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Method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using triethylene tetramine auxiliary polyhydric alcohol solution

A technology of triethylenetetramine and copper indium aluminum selenium, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of difficult control of chemical components, unfavorable large-scale production, complicated operation, etc., and achieve product quality Phase stability, low cost, good repeatability

Inactive Publication Date: 2014-02-19
TIANJIN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the prior art, such as time-consuming, energy-consuming, high cost, complicated operation, unfavorable for large-scale production, and difficult control of chemical components. Ethylenetetramine is used as a reaction auxiliary agent to provide a method for preparing CIASe nanocrystals that is safe in process, beneficial to product purity and stoichiometric control, green, non-toxic, and low in cost

Method used

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  • Method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using triethylene tetramine auxiliary polyhydric alcohol solution
  • Method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using triethylene tetramine auxiliary polyhydric alcohol solution
  • Method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using triethylene tetramine auxiliary polyhydric alcohol solution

Examples

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Embodiment 1

[0032] The process parameters of Examples 1-6 are injection temperature / reflux temperature. As can be seen from Table 2, when the injection temperature / reflux temperature of Example 1 was 170 / 170°C, the synthetic product phases were CISe, CuSe, Se, and no target CIASe phase was generated, and its stoichiometry and reaction solution Cu: The stoichiometry of In:Al:Se=1:0.75:0.25:2 is quite different. The phases of the synthesis products of Examples 2-4 are CIASe and Se. The synthetic products of Examples 5 and 6 are a single CIASe phase. The stoichiometric ratios of Examples 2-6 are all close to the stoichiometric ratio of the reaction solution Cu:In:Al:Se=1:0.75:0.25:2, and Example 6 is the best. As the temperature increases, the morphology of the synthesized products changes from sheet to granular, and the products of Examples 5 and 6 are granular. From the above analysis, it can be seen that for the parameters of injection temperature / reflow temperature, Example 6 is the o...

Embodiment 6

[0033] The technological parameter of embodiment 6~9 is that the addition amount of TETA is different. Wherein the synthetic product of embodiment 7 and 9 is the mixed phase of CIASe and Se, and embodiment 6 and 8 is the single phase of CIASe. From the results of the stoichiometric ratio of the synthesized products in Examples 6-9, the stoichiometric ratio of Example 6 is closest to the stoichiometric ratio of the reaction solution Cu:In:Al:Se=1:0.75:0.25:2. The morphology of the synthesized products is granular. As can be seen from the above analysis, for the TETA addition parameter, Example 6 is the optimum TETA addition, which is 3ml.

[0034]Examples 10-15 are the results of changing the In:Al molar ratio of the reaction solution under the optimal process parameters of Example 6, that is, Al / (In+Al) is 0, 0.1, 0.2, 0.3, 0.4, 0.5, respectively. It can be seen from Table 2 that Examples 11-13 are single CIASe phases, and other secondary phases exist. With the increase of ...

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Abstract

The invention discloses a method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using a triethylene tetramine auxiliary polyhydric alcohol solution; the method is as follows: first, preparing a precursor solution, weighing copper chloride dihydrate, indium chloride tetrahydrate and aluminum chloride hexahydrate to dissolve in triethylene glycol, wherein the molar ratio of Cu / (In + Al) being 1, the molar ratio of In / Al being 7 ~ 10:0 ~ 3; then adding the triethylene glycol into a the three-port round-bottom flask, adding selenium powder, then adding polyvinylpyrrolidone to produce an anion source reaction based liquid; then putting the three-port round-bottom flask into a thermal-type reaction reflux device for synthesis of the CIASe (Cu-In-Al-Se) nanocrystalline. According to the method, a polyhydric alcohol solution chemical synthesis method is firstly used, triethylene tetramine is used as a reaction auxiliary agent, the method for synthesis of the CIASe (Cu-In-Al-Se) nanocrystalline is provided, and the method is safe in process, facilitates product purity and chemometry control, and is green, nontoxic, and low in cost.

Description

technical field [0001] The invention relates to nanometer materials, in particular to a method for synthesizing copper indium aluminum selenium nanocrystals from triethylenetetramine assisted polyol-based solution. Background technique [0002] As a representative light-absorbing semiconductor material for thin-film photovoltaic cells, copper indium selenium CuInSe 2 (CISe) compounds have the advantages of high visible light absorption coefficient, lower manufacturing cost and energy repayment time than crystalline silicon solar cells, good battery stability, almost no attenuation, good weak light performance and high photoelectric conversion efficiency. However, since the bandgap of CISe is about 1.04eV, and the bandgap that best matches the solar spectrum is around 1.4eV, in order to achieve the most suitable bandgap, improve conversion efficiency and match with other layers, it is necessary to CISe is doped. Replace In in CISe with Al to form copper indium aluminum sele...

Claims

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Application Information

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IPC IPC(8): C01B19/00B82Y30/00
Inventor 靳正国王大龙
Owner TIANJIN UNIV
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