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Mass production device and mass production method of a chalcogen compound

A technology of chalcogen compounds and chalcogen elements, applied in the direction of binary selenium/tellurium compounds, tin compounds, chemical instruments and methods, etc., can solve problems such as evaporation and loss of highly volatile chalcogen elements, environmental threats, safety accidents, etc. To achieve the effect of maintaining consistency and stability

Active Publication Date: 2018-08-07
PIONEER MATERIALS INC CHENGDU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the vapor pressure of these elements leaks due to the damage of the reaction vessel, it is easy to react with the moisture in the surrounding atmosphere to form highly toxic H 2 Se, H 2 Te or H 2 S, etc., causing serious safety accidents and serious threats to the environment
[0007] Moreover, highly volatile chalcogen elements will evaporate and lose during the heating and melting reaction process, so that the atomic ratio of the final compound cannot be well controlled, and the technical indicators of the material cannot meet the requirements
[0008] In addition, the quartz tube reaction vessel can only be used once, resulting in waste and a corresponding increase in cost

Method used

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  • Mass production device and mass production method of a chalcogen compound
  • Mass production device and mass production method of a chalcogen compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1: CuSe 2 Compound preparation

[0065] The copper (Cu) and selenium (Se) pellets with a total weight of 4 kg and a purity >= 4N are in the atomic ratio Cu:Se=1:2, or the corresponding weight ratio Cu:Se=1:0.4, That is, 1.14Kg of copper and 2.86Kg of selenium are put into the quartz container 110, and the first flange 121, the second flange 122 and the nickel alloy gasket 124 are locked with screws. Start the vacuum pump to evacuate the system. When the vacuum reaches 5x10 -4 When Pa, close the VAT valve. The quartz vessel 110, the first flange 121 and the VAT valve form a sealed vacuum reaction space. In this embodiment, the thickness of the quartz container 110 is 4 mm, the ratio of the inner diameter to the length is 1:3, and the area ratio of the inner surfaces of the second part 112 and the first part 111 of the quartz container 110 is 2:1.

[0066] During the main reaction period: the first heating component 140 is controlled to raise the temperature ...

Embodiment 2

[0070] Example 2: As 2 Se 3 Compound preparation

[0071] Arsenic (As) and selenium (Se) small particles with a total weight of 2Kg and a purity of >=4N are according to the atomic ratio As:Se=2:3, or the corresponding weight ratio is the ratio of As:Se=0.63:1, namely , arsenic 0.77Kg, selenium 1.23Kg, put into the quartz container 110, and then the first flange 121, the second flange 122 and the nickel alloy gasket 124 are locked with screws. Evacuate the reaction vessel to a vacuum of 3x10 -4 Pa, and then close the VAT valve. The quartz vessel 110, the first flange 121 and the VAT valve form a sealed vacuum reaction space. In this embodiment, the thickness of the quartz container 110 is 6 mm, the ratio of the inner diameter to the length is 1:4, and the area ratio of the inner surfaces of the second part 112 and the first part 111 of the quartz container 110 is 2.5:1.

[0072] The process enters the main reaction period: the first temperature is controlled to rise at a ...

Embodiment 3

[0075] Embodiment 3: copper zinc tin sulfur CZTS (Cu 2 ZnSnS 4 ) Preparation of quaternary compounds

[0076] Quaternary alloy copper-zinc-tin-sulfur (CZTS), as a new generation of surface solar cell materials, has begun to attract the attention of the photovoltaic industry, especially its raw materials are abundant in the earth and the cost is very low. But its disadvantage is that when the quaternary compound is formed, the reaction is very violent, and because it contains highly volatile sulfur, it is difficult to control the atomic ratio between its elements. The molecular formula of copper zinc tin sulfur used in thin film photovoltaic materials is usually: Cu 2 ZnSnS 4 , the ideal atomic ratio is: Cu:Zn:Sn:S=2:1:1:4, and the corresponding weight percentages are: Cu29.04%, Zn14.53%, Sn27.13%, S29.30%. Put the copper, zinc, tin, and sulfur pellets with a total weight of 2Kg and a purity higher than 4N into the reaction vessel according to the weight: 0.58Kg of copper, ...

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Abstract

The invention provides a mass-production apparatus and a mass-production method for sulfur-group element compounds. In the invention, the whole reaction process is divided into a main reaction section and a reflux reaction section, which are respectively controlled by first and second heating assemblies that are individually arranged. During the main reaction section, a first portion of a quartz container is heated by the first heating assembly while the second heating assembly does not work so as to maintain a low temperature in a second portion of the quartz container, so that high-volatile sulfur-group elementary substance, which is evaporated to the second portion of the quartz container, is condensed and deposited on inner wall of the quartz container, thereby reducing the vapor pressure in the quartz container and preventing tube explosion; and then the second heating assembly heats the second portion of the quartz container, so that the deposited sulfur-group elementary substance flows back to the first portion and continuously participates in the reaction, thus maintaining the atom ratio of the target sulfur-group compound. The apparatus and the method are used for producing the sulfur-group element compound in large scale, are safe and are environment-friendly.

Description

technical field [0001] The invention relates to the field of preparation of chalcogen compounds, in particular to a mass production method and mass production device of chalcogen compounds. Background technique [0002] The use of vacuum melting to produce compounds is not a new technology. For example, vacuum induction melting (Vacuum Induction Melting), which is commonly used in the industry, uses the induction of alternating current to cause the metal conductor to generate eddy currents in a vacuum to heat until the metal melts and fully reacts, and finally crystallizes during cooling and forms related compounds. . But with many new technology applications, such as the new generation of non-volatile memory chips under development, many chalcogen compounds, such as GeSe 2 , GeAsSe, GeAsSeTe,As 2 Se 3 Wait. Especially for the new generation of thin film solar cells, copper indium gallium selenide (CuInGaSe, CIGS), copper zinc tin sulfur (Cu 2 ZnSnS 4 , CZTS) and In ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04C01G19/00
CPCC01B19/007C01G19/006
Inventor 李宗雨丘立安
Owner PIONEER MATERIALS INC CHENGDU
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