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Preparation method of copper-indium-gallium-selenium alloy

A copper indium gallium selenide and alloy technology, which is applied in the field of preparation of copper indium gallium selenide alloy, can solve the problems of increasing production steps, long production cycle, difficult control of product components, etc., and achieves the effects of high yield and low impurity content.

Active Publication Date: 2017-10-13
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the vacuum one-step synthesis method is to synthesize copper indium gallium selenide alloy in a quartz tube by means of segmented horizontal heating. Please refer to the Chinese invention patent CN201010571436.8. Less, relatively low production capacity, and the quartz tube is a consumable, so the production cost is high
The two-step synthesis method generally synthesizes binary or ternary alloys first, and then synthesizes them again. The production cycle is long, and the product components are not easy to control. This increases the production steps and increases the risk of impurity introduction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0017] The preparation method of a kind of copper indium gallium selenide alloy of the present invention comprises the following steps:

[0018] S1: Feeding: Under certain pressure conditions, simple copper, indium, gallium, and selenium are used as raw materials. The four raw materials exist in the form of pellets or blocks. The four raw materials are based on the mass ratio of selenium: indium: gallium: copper = 15~100 : 50~180: 10: 37.7~298 Put selenium, indium, gallium, and copper into the crucible in turn, seal the crucible and place the crucible in a closed heat-resistant container;

[0019] S2: Vacuumize and remove oxygen: vacuumize the heat-resistant container to 1×10 -3 ~1Pa, then pass in an inert gas to 0.1~0.15 MPa, then evacuate to 1~10 Pa, remove all the oxygen in the heat-resistant container, and finally pass in an inert gas to adjust the pressure in the heat-resistant container to 1.3~3.0MPa;

[0020] S3: Heating: heat up to 750~900°C in the heat-resistant cont...

Embodiment 1

[0027] Take 5N selenium grain / block, 5N indium block, 5N gallium block, 5N copper grain / nail (1-5mm copper grain is suitable), according to the mass ratio selenium: indium: gallium: copper = 36:50:10:90 Ingredients 6000g, put the selenium material on the bottom layer of the high-purity graphite crucible, then put in indium and gallium, and finally put copper on the top layer, seal the crucible and put the crucible in a closed heat-resistant container, and then vacuumize the heat-resistant container to 1Pa, then pass high-purity nitrogen until the pressure inside the heat-resistant container is 0.1 MPa, then evacuate to below 10Pa, and finally pass high-purity nitrogen to adjust the pressure inside the heat-resistant container to 1.3MPa, and raise the temperature of the heat-resistant container to 750 ℃ and keep it warm for 30 minutes, then raise it to 1200 ℃ for 1 hour and keep it warm for 4 hours; after cooling down to 50 ℃ in the heat-resistant container, exhaust and release ...

Embodiment 2

[0030] Take 5N selenium grain / block, 5N indium block, 5N gallium block, 5N copper grain / nail (1-5mm copper grain is suitable), according to the mass ratio of selenium:indium:gallium:copper=46:66:10:113 The ingredients are 6000g, put the selenium material on the bottom layer of the high-purity graphite crucible, then put in the elemental indium and gallium, and finally put the copper particles on the top layer, seal the crucible and put the crucible in a closed heat-resistant container, and then put it in the heat-resistant container Vacuumize to 0.1Pa, then pass high-purity nitrogen until the pressure inside the heat-resistant container is 0.12 MPa, then evacuate to below 5Pa, and finally pass high-purity nitrogen to adjust the pressure inside the heat-resistant container to 1.6MPa, and heat up the heat-resistant container for 1 hour Heat to 850°C, keep warm for 20 minutes, then raise the heat-resistant container to 1300°C for 5 hours and keep warm for 5 hours; then cool the he...

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Abstract

The invention relates to a preparation method of a copper-indium-gallium-selenium alloy. The preparation method comprises the following steps of S1, material charging; S2, vacuum pumping and deoxygenating; S3, heating; and S4, cooling. According to the preparation method of the copper-indium-gallium-selenium alloy, a preparation technology different from the prior art is adopted, the defects existing in the prior art are overcome, and the prepared copper-indium-gallium-selenium alloy is high in product yield and little in impurity content and accords with the tendency of technological development.

Description

technical field [0001] The invention relates to a method for preparing an alloy, in particular to a method for preparing a copper indium gallium selenide alloy. Background technique [0002] copper indium gallium selenide alloy (CuIn x Ga (1-x) Se 2 , abbreviated as CIGS) are often used to prepare thin-film solar cells, which have the advantages of good stability, low cost, and high light conversion efficiency. In recent years, the record of the highest photoelectric conversion efficiency of small sample CIGS thin film solar cells has been repeatedly refreshed. At present, the conversion rate of CIGS thin film prepared by ZSW in Germany using the three-step method has reached 20.3%, ranking first among all kinds of thin film solar cells, close to crystalline silicon The cost of solar cells is one-third of that of crystalline silicon cells, so it is called "a very promising new thin-film solar cell in the next era" internationally. The conversion efficiency and output of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C30/02C22C1/02C22C1/10
CPCC22C1/02C22C1/1036C22C30/02C22C1/1047
Inventor 朱刘王波康冶
Owner FIRST RARE MATERIALS CO LTD