A kind of microwave hydrothermal method prepares the method for cualo2 thin film

A microwave hydrothermal method and thin film technology, which is applied in the field of preparing CuAlO2 thin films by microwave hydrothermal method, can solve the problems of high equipment requirements, complex process, poor repeatability, etc., and achieve the effects of low preparation cost, uniform particle size distribution and controllable shape.

Inactive Publication Date: 2012-02-15
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods either have high requirements on equipment, complex operation and high cost, or complex process, long cycle and poor repeatability, etc.

Method used

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  • A kind of microwave hydrothermal method prepares the method for cualo2 thin film

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Experimental program
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Effect test

Embodiment 1

[0014] Step 1: First, add analytically pure copper acetate monohydrate to ethylene glycol to prepare Cu 2+ A blue transparent solution with a concentration of 0.1mol / L, the resulting solution is denoted as A;

[0015] Step 2: then add analytically pure aluminum nitrate nonahydrate in the A solution, so that (Cu 2+ ): (Al 3+ )=1:1 molar ratio, and constantly stirring, while adding the HCOOH reagent with a molar fraction of 0.5%, adjusting the pH value to 2.0 under stirring to form a uniform precursor solution B;

[0016] Step 3: Soak the silicon substrate in HF solution with a volume concentration of 20% for 5 minutes, clean it with deionized water, and then perform ultrasonic cleaning with ethanol solution, then pour solution B into a hydrothermal reaction kettle, and the filling degree is controlled At 60%; place the silicon substrate after ultrasonic cleaning in the hydrothermal reaction kettle and immerse it in the B solution; then seal the hydrothermal reaction kettle an...

Embodiment 2

[0019] Step 1: First, add analytically pure copper acetate monohydrate to ethylene glycol to prepare Cu 2+ Concentration is the blue transparent solution of 0.2mol / L, and the obtained solution is recorded as A;

[0020] Step 2: then add analytically pure aluminum nitrate nonahydrate in the A solution, so that (Cu 2+ ): (Al 3+ )=1:1 molar ratio, and constantly stirring, while adding the HCOOH reagent with a molar fraction of 0.6%, adjusting the pH value to 3.0 under stirring to form a uniform precursor solution B;

[0021] Step 3: Soak the silicon substrate in HF solution with a volume concentration of 20% for 5 minutes, clean it with deionized water, and then perform ultrasonic cleaning with ethanol solution, then pour solution B into a hydrothermal reaction kettle, and the filling degree is controlled At 50%; place the silicon substrate after ultrasonic cleaning in the hydrothermal reaction kettle and immerse it in the B solution; then seal the hydrothermal reaction kettle ...

Embodiment 3

[0024] Step 1: First, add analytically pure copper acetate monohydrate to ethylene glycol to prepare Cu 2+ Concentration is the blue transparent solution of 0.4mol / L, and the obtained solution is recorded as A;

[0025] Step 2: then add analytically pure aluminum nitrate nonahydrate in the A solution, so that (Cu 2+ ): (Al 3+ )=1:1 molar ratio, and constantly stirring, while adding the HCOOH reagent with a molar fraction of 0.8%, adjusting the pH value to 4.0 under stirring to form a uniform precursor solution B;

[0026] Step 3: Soak the silicon substrate in HF solution with a volume concentration of 20% for 5 minutes, clean it with deionized water, and then perform ultrasonic cleaning with ethanol solution, then pour solution B into a hydrothermal reaction kettle, and the filling degree is controlled At 70%; place the silicon substrate after ultrasonic cleaning in a hydrothermal reaction kettle and immerse it in solution B; then seal the hydrothermal reaction kettle and pu...

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Abstract

A method for preparing CuAlO2 thin film by microwave hydrothermal method. First, copper acetate monohydrate is added to ethylene glycol to obtain solution A; then aluminum nitrate nonahydrate is added to solution A and the pH value is adjusted to 2.0-4.0 to form a uniform precursor material solution B; pour the B solution into the hydrothermal reactor, and immerse the silicon substrate in the B solution; seal the hydrothermal reactor, and put it into the MDS-8 type temperature-pressure dual-controlled microwave hydrothermal reactor; Select temperature control mode or pressure control mode for reaction and then naturally cool to room temperature; open the hydrothermal reactor, take out the silicon base, then wash several times with deionized water, absolute ethanol or isopropanol, and dry to obtain CuAlO2 film . The invention adopts microwave hydrothermal method to prepare CuAlO2 thin film. Not only the preparation cost is low, the operation is simple, and the reaction period is short, but also the product has high purity, complete grain development, uniform particle size distribution, controllable shape and no calcination treatment. The CuAlO2 thin film prepared according to the preparation method of the present invention is uniform and dense, and has strong bonding force.

Description

technical field [0001] The invention relates to a preparation method of a p-type transparent conductive oxide (TCO) film, in particular to a microwave hydrothermal method for preparing CuAlO 2 thin film method. Background technique [0002] CuAlO 2 It is a p-type transparent conductive oxide (TCO) material with direct and indirect band gaps of 1.8 and 3.5 eV, respectively, and a delafossite structure. Due to its high transparency (wide band gap) and conductivity in the visible range, it has been widely used It is used in solar cells, flat panel displays, special function window coatings and other optoelectronic devices. (Z. Deng, X. Zhu, R. Tao, W. Dong, X. Fang, Synthesis of CuAlO2 ceramics using sol-gel, Mater. Lett. 61 (2007) 686-689.) The emergence of TCO has opened up the research of optoelectronic devices However, the relative scarcity of p-type TCOs seriously restricts the development and application of transparent oxide semiconductor (TOS) related devices, and hin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/50
Inventor 黄剑锋李抗曹丽云吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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