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Preparation method of Cu-In-Ga-Se-S nano powder material

A copper indium gallium selenide sulfur and nano-powder technology, which is applied in chemical instruments and methods, selenium/tellurium compounds, inorganic chemistry, etc., can solve the problems of high price, increase the complexity and cost of process operation, and achieve low cost and easy operation. Control, short time effect

Inactive Publication Date: 2011-07-20
UNIV OF ELECTRONIC SCI & TECH OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solvents used in the above-mentioned "hot injection method" are expensive oleylamine, and CHCl needs to be added at the end of the reaction. 3 To terminate the reaction, in addition, in order to prevent the formation of by-products, it is necessary to add dispersants and flocculants at the same time to make the black CuInSe 2 Continuous powder precipitation increases the complexity and cost of process operation

Method used

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  • Preparation method of Cu-In-Ga-Se-S nano powder material
  • Preparation method of Cu-In-Ga-Se-S nano powder material
  • Preparation method of Cu-In-Ga-Se-S nano powder material

Examples

Experimental program
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Effect test

Embodiment 1

[0034] In the synthesis of CuInSe 2 In the process of nano powder, triethanolamine is used as solvent. During the reaction, triethanolamine participates in the reaction as a complexing agent and is finally reduced to triethanolamine. CuCl, InCl 3 4H 2 O and Se were refluxed at 220°C in triethanolamine solution to form CuInSe 2 Nano powder.

[0035] Weigh 2.5mmolCuCl and 2.5mmolInCl 3 4H 2 O in a 100mL three-necked flask filled with 50mL triethanolamine, stirred under inert gas protection conditions, and stopped heating when the oil bath was heated to 160°C, the color of the solution changed from light blue to dark blue and then reddish brown, counted as solution a. Weigh 5 mmol of Se powder and add it into a 100 mL three-necked flask filled with 50 mL of triethanolamine, and slowly raise the temperature to 240 °C. The solution immediately turns brown, which is designated as solution B. Mix solution A and solution B, stir under inert gas protection conditions, heat the ...

Embodiment 2

[0037] In the synthesis of CuInSe 2 In the process of nano-powder, the supernatant liquid after reaction is used as solvent. During the reaction, triethanolamine participates in the reaction as a complexing agent and is finally reduced to triethanolamine. CuCl, InCl 3 4H 2 O and Se were refluxed at 220°C in triethanolamine solution to form CuInSe 2 Nano powder.

[0038] Weigh 2mmolCuCl and 2mmolInCl 3 4H 2 O in a 100mL three-neck flask filled with 50mL of triethanolamine solution recovered after the reaction, stirred under inert gas protection conditions, and stopped heating when the oil bath was heated to 180°C. The color of the solution changed from light blue to dark blue and then to red. Brown, counted as solution A. Weigh 4mmol of Se powder and add it to a 100mL three-neck flask containing 50mL of triethanolamine solution recovered after the reaction, and slowly raise the temperature to 230°C. The solution immediately turns brown, which is designated as solution B....

Embodiment 3

[0040] In the process of synthesizing CuInGaSe nano powder, triethanolamine is still used as solvent.

[0041] Weigh 1mmolCuCl, 0.6mmolInCl 3 4H 2 O, 0.6mmol GaCl 3 In a 100mL three-necked flask filled with 25mL of triethanolamine solution, heat and stir in an oil bath, and at 200°C, these solid particles are all dissolved in the solvent under the protection of an inert gas, which is designated as A. Add 25mL of triethanolamine and 2mmol of Se powder into another 100mL three-necked flask, heat to 200°C, the Se powder is completely complexed, and the solution turns reddish brown, which is marked as B. Heat A to the reaction temperature, then quickly inject B, a large number of gray solid particles are formed, and then reflux for 4 hours, stop stirring and cool to room temperature, pour out the upper liquid, and centrifuge the lower black solid powder at 10,000 rpm for 30 minutes, Then wash with n-hexane, centrifuge 3 times, and vacuum-dry the centrifuged product at 40°C for ...

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Abstract

The invention provides a preparation method of a Cu-In-Ga-Se-S nano powder material, belonging to the technical field of inorganic chemical materials. The preparation method comprises the following steps: based on alkanolamine with a boiling point large than or equal to 180 DEG C as a solvent, dissolving Cu, In and Ga compounds into the alkanolamine in a mole ratio of Cu: (In+Ga) of 1: (1-1.5); then dissolving Se and S in the alkanolamine, wherein the sum of molar weights of Se and S is twice as heavy as molar weight of Cu; and subsequently, mixing two solutions, stirring under the protective condition of inert gas, heating to 200-280 DEG C for refluxing, maintaining the reaction for 4-10 hours and then stopping heating and stirring, cooling to room temperature, centrifuging, washing and drying the black powder on the lower layer, so as to obtain the Cu-In-Ga-Se-S nano powder material. By using the preparation method in the invention, the Cu-In-Ga-Se-S nano powder material which is in a nano grade and has uniform scale, good dispersibility and high phase purity can be prepared, the whole preparation process is high in efficiency and low in cost, and operation is simple and is easy to control. The Cu-In-Ga-Se-S nano powder material prepared by the method in the invention can be used in a solar battery as an absorption layer material.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical materials, and relates to a preparation method of copper indium gallium selenide sulfur compound nano powder material. Background technique [0002] CuInSe 2 、CuInS 2 , CuGaSe 2 , CuGaS 2 , Cu(In x Ga 1-x ) Se 2 (CIGS), Cu(In x Ga 1-x )S 2 and Cu(In x Ga 1-x )(Se y S 2-y ) etc. are collectively referred to as copper indium gallium selenide sulfur compounds. Because of its good light absorption properties, high stability, and unique structural and electrical properties, it has become a promising photovoltaic material. In particular, the conversion efficiency of solar cells using copper indium gallium selenide as the absorbing layer has exceeded 20%, which has become a research hotspot in this field and has attracted extensive attention from scientific research, development and industry. [0003] The existing preparation methods of copper indium gallium selenide sulfur powd...

Claims

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Application Information

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IPC IPC(8): C01B19/00
Inventor 吴孟强张树人张其翼刘文龙
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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