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Preparation method of large-particle-size indium oxide

An indium oxide, large particle size technology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of small particle size of indium oxide particles, large specific surface area, increased complexity and difficulty, etc. , to achieve the effect of easy enlargement, simplified process flow and easy operation

Active Publication Date: 2019-04-12
TSINGHUA UNIV
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Problems solved by technology

However, the indium oxide particles prepared by the traditional precipitation process of directly mixing raw materials have a smaller particle size and a larger specific surface area. In order to obtain particles with a larger particle size during target preparation, the calcination temperature needs to be increased (for indium oxide, The traditional calcination temperature is 400-600°C, and the particle size is 10-20nm. Increase the calcination temperature to 1000-1100°C, and the particle size can increase to 70-100nm), or add a large amount of surfactant, which greatly increases the target preparation. complexity and difficulty

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  • Preparation method of large-particle-size indium oxide
  • Preparation method of large-particle-size indium oxide
  • Preparation method of large-particle-size indium oxide

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preparation example Construction

[0023] The invention provides a preparation method of large particle size indium oxide, comprising the following steps:

[0024] (1) The indium chloride solution and the ammonia solution are respectively flowed into the membrane microreactor to carry out a co-precipitation reaction to obtain a seed solution;

[0025] (2) taking out the described seed crystal liquid, adding indium chloride solution and ammonia aqueous solution to the seed crystal liquid under heating conditions in parallel to obtain a reaction solution;

[0026] (3) centrifuging, washing and drying the reaction solution successively to obtain precursor powder;

[0027] (4) calcining the precursor powder to obtain large particle size indium oxide; the particle size of the large particle size indium oxide is ≥30 nm.

[0028] In the present invention, the indium chloride solution and the ammonia solution are respectively flowed into the membrane microreactor to carry out co-precipitation reaction to obtain the se...

Embodiment 1

[0036] (1) prepare an indium chloride solution with a concentration of 10 g / L, and make it flow into the microreactor at a flow rate of 5 mL / min;

[0037] (2) preparing the ammonia solution with a concentration of 1 mol / L, and making it flow into the microreactor at a flow rate of 5 mL / min, realizing rapid mixing of the two phases by shearing the dispersed phase, and carrying out a co-precipitation reaction;

[0038] (3) take 20mL of reacted slurry and flow into the three-necked flask to continue stirring, wherein the three-necked flask is placed in a water bath of 70°C;

[0039] (4) add 10 g / L of indium chloride solution and 1 mol / L of ammonia aqueous solution dropwise to a total of 80 mL at a flow rate of 1 mL / min;

[0040] (5) centrifugation of the mixed solution in the stirred tank, the obtained solid is washed twice with deionized water and ethanol, respectively, and is dried to obtain the precursor powder;

[0041] (6) The precursor powder is placed in a muffle furnace, a...

Embodiment 2

[0044] (1) prepare an indium chloride solution with a concentration of 50 g / L, and make it flow into the microreactor at a flow rate of 5 mL / min;

[0045] (2) The ammonia aqueous solution with a concentration of 2 mol / L is prepared, and it flows into the microreactor at a flow rate of 5 mL / min, and the two phases are rapidly mixed by shearing the dispersed phase, and a co-precipitation reaction is carried out;

[0046] (3) take 5mL of reacted slurry and flow into the three-necked flask to continue stirring, wherein the three-necked flask is placed in a water bath of 50°C;

[0047] (4) 100mL of indium chloride solution of 10g / L and ammonia solution of 1mol / L were added dropwise in parallel at a flow rate of 1mL / min;

[0048] (5) centrifugation of the mixed solution in the stirred tank, the obtained solid is washed twice with deionized water and ethanol, respectively, and is dried to obtain the precursor powder;

[0049] (6) The precursor powder is placed in a muffle furnace, a...

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Abstract

The invention provides a preparation method of a large-particle-size indium oxide, which comprises the following steps of: respectively flowing an indium chloride solution and an ammonia aqueous solution into a membrane microreactor for coprecipitation reaction, and dripping the obtained seed crystal solution into the indium chloride solution and the ammonia aqueous solution in parallel flow underthe heating condition, so as to obtain a reaction solution; then centrifuging, washing and drying the reaction solution in sequence to obtain a precursor powder, and roasting to obtain the large-particle-size indium oxide. According to the preparation method of a large-particle-size indium oxide, a precipitation method is used for preparing slurry as seed crystal liquid, indium chloride and the ammonia aqueous solution are dripped in parallel subsequently to promote the growth process of particles, the large-particle-size indium oxide particles are prepared through a seed crystal induction method, and the particle size regulation and control range of the indium oxide particles is expanded; Compared with the prior method for greatly improving the roasting temperature to obtain the particles with larger particle size, the preparation method of a large-particle-size indium oxide simplifies the process flow, saves energy, which is more convenient to operate and easy to amplify, and can prepare the indium oxide with the particle size of more than or equal to 30nm at the roasting temperature of 300-500 DEG C.

Description

technical field [0001] The invention relates to the technical field of semiconductor materials, in particular to a preparation method of large particle size indium oxide. Background technique [0002] Indium tin oxide (ITO) is an n-type semiconductor material with excellent optoelectronic properties. The thin film sputtered with ITO material has very low resistivity and good transmittance to visible light. Therefore, ITO films are widely used in liquid crystal displays, organic light emitting diodes, touch screens, solar cells and other fields. With the development of the current flat panel display industry, the requirements for ITO films are also developing towards large-scale, high-density, and high-purity. The properties of ITO films are fundamentally determined by the properties of ITO powders. Therefore, in order to meet the requirements of industrial development, the preparation process of ITO powders needs to be further optimized. [0003] ITO powder is a mixture o...

Claims

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Application Information

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IPC IPC(8): C01G15/00B82Y40/00
CPCB82Y40/00C01G15/00C01P2004/04C01P2004/64
Inventor 王玉军王景绰白少清骆广生
Owner TSINGHUA UNIV
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