Process for liquid-phase synthesis of diindium triselenide in double temperature zone vacuum tight tube

A technology of diindium triselenide and liquid phase synthesis, applied in the direction of binary selenium/tellurium compounds, etc., can solve the problems of heterogeneous composition, long synthesis cycle, low production capacity, etc., to increase the output of a single furnace, speed up Synthesis speed and the effect of increasing the reaction temperature

Inactive Publication Date: 2011-12-14
江西科泰新材料有限公司
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AI Technical Summary

Problems solved by technology

Synthetic In 2 Se 3 The commonly used process is single temperature zone vacuum tight tube liquid phase synthesis method. The weakness of this method is that the synthesis period is long, and there is a possibility of cracking or explosion, so the production capacity is low, and the synthesis will also appear heterogeneous.

Method used

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Embodiment Construction

[0017] The vacuum-tight tube liquid-phase synthesis process of diindium triselenide in the present invention includes the following steps:

[0018] (1) Ingredients and packaging

[0019] The high-purity metal In of the first raw material 5N (representing a purity of 99.999%) is pressed and broken into small pieces or powder, and the high-purity metal Se of the second raw material 5N is also broken into small pieces and put into a quartz tube together. The measurement accuracy is 0.01%.

[0020] The wall thickness of the quartz glass tube is 2.5-3.5 mm, the diameter and length are Φ35 mm×450 mm, the charging capacity is 200-350 g, and the softening point is 1400 °C. The quartz tube needs to be cleaned with aqua regia, then washed with deionized water, and then dried with infrared rays. As long as there is a particle of dust in the tube, the purity of the raw material will be reduced. Use a vacuum unit composed of 2X-8 rotary mechanical pump and Φ200 mm oil diffusion pump to p...

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Abstract

A liquid phase synthesis process of diindium triselenide double-temperature zone vacuum tight tube is characterized by comprising the following steps: 5N high-purity metal In is pressed and broken into small blocks or powders, and 5N high-purity metal Se is also Crush into small pieces and put them into a quartz tube together, use a vacuum unit to evacuate the quartz tube to a vacuum of 10-3 Torr, and then seal the quartz tube; put the sealed tube filled with raw materials into a high-temperature box furnace for heating, and the double-temperature zone is dense. The tube synthesis method is that the sealed tube is kept at an atmospheric pressure, one end of the sealed tube is in the high temperature zone of the heating furnace, the temperature in the tube reaches 900-1000°C, and the other end is kept at 120-200°C in the water-cooled low-temperature zone, and the reaction in the tube is controlled. The In2Se3 compound was synthesized from In and Se within 4 hours; after the reaction in the tube was completed, the quartz tube was cut open, the In2Se3 pieces were poured out, and then vacuum-packed in a plastic bag with a vacuum degree of 10-1 Torr, and put into the finished product warehouse. The liquid phase synthesis process of the diindium triselenide double temperature zone vacuum tight tube of the invention is simple and safe in production.

Description

technical field [0001] The invention relates to a synthesis process of diindium triselenide. Background technique [0002] CIGS.S thin-film solar cells are now forwarding Indium Copper Selenium (In 2 Se 3 ) and Indium Copper Sulfur (In 2 S 3 ) are developing in two directions, and there is huge room for development in the development of raw materials and industrialization of these two batteries. Therefore, in the production of these two raw materials, the homogeneity of the materials and shortening the synthesis time, ensuring the safety and reliability of the production process, and increasing production capacity are issues of concern to everyone. [0003] The reaction of two elements, indium (In) and selenium (Se), can produce four kinds of compounds, namely In 2 Se (melting point 540 ℃), InSe (melting point 660 ℃), In 5 Se 6 (melting point 650 ℃), In 2 Se 3 (melting point 900°C). [0004] The melting point of the element In is 156.634 °C and the boiling poin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04
Inventor 舒小敏吴文斌
Owner 江西科泰新材料有限公司
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