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High-dispersity indium oxide and preparation method thereof

A high-dispersion, indium oxide technology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve problems such as difficult to form large-scale production, achieve high-dispersion crystal structure, overcome easy agglomeration , the effect of uniform size distribution

Inactive Publication Date: 2021-04-13
FIRST RARE MATERIALS CO LTD
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  • Abstract
  • Description
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Problems solved by technology

For example: the Chinese patent with the publication number CN105683089A has prepared a high-density sintered body. By controlling the parameters of the electrolysis, an indium hydroxide powder with a specific crystal plane is prepared, that is, a highly crystalline indium hydroxide powder with a specific orientation index. , and then obtain indium oxide through pre-sintering, which avoids the problem of serious agglomeration of fine indium hydroxide synthesized by general electrolysis during the calcination process; Parameter monitoring puts forward higher requirements, and it is difficult to form large-scale production

Method used

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preparation example Construction

[0025] The invention provides a method for preparing highly dispersible indium oxide, comprising the following steps:

[0026] a) using metal indium as an anode, an inert electrode as a cathode, and an ammonium nitrate aqueous solution as an electrolyte, and obtaining an indium hydroxide slurry by electrolysis;

[0027] b) Add indium nitrate solution to the indium hydroxide slurry obtained in step a), so that the mass ratio of the added indium ions to indium hydroxide is 0.01% to 1%, and after adjusting the pH value to 4 to 8, carry out water Thermal reaction, the product is washed and dried to obtain highly crystalline and highly dispersible indium hydroxide powder;

[0028] c) Calcining the highly crystalline and highly dispersible indium hydroxide powder obtained in step b) to obtain highly dispersible indium oxide.

[0029] In the present invention, the indium hydroxide slurry is firstly obtained by an electrolysis method by using metal indium as an anode, an inert electr...

Embodiment 1

[0048] (1) Prepare indium hydroxide slurry with D50 less than 1 μm by electrolysis. In the electrolysis method of this embodiment, the anode and the cathode are installed in an electrolysis chamber at the same time. Ammonium nitrate aqueous solution with a concentration of 2.8mol / L, then heat the electrolytic chamber to 65°C, turn on the power, and set the current density to 500A / m 2 , and continued electrolysis for 15 hours to obtain a slurry with a D50 of less than 1 μm.

[0049] (2) Using centrifugal sedimentation, separate an appropriate amount of supernatant from the slurry obtained in step (1), prepare it to a concentration of about 100g / L, pour it into a hydrothermal reaction kettle, add indium nitrate solution to make the The mass ratio of indium ions to indium hydroxide is 0.5%, and dilute nitric acid is used to adjust the pH value to 4; then hydrothermal reaction is carried out at 200°C for 24h, and then washed, centrifugal spray-dried (temperature 150°C, atomizatio...

Embodiment 2

[0053] (1) Prepare indium hydroxide slurry with D50 less than 1 μm by electrolysis. In the electrolysis method of this embodiment, the anode and the cathode are installed in an electrolysis chamber at the same time. Ammonium nitrate aqueous solution with a concentration of 2.8mol / L, then heat the electrolytic chamber to 65°C, turn on the power, and set the current density to 500A / m 2 , and continued electrolysis for 15 hours to obtain a slurry with a D50 of less than 1 μm.

[0054] (2) Using centrifugal sedimentation, separate an appropriate amount of supernatant from the slurry obtained in step (1), prepare it to a concentration of about 100g / L, pour it into a hydrothermal reaction kettle, add indium nitrate solution to make the The mass ratio of indium ions to indium hydroxide is 0.05%, and the pH value is adjusted to 6.5 with nitric acid; then hydrothermal reaction is carried out at 200°C for 24h, and then washed and centrifugally spray-dried (temperature 150°C, atomizing ...

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Abstract

The invention provides high-dispersity indium oxide and a preparation method thereof. The preparation method comprises the following steps: a) taking metal indium as an anode, an inert electrode as a cathode and an ammonium nitrate aqueous solution as an electrolyte, and obtaining indium hydroxide slurry through an electrolytic method; b) adding an indium nitrate solution into the indium hydroxide slurry obtained in the step a) to enable the mass ratio of the added indium ions to indium hydroxide to be 0.01%-1%, adjusting the pH value to be 4-8, then carrying out hydrothermal reaction, and washing and drying a product to obtain indium hydroxide powder with high crystallinity and high dispersity; and c) calcining the high-crystallinity and high-dispersity indium hydroxide powder obtained in the step b) to obtain the high-dispersity indium oxide. According to the preparation method, indium hydroxide and indium oxide which are uniform in size distribution, high in dispersity and complete in crystal structure are successfully prepared in an electrolytic hydrothermal method combined mode, and the problem that indium oxide prepared from fine indium hydroxide powder synthesized through a common electrolytic method is prone to agglomeration in the calcining process is solved.

Description

technical field [0001] The invention relates to the technical field of preparation of ITO target materials, and more specifically relates to a highly dispersed indium oxide and a preparation method thereof. Background technique [0002] ITO sputtering target uses target sputtering technology to form ITO conductive film with excellent optical and electrical properties, which is widely used in liquid crystal display, touch screen, plasma display and other fields. However, the preparation of high-density and high-uniformity ITO targets has always been a technical difficulty in the ITO field. Indium oxide is the main component of ITO targets. In order to prepare high-performance ITO targets, the synthesis of indium oxide powders with good dispersion and uniform size distribution has always been the focus of research by researchers. At present, the methods for synthesizing indium oxide mainly include: sol-gel method, precipitation method, microemulsion method, template method, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00C25B1/01
CPCC01G15/00C25B1/00C01P2004/51C01P2004/03C01P2006/12C01P2004/62C01P2004/61
Inventor 王权朱刘邵学亮曾嘉豪李永鹏
Owner FIRST RARE MATERIALS CO LTD
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