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Preparation method of indium oxide nano-powder

A nano-powder and indium oxide technology, which is applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of long preparation process cycle, complicated process, and environmental pollution, so as to achieve large-scale controllable production and avoid Emission of pollutants, the effect of simple preparation means

Active Publication Date: 2017-06-09
宁波甬兴电子有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

(3) The preparation process cycle is long: for example, in the process of preparing indium oxide powder by precipitation method, the precipitation reaction period is very long, and the precipitate needs to be washed many times, followed by drying and roasting; (4) it is easy to bring environmental pollution Pollution: For example, a large amount of water washing is required in the precipitation method, and if the waste water is not treated, it will cause environmental pollution; in the spray pyrolysis process, InCl 3 、In(ON) 3 Such precursor substances will be decomposed into HCl, NO and other gases, which will pollute the environment if they are discharged without treatment; (5) The overall cost is high: long preparation cycle, complicated process and environmental protection treatment of waste water and waste gas will lead to In 2 o 3 The production cost of nano powder is high

Method used

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  • Preparation method of indium oxide nano-powder

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Effect test

Embodiment 1

[0031] (1) Mix 90g of stearic acid and 12g of indium particles with a purity of 5N, continue to pass in 1L / min of argon gas, heat to 170°C while stirring, and keep for 10h until the indium particles are completely dissolved, and then cool to obtain organic Indium compounds;

[0032] (2) Add 13.6g of hydrogen peroxide and 3.6g of deionized water to the organic indium compound prepared in step (1), mix them and place them in a supercritical hydrothermal reactor for reaction, the reactor heating temperature is 290°C, and the reaction time is 3h, after the completion of the reaction, cool to room temperature, and obtain the reaction product by filtration;

[0033] (3) Calcining the reaction product in step (2) at 400°C in the air for 2 hours to obtain indium oxide nanopowder, the SEM characterization picture is as follows figure 1 As shown, the particle size of the obtained indium oxide nanopowder is 50-200 nm, the distribution is uniform, and the phase is a cubic phase structure...

Embodiment 2

[0035] (1) Mix 70g of capric acid and 12g of indium wire with a purity of 4N, continuously pass in 2L / min of argon gas, heat to 200°C while ultrasonically stirring, and keep it for 6h until the indium wire is completely dissolved, then cool to obtain organic Indium compounds;

[0036] (2) Add 15.1g of hydrogen peroxide and 3.9g of deionized water to the organic indium compound prepared in step (1), mix them and place them in a supercritical hydrothermal reactor for reaction, the reactor heating temperature is 350°C, and the reaction time is 2.5h, after the completion of the reaction, cool to room temperature, and obtain the reaction product by filtration;

[0037] (3) Calcining the reaction product in step (2) in air at 500° C. for 2.5 hours to obtain indium oxide nanopowder with a particle size of 100-300 nm, uniform distribution, and a cubic phase structure.

Embodiment 3

[0039] (1) Mix 85g of capric acid and 12g of indium particles with a purity of 4N, continuously feed 2L / min of titanium dioxide, heat to 270°C while stirring, and keep for 2h until the indium particles are completely dissolved, and cool to obtain an organic indium compound ;

[0040] (2) Add 11.5g of hydrogen peroxide and 2.0g of deionized water to the organic indium compound prepared in step (1), mix them and place them in a supercritical hydrothermal reactor for reaction, the reactor heating temperature is 450°C, and the reaction time is 1.5h, after the completion of the reaction, cool to room temperature, and obtain the reaction product by filtration;

[0041](3) Calcining the reaction product in step (2) in air at 650° C. for 2 hours to obtain indium oxide nanopowder with a particle size of 300-400 nm, uniform distribution, and a cubic phase structure.

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Abstract

The invention discloses a preparation method of indium oxide nano-powder. The preparation method comprises the following steps: (1) mixing metal indium with organic acid, and performing heating and dissolution in a protective gas to obtain an organic indium compound: (2) adding hydrogen peroxide and water in the organic indium compound, performing mixing, then placing the mixture into a supercritical hydrothermal reactor for reaction, and filtering after finish of reaction to obtain a reaction product; and (3) placing the reaction product obtained in the step (2) to be calclined in air to obtain the indium oxide nano-powder. The supercritical mode is adopted, so that the organic indium compound is finally converted into an In2O3 precipitate, CO2 and H2O; as a precipitator does not need to be additionally added, discharge of pollutants is avoided; and the preparation method is an environment-friendly preparation method, is simple in process, does not need complicated preparation processes, and can realize large-scale controllable production.

Description

technical field [0001] The invention belongs to the technical field of preparation of oxide nanomaterials, in particular to a preparation method of indium oxide nanopowder. Background technique [0002] In 2 o 3 It is a very important n-type wide bandgap transparent semiconductor material, which has both high visible light transmittance and high electrical conductivity. Due to its excellent properties, In 2 o 3 Base magnetron sputtering ceramic target (mainly doped SnO 2 , ZnO, etc.) have been widely used in solar cells, optoelectronic devices, liquid crystal displays, etc. Indium oxide powder is the main raw material required for the preparation of the above-mentioned ceramic targets, and its prerequisites are high purity, good dispersibility, fine and uniform particle size, and the ability to be scaled up. [0003] Preparation of In 2 o 3 There are many methods for powder, and the neutralization precipitation method is a kind of indium oxide powder manufacturing me...

Claims

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Application Information

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IPC IPC(8): C01G15/00B82Y40/00
CPCC01G15/00C01P2002/30C01P2004/03C01P2004/62C01P2004/64Y02P20/54
Inventor 宋伟杰杨晔李佳赵训娜王木钦兰品军
Owner 宁波甬兴电子有限公司
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