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A kind of preparation method of three-dimensional hollow cuins2 microsphere

A three-dimensional hollow, microsphere technology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of high equipment requirements, poor system controllability and repeatability, long reaction time, etc. Improved stability and reproducibility, favorable photocurrent transmission, and good photoelectric performance

Active Publication Date: 2016-06-15
WENZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These three-dimensional CuInS 2 The common feature of the preparation method is: the use of one-dimensional CuInS 2 Three-dimensional CuInS prepared by self-assembly 2 , the semiconductor particles obtained in this way are relatively large, which is not convenient for making devices; moreover, the obtained three-dimensional CuInS 2 The microspheres all have tetragonal chalcopyrite structure; in addition, the solvothermal method requires pressurization, which requires high equipment, long reaction time makes the production cycle long, and the preparation conditions of the precursor are harsh. Some solvents used have certain toxicity, There are potential safety hazards and increased production costs. The reaction has high requirements on the ratio of materials and the filling ratio of the reactor, and the system has poor controllability and repeatability, which hinders the scale-up of the experiment and is not conducive to large-scale production.

Method used

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  • A kind of preparation method of three-dimensional hollow cuins2 microsphere
  • A kind of preparation method of three-dimensional hollow cuins2 microsphere
  • A kind of preparation method of three-dimensional hollow cuins2 microsphere

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preparation example Construction

[0049] Preparation of indium source

[0050] Take by weighing 5.13g (30mmol) sodium diethyldithiocarbamate (Nadedc) and add in the beaker, add the deionized water of 200mL in the beaker, stir at room temperature for 30 minutes and make it dissolve completely (the aqueous solution is colorless, clear and transparent) ) to obtain sodium diethyldithiocarbamate aqueous solution; Weigh 2.92g (10mmol) indium acetate and join in another beaker, add 50mL deionized water in this beaker, stir at room temperature for 15 minutes and make it dissolve completely (aqueous solution It is colorless, clear and transparent) to obtain indium acetate aqueous solution; the prepared indium acetate aqueous solution is dripped into the aqueous solution of sodium diethyldithiocarbamate (the solution starts to become white turbidity), continue to stir magnetically at room temperature for 3 hours to completely react the raw materials after the dropwise addition; The white powder was dried in a vacuum ov...

Embodiment 1

[0052] Weigh 6.4mg (0.1mmol) of ultra-fine spherical copper powder with a diameter of 0.5-1.0μm and put it into a tube furnace, pass oxygen into the furnace at 60°C for 10 minutes to oxidize, and obtain the copper source product, which is copper oxide Copper powder coated structure.

[0053] Weigh 25mg (0.07mmol) copper diethyldithiocarbamate and put it into a round bottom flask, add 4mL dodecanethiol and 2mL oleylamine to it, put it in a constant temperature oil bath at 200°C for 10 minutes, and centrifuge the reacted solution Afterwards, the obtained precipitate was washed several times and centrifuged, and the final obtained precipitate was dried to obtain 5.0 mg of Cu 7 S 4 Nanocrystalline. The prepared Cu 7 S 4 The nanocrystals were dispersed in 10 mL of n-hexane to obtain Cu 7 S 4 The mass concentration of nanocrystals is 0.5 mg / mL of Cu 7 S 4 nanocrystal dispersion.

[0054] The copper source product prepared above, 10 μL of Cu 7 S 4The nanocrystal dispersion...

Embodiment 2

[0081] Weigh 6.4mg (0.1mmol) of ultra-fine spherical copper powder with a diameter of 0.5-1.0μm and put it into a tube furnace, and pass oxygen into the furnace at 60°C for 20 minutes to oxidize to obtain a copper source product, which is copper oxide Copper powder coated structure.

[0082] Weigh 10.8mg (0.03mmol) of copper diethyldithiocarbamate into a round bottom flask, add 2mL of dodecanethiol and 1mL of oleylamine to it, place it in a constant temperature oil bath at 220°C for 10 minutes, and centrifuge the reacted solution After separation, the resulting precipitate was washed multiple times and centrifuged, and the final resulting precipitate was dried to obtain 2.2 mg of Cu7 S 4 Nanocrystalline. The prepared Cu 7 S 4 The nanocrystals were dispersed in 10 mL of n-hexane to obtain Cu 7 S 4 The mass concentration of nanocrystals is 0.22 mg / mL of Cu 7 S 4 nanocrystal dispersion.

[0083] The copper source product prepared above, 15 μL of Cu 7 S 4 Nanocrystalline...

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Abstract

The invention discloses a preparation method of a three-dimensional hollow CuInS2 microsphere. The three-dimensional hollow CuInS2 microsphere is prepared from Cu7S4 as a catalyst, a copper oxide coated copper powder structure as a copper source, indium thiocarbamate as an indium source, oleylamine as an activating agent and dodecanethiol as a sulfur source and solvent by the steps of reacting at a relatively low temperature for a short time by a one-pot method and then performing centrifugal separation. The three-dimensional hollow CuInS2 microsphere prepared by the method has a hierarchical structure consisting of a hollow microsphere core and a surface nanobelt connected with the hollow microsphere core, wherein the diameter of the hollow microsphere core is 0.5 to 3.5 microns; the width of the surface nanobelt is 25 to 70 nm; and the length of the surface nanobelt is 250 to 550 nm. The three-dimensional hollow CuInS2 microsphere has a wurtzite and sphalerite coexisting crystalline phase structure, has excellent photoelectric property and is applicable to photoelectric devices. The method provided by the invention is simple and controllable, low in cost and short in technology period, and mass production can be realized.

Description

technical field [0001] The invention belongs to the field of photovoltaic materials, in particular to a three-dimensional hollow CuInS 2 Preparation method of microspheres. Background technique [0002] In today's increasingly tense energy and severe environmental problems, the development of low-carbon and environmentally friendly new energy materials and the optimization of the performance of traditional materials have become the direction guide for future material science research. As an "inexhaustible and inexhaustible" clean energy, solar energy has become a new type of energy that countries around the world focus on developing. Silicon-based solar cells are favored by people and are considered to be the most potential solar cells. However, the production process of monocrystalline silicon and polycrystalline silicon will produce large environmental pollution and energy consumption, which cannot meet the requirements of low-carbon environmental protection. Due to its ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00
Inventor 邹超马亚辉黄少铭杨云张礼杰
Owner WENZHOU UNIV