium hydraulide (in 2 S 3 It is an important semiconductor material with special photoelectric, photoluminescence and other properties, which have a large value in the fields of fuel cells, electrochemical sensors, and optoelectronic function materials. In 2 S 3 There are three different defective structures: α-in 2 S 3 (Defect Cube), β-in 2 S ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/547C04B35/626C04B35/622C04B35/645C01G15/00C23C14/34C23C14/06
CPCC04B35/547C04B35/626C04B35/622C04B35/645C01G15/00C23C14/3414C23C14/0623C04B2235/6562C04B2235/6567C04B2235/6581C04B2235/765C04B2235/786C04B2235/96C01P2004/61C01P2002/30
Inventor 沈文兴白平平童培云谢小豪
Owner 先导薄膜材料(安徽)有限公司
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