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Preparation method of indium oxide with controllable crystal form

An indium oxide, crystal form technology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of difficult industrial application, difficult adjustment, discontinuous reaction process, etc. The effect of mass transfer efficiency

Active Publication Date: 2019-01-15
TSINGHUA UNIV
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  • Claims
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Problems solved by technology

However, it is generally difficult to adjust by adding surfactants.
Moreover, the hydrothermal method usually requires several hours or even several days of reaction time, and the reaction process is not continuous, so it is not easy for industrial application.

Method used

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  • Preparation method of indium oxide with controllable crystal form
  • Preparation method of indium oxide with controllable crystal form
  • Preparation method of indium oxide with controllable crystal form

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preparation example Construction

[0020] The invention provides a method for preparing indium oxide with controllable crystal form, comprising the following steps:

[0021] In the microreactor, the indium chloride solution and the sodium hydroxide solution are mixed for a precipitation reaction to obtain a precipitated product, and the precipitated product is subjected to a high-temperature reaction in a coil to obtain an indium oxide precursor suspension;

[0022] The indium oxide precursor suspension is sequentially separated, washed, dried, and high-temperature roasted to obtain indium oxide; when the temperature of the high-temperature reaction is [100,140]°C, the obtained indium oxide has a cubic structure, and when the high-temperature reaction When the reaction temperature is [160,180]°C, the obtained indium oxide has a hexagonal structure.

[0023] In the present invention, in a microreactor, an indium chloride solution and a sodium hydroxide solution are mixed for a precipitation reaction to obtain a ...

Embodiment 1

[0035] 1) Prepare an indium chloride solution with a concentration of 1g / L, and make it flow into the microreactor at a flow rate of 5mL / min.

[0036] 2) Prepare a sodium hydroxide aqueous solution with a concentration of 2mol / L, and make it flow into the microreactor at a flow rate of 5mL / min, realize rapid mixing of the two phases by shearing the dispersed phase, and pass it into the subsequent coil.

[0037] 3) Pass the mixed solution through a 16-meter-long coil pipe to continue the reaction at 140° C., and the reacted mixed solution is collected in a stirred tank after being cooled.

[0038] 4) Centrifuge the mixed liquid in the stirred tank, wash the obtained solid twice with deionized water and ethanol, and then dry to obtain the precursor powder.

[0039] 5) Put the precursor powder in a muffle furnace and bake it at 400°C to obtain a yellow indium oxide powder, denoted as a.

Embodiment 2

[0041] 1) Prepare an indium chloride solution with a concentration of 1g / L, and make it flow into the microreactor at a flow rate of 10mL / min.

[0042] 2) Prepare a sodium hydroxide aqueous solution with a concentration of 1mol / L, and make it flow into the microreactor at a flow rate of 10mL / min, realize rapid mixing of the two phases by shearing the dispersed phase, and pass it into the subsequent coil.

[0043] 3) Pass the mixed solution through an 8-meter-long coil pipe to continue the reaction at 100° C., and the reacted mixed solution is collected in a stirred tank after being cooled.

[0044] 4) Centrifuge the mixed liquid in the stirred tank, wash the obtained solid twice with deionized water and ethanol, and then dry to obtain the precursor powder.

[0045] 5) Put the precursor powder in a muffle furnace and bake it at 400°C to obtain a yellow indium oxide powder, denoted as b.

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Abstract

The invention provides a preparation method of indium oxide with controllable crystal forms, and belongs to the field of inorganic material preparation. In a microreactor, fluid cross-flow shearing isused for realizing fast mixing of indium chloride solution and sodium hydroxide solution; the mass transfer efficiency of the system is effectively improved; the mixing requirements in the fast precipitation process are met; meanwhile, a continuous coil pipe is continuously introduced for high-temperature reaction; fast growth of particles in indium oxide precursor suspension is realized; temperature regulation is utilized; the crystal formation transition is realized in the growth process; indium oxide of different crystal form structures is finally prepared.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to a preparation method of indium oxide with controllable crystal form. Background technique [0002] Indium oxide is an n-type semiconductor material with excellent photoelectric performance and good transmission performance for visible light. Therefore, ITO (indium tin oxide) thin films are widely used in the field of optoelectronic displays, such as liquid crystal displays, OLEDs, and the like. Currently, 85% of the world's indium resources are used to synthesize indium oxide. At the same time, because the surface of indium oxide reacts obviously to redox gases, it is also widely used in the production of gas sensitive elements. Indium oxide has two crystal structures, cubic and hexagonal. The crystal structure has a significant impact on the performance of the final product. For example, the sintering performance of the cubic structure is better, whi...

Claims

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Application Information

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IPC IPC(8): C01G15/00
CPCC01G15/00
Inventor 王玉军王景绰白少清骆广生
Owner TSINGHUA UNIV
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