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Method for preparing doping-type crystalline titanium dioxide photoelectrode at low temperature by virtue of microwave auxiliary reaction supercharge method

A titanium dioxide, microwave-assisted technology, applied in capacitor electrodes, circuits, electrical components, etc., can solve the problems of difficulty in preparing doped crystalline titanium dioxide, and achieve the effects of short preparation process time, high conversion efficiency, and good dispersion.

Inactive Publication Date: 2013-04-03
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a low-temperature preparation of doped crystalline titanium dioxide photoelectrodes by a microwave-assisted reaction pressurized method to solve the problem that it is difficult to prepare doped crystalline titanium dioxide at a low temperature of 85-100°C

Method used

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  • Method for preparing doping-type crystalline titanium dioxide photoelectrode at low temperature by virtue of microwave auxiliary reaction supercharge method
  • Method for preparing doping-type crystalline titanium dioxide photoelectrode at low temperature by virtue of microwave auxiliary reaction supercharge method

Examples

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Effect test

Embodiment 1

[0021] Example 1: Add 0.07mol tetrabutyl titanate to 2.30mol ethanol, stir and mix evenly, add 0.013mol tantalum ethoxide, stir well, add 0.08mol concentrated nitric acid dropwise, stir for 5min, then slowly add 0.20mol deionized water , maintain high-speed stirring during the dropwise addition to obtain a mixed solution. Heat the above-prepared mixed solution with a water bath at a temperature of 65° C., keep stirring and reflux, and react for 1 hour to prepare a colloid containing titanium and tantalum. After the colloid to be prepared is cooled to room temperature, move it into a high-pressure container, then add 2.90 mol of hydrogen peroxide, and quickly seal the container. Put the sealed container into a microwave reaction device with a microwave power of 200W, rapidly heat it to 95°C, keep it warm for 2.5h until the reaction is complete, and keep stirring during the whole process. The reaction product was filtered, rinsed with deionized water, and dried at 60° C. to obt...

Embodiment 2

[0026] Example 2: Add 0.05 mol tetrabutyl titanate to 1.60 mol ethanol, stir and mix evenly, add 0.03 mol zinc acetate, add 0.04 mol concentrated nitric acid dropwise after fully stirring, slowly add 0.10 mol deionized water dropwise after stirring for 5 minutes , maintain high-speed stirring during the dropwise addition to obtain a mixed solution. Heat the above-prepared mixed solution with a water bath at a temperature of 60° C., keep stirring and reflux, and react for 1.5 hours to obtain a colloid containing titanium and zinc. After the prepared colloid is cooled to room temperature, move it into a high-pressure container, then add 0.05mol zinc carbonate, and quickly seal the container. Put the sealed container into a microwave reaction device with a microwave power of 300W, rapidly heat it to 90°C, keep it warm for 2h until the reaction is complete, and keep stirring during the whole process. The reaction product was filtered, rinsed with deionized water, and dried at 60°...

Embodiment 3

[0027] Example 3: Add 0.20 mol tetrabutyl titanate to 3.05 mol isopropanol, stir and mix evenly, add 0.20 mol tin tetrachloride, add 0.15 mol concentrated nitric acid dropwise after fully stirring, slowly add 0.40 mol deionized water, keep stirring at a high speed during the dropwise addition to obtain a mixed solution. Heat the above-prepared mixed solution with a water bath at a temperature of 70° C., keep stirring and reflux, and react for 1 hour to prepare a colloid containing titanium and tin. After the colloid to be prepared is cooled to room temperature, move it into a high-pressure container, then add 0.04mol ammonium carbonate, and quickly seal the container. Put the sealed container into a microwave reaction device with a microwave power of 500W, rapidly heat it to 98°C, keep it warm for 2.5h until the reaction is complete, and keep stirring during the whole process. The reaction product was filtered, rinsed with deionized water, and dried at 60° C. to obtain tin-do...

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Abstract

The invention provides a method for preparing a doping-type crystalline titanium dioxide photoelectrode at low temperature by virtue of a microwave auxiliary reaction supercharge method and belongs to a low-temperature synthesis method of a solar battery photoelectrode. The preparation method comprises the following steps: 1, adding a titaniferous precursor into alcohol, uniformly mixing, then adding an adulterant, stirring, then adding a hydrolysis inhibitor, and slowly dropwise adding deionized water, thus obtaining a mixed solution; 2, heating the mixed solution in a water bath, stirring, refluxing and reacting until the reaction is over, thus obtaining a titaniferous and element-doped colloid; 3, cooling the colloid to room temperature, then transferring the cooled colloid into a high-pressure vessel, adding a decomposition agent and then rapidly sealing the vessel; 4, placing the vessel into a microwave reaction device, rapidly heating, keeping stirring, filtering reaction products, washing with deionized water, and drying, thus obtaining doping-type crystalline titanium dioxide. The method provided by the invention has the advantages that the doping-type crystalline titaniumdioxide with grains of about 120nm can be prepared at low temperature; the dispersibility is better; the preparation process time is shorter; and long-term follow-up high-temperature crystallization treatment is not required.

Description

technical field [0001] The invention relates to a low-temperature synthesis method of a photoelectrode of a solar cell, in particular to a low-temperature preparation of a doped crystalline titanium dioxide photoelectrode by a microwave-assisted reaction pressurized method. Background technique [0002] Doped titanium dioxide is the main material for photoelectrodes of solar cells, and its preparation methods can be divided into physical deposition and chemical preparation. The physical deposition method usually has a high deposition temperature, and the deposition equipment is complicated and expensive. Chemical preparation methods mainly include liquid phase precipitation method, sol-gel method and hydrothermal method. The liquid phase precipitation method and the sol-gel method prepare amorphous titanium dioxide. If it needs to be converted into crystalline titanium dioxide, subsequent high-temperature treatment is required; although the hydrothermal method can prepare c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G9/04H01G9/20H01M14/00H01L31/18
CPCY02P70/521Y02P70/50
Inventor 许程强颖怀朱亚波张生辉钟耀东许林敏刘炯天
Owner CHINA UNIV OF MINING & TECH
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