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Single crystal submicron cu 2 znsns 4 High temperature solvothermal preparation method and application of particles

A submicron-scale, high-temperature solvent technology, applied in the direction of solution from liquid solvent at room temperature, single crystal growth, single crystal growth, etc., can solve the poor crystallinity of copper-zinc-tin-sulfur nanoparticles and the characteristics of copper-zinc-tin-sulfur nanocrystals Small peak intensity, long reaction time and other problems, to achieve the effect of easy large-scale application and promotion, good crystallinity, and short preparation cycle

Active Publication Date: 2017-01-18
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

[0004] On April 16, 2014, the Chinese invention patent CN102674435B disclosed a solvothermal synthesis method of copper-zinc-tin-sulfur nanocrystals. The method reacted at 130-140°C for 15h-20h to obtain CZTS nanocrystals. The prepared copper-zinc The characteristic peak intensity of tin-sulfur nanocrystals is small, which indicates that the prepared powder is copper-zinc-tin-sulfur nanoparticles with poor crystallinity
In addition, the solvothermal method generally uses a reaction temperature of about 140-200°C to obtain CZTS powder. The particle size obtained is at the nanometer level, and the crystallinity cannot be compared with the CZTS prepared by the vacuum method. There are many intrinsic defects and the density is not high. In addition, the reaction time required to prepare materials is also longer, usually 18-30h

Method used

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  • Single crystal submicron cu <sub>2</sub> znsns <sub>4</sub> High temperature solvothermal preparation method and application of particles
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  • Single crystal submicron cu <sub>2</sub> znsns <sub>4</sub> High temperature solvothermal preparation method and application of particles

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Embodiment 1

[0025] like figure 1 As shown, a single crystal submicron Cu of the present invention 2 ZnSnS 4 The specific steps of the high-temperature solvothermal preparation method of (CZTS) particles are as follows:

[0026] The first step, get the copper acetate monohydrate solution of 1mmol / L, the zinc acetate solution of 0.5mmol / L, the tin tetrachloride pentahydrate solution of 0.5mmol / L and the L-cysteine ​​of 3mmol / L respectively, press The volume ratio is 1:1:1:1 to form a mixed solution and place it in a stainless steel reaction kettle, then pour it into analytical pure anhydrous ethanol for dilution to obtain a reaction precursor solution; the volume ratio of the mixed solution to analytical pure anhydrous ethanol is 1:1, the stainless steel reactor is polished with graphite powder before use.

[0027] In the second step, seal the stainless steel reaction kettle and place it in a high-temperature blast oven. Adjust the temperature rise rate of the oven to 10°C / min, keep it a...

Embodiment 2

[0033] The first step, get the copper acetate monohydrate solution of 0.5mmol / L, the zinc acetate solution of 0.5mmol / L, the tin tetrachloride pentahydrate solution of 0.5mmol / L and the L-cysteine ​​of 4mmol / L respectively, According to the volume ratio of 1:1:1:1, the mixed solution is formed and placed in a stainless steel reaction kettle, and then poured into analytical pure anhydrous ethanol for dilution to obtain a reaction precursor solution; the volume ratio of the mixed solution to analytical pure anhydrous ethanol The ratio is 1:1, and the thread of the stainless steel reactor is polished with graphite powder before use; the rest of the steps are the same as in Example 1.

Embodiment 3

[0035]The first step, get respectively the copper acetate monohydrate solution of 0.7mmol / L, the zinc acetate solution of 0.5mmol / L, the tin tetrachloride pentahydrate solution of 0.5mmol / L and the L-cysteine ​​of 4mmol / L, According to the volume ratio of 1:1:1:1, the mixed solution is formed and placed in a stainless steel reaction kettle, and then poured into analytical pure anhydrous ethanol for dilution to obtain a reaction precursor solution; wherein, the volume of the mixed solution and analytical pure anhydrous ethanol The ratio is 1:1, and the thread of the stainless steel reactor is polished with graphite powder before use; the rest of the steps are the same as in Example 1.

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Abstract

The invention discloses a high temperature solvent thermal preparation method and applications of a monocrystalline submicron Cu2ZnSnS4 particle, and belongs to the technical field of nano material synthesis. The method comprises the following steps: individually fetching a copper salt solution, a zinc salt solution, a tin salt solution, and a sulfur source solution, adding the solutions into a reactor in order, then diluting the mixed solution with waterless ethanol so as to obtain a precursor solution, sealing the reactor, heating to a temperature of 300 to 400 DEG C, maintaining the temperature for 1 to 12 hours, taking out the black powder in the bottom layer of the reactor, carrying out centrifugation, and washing so as to obtain the target product. Under a condition of high temperature, CZTS particles, which have excellent crystallizing performance and do not contain any impurity phase, can be synthesized within a short time period. The CZTS particle has a good crystallizing performance and a monocrystal structure, the performance of the obtained CZTS particle is similar to that of a sample which has been vulcanized and annealed, the particle size of the CZTS particle is in a submicron level, and the post annealing treatment is not required. The invention further discloses the applications of the CZTS particle in solar cell and photocatalysis.

Description

technical field [0001] The present invention relates to a Cu 2 ZnSnS 4 Particle preparation method and application, specifically a kind of single crystal submicron Cu 2 ZnSnS 4 The high-temperature solvothermal preparation method and application of particles belong to the technical field of nanomaterial synthesis. Background technique [0002] With the depletion of fossil fuels and the environmental pollution caused during their use, the development of new energy-saving and environmentally friendly energy devices has become an important way to solve energy and environmental problems. Among them, solar cells have a wide range of applications, clean and The virtues of pollution have been the subject of intense research. With the widespread use of photovoltaic modules, how to obtain high-efficiency, green, and low-cost solar energy absorbing materials is a research hotspot in photovoltaic power generation. [0003] In 1996, the Japanese H. Katagiri research group prepared ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C30B29/46C30B29/60H01L31/032C01G19/00
Inventor 陶杰陈善龙陶海军沈一洲朱露敏曾小飞蒋佳佳
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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