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CIGS thin film preparation method by using supercritical fluid for low-temperature selenizing

A supercritical fluid and thin film technology, applied in semiconductor devices, final product manufacturing, sustainable manufacturing/processing, etc., can solve the problems of flammability and explosion, high toxicity of Se, poor effect, etc., and achieve easy availability of raw materials and easy industrialization. , the effect of simple process

Inactive Publication Date: 2015-02-18
徐东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with this method is that the surfactant on the CIGS nanocrystalline particles is not easy to remove in the traditional selenization atmosphere, and carbon residues are easy to remain between the grain boundaries, which makes it difficult to form larger CIGS particles and form continuous particles. CIGS Thin Film
[0008] At present, CIGS / CIS / CGS / CIGSS thin films usually undergo selenization annealing treatment, and the conversion efficiency of thin films without selenization annealing treatment is often poor
The traditional selenization annealing treatment has a high selenization temperature (400~550°C), and the selenium source can be roughly divided into two types: one is the selenization of elemental Se powder and Se vapor; the other is the use of H 2 Se selenization, Se vapor toxicity is small, but the effect is poor; and H 2 Although Se selenization effect is good, but H 2 Se is highly toxic, flammable and explosive

Method used

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  • CIGS thin film preparation method by using supercritical fluid for low-temperature selenizing
  • CIGS thin film preparation method by using supercritical fluid for low-temperature selenizing
  • CIGS thin film preparation method by using supercritical fluid for low-temperature selenizing

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preparation example Construction

[0030] The embodiment of the present invention provides a method for preparing CIGS thin film by supercritical fluid low-temperature selenization. For the preparation method, see figure 1 shown. The method for preparing CIGS film by supercritical fluid low-temperature selenization comprises the following steps:

[0031] S01. After mixing cuprous chloride, indium chloride, gallium chloride and selenium powder, they are added to alkylamine for reaction to obtain CIGS nanocrystals;

[0032] S02. Coating the CIGS nanocrystals on the substrate: mixing and dispersing the CIGS nanocrystals with an organic solvent to obtain a CIGS nanocrystal ink, immersing the substrate in the CIGS nanocrystal ink, and dipping and pulling for coating, After drying, a coated substrate is obtained;

[0033] S03. The substrate coated with CIGS nanocrystals is subjected to selenization treatment: the coated substrate and the supercritical fluid solution are separated and placed in a closed environment,...

Embodiment 1

[0060] A method for preparing CIGS film by supercritical fluid low-temperature selenization, comprising the steps of:

[0061] (1) Preparation of CIGS nanocrystals: in N-rich 2 In the glove box, weigh 10mmolCuCl, 7mmolInCl 3 , 3mmolGaCl 3 and 20mmol Se were placed in a 250mL three-necked flask with a condenser tube and a stopcock; after closing the stopcock, the device was removed from the glove box, and the stopcock port of the device was immediately connected to the Schlenk tube. After the flask was wrapped with quartz wool, it was placed in a heating mantle, and 100 ml of oleylamine was injected into the flask. Open the piston and vacuumize at 100°C for 1h to remove water and oxygen in the device; 2 The reaction was carried out under magnetic stirring at 130° C. for 1 h under bubbling. Then the temperature was raised to 220° C. and reacted for 4 h under vigorous stirring, then the heating mantle was removed, and the reactant was cooled to room temperature.

[0062] Th...

Embodiment 2

[0071] A method for preparing CIGS film by supercritical fluid low-temperature selenization, comprising the steps of:

[0072] (1) Preparation of CIGS nanocrystals: in N-rich 2 In the glove box, weigh 2mmolCuCl, 0.18mmolInCl 3 , 0.2mmolGaCl 3 and 4mmolSe were placed in a 100mL three-neck flask with a condenser tube and a stopcock; after closing the stopcock, the device was removed from the glove box, and the stopcock port of the device was immediately connected to the Schlenk tube. The flask was wrapped with quartz wool and placed in a heating mantle, and then 10 ml of oleylamine was injected into the flask. Open the piston and vacuumize at 100°C for 1h to remove water and oxygen in the device; 2 The reaction was carried out under magnetic stirring at 130° C. for 1 h under bubbling. Then the temperature was raised to 220° C. and reacted for 3 h under vigorous stirring, then the heating mantle was removed, and the reactant was cooled to room temperature.

[0073] The speci...

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Abstract

The invention belongs to the field of photoelectric materials and provides a CIGS thin film preparation method by using supercritical fluid for low-temperature selenizing. The method includes: firstly, preparing forbidden-band-adjustable CIGS nanocrystals by a particle method, then preparing a film-coated substrate in gradient distribution by a dip-coating method, and finally, using the supercritical fluid for selenizing the film-coated substrate at a low temperature of 100-400 DEG C so as to obtain a continuous CIGS thin film. The CIGS thin film preparation method has the advantages that a process of using the supercritical fluid for low-temperature selenizing to prepare the CIGS nanocrystal thin film can be conducted at the lower temperature of 100-400 DEG C, thus, film coating performed on the flexible substrate with low bearing temperature is benefited, using high-toxic H2Se is avoided during selenizing by the supercritical fluid, and good selenizing effects can be gained and crystal boundaries can be better eliminated.

Description

technical field [0001] The invention belongs to the field of new energy sources of photoelectric materials, and in particular relates to a method for preparing CIGS thin films by low-temperature selenization of supercritical fluids. Background technique [0002] At present, due to the impact of the global energy crisis, solar energy has become a hot spot for alternative energy. Copper indium sulfide (CIS) thin-film solar cells (including copper indium sulfide, copper gallium selenide, copper gallium sulfide, copper indium gallium selenide (hereinafter referred to as CIGS), copper indium gallium sulfide and copper indium gallium sulfide selenide, etc.) The optoelectronic properties and structural stability of the material are recognized as one of the most promising third-generation photovoltaic materials. Although the current highest efficiency of CIGS thin-film solar cells is 20.3% created by the traditional vacuum process, the traditional vacuum method cannot overcome high...

Claims

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Application Information

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IPC IPC(8): H01L31/18C23C24/08
CPCC23C24/10H01L31/03923H01L31/18Y02E10/541Y02P70/50
Inventor 徐东仁昌义
Owner 徐东
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