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Preparation method of indium tin oxide nano-powder with controllable crystalline form

A technology of indium tin oxide and indium tin hydroxide, applied in chemical instruments and methods, gallium/indium/thallium compounds, tin oxide, etc. Difficult to disperse and other problems, to achieve the effect of inhibiting powder agglomeration, excellent dispersibility, and avoiding hard agglomeration of particles

Inactive Publication Date: 2010-05-12
NANCHANG HANGKONG UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the fine particle size of the precursor grains, it is very easy to agglomerate. During the calcination process, the ITO grains formed by thermal decomposition in the agglomerate are prone to surface adhesion, that is, hard agglomeration (CN100343273C, CN100364897C), which causes the powder to be difficult to disperse. As an ITO coating material or as a conductive filler, the transparency and conductivity of the material will be greatly reduced
In addition, the ITO nano-grains prepared by the co-precipitation method are generally spherical, not only the shape of the grains is single, but also the grains are generally polycrystalline, which reduces its conductivity. It can only be used for anti-static fillers with low conductivity requirements and For further sintering ITO target

Method used

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  • Preparation method of indium tin oxide nano-powder with controllable crystalline form
  • Preparation method of indium tin oxide nano-powder with controllable crystalline form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 11g InCl 3 Dissolve in 250ml of deionized water and stir mechanically. After 10 minutes, take out 50ml of the solution, add 1g of anhydrous SnCl 4 , after being completely dissolved, slowly added to the stirring InCl 3 aqueous solution, and placed in a constant temperature water bath for mechanical stirring. Prepare 80 ml of 3M ammonia solution with deionized water, slowly add it to the indium tin solution at room temperature until the pH value of the solution reaches 3.0, then raise the temperature of the water bath to 70°C, and continue to add the ammonia solution until the pH is 7.0 as of now. After the white precipitate was separated, it was stirred and washed in 200ml of 60°C distilled water and 60°C ethanol for 1 hour respectively. After suction filtration, it was dispersed with absolute ethanol, dried, and sieved to obtain the precursor powder. The XRD structure analysis results show that the precursor powder contains two phases: In(OH) 3 and InOOH, whe...

Embodiment 2

[0020] Take 1.5g of precursor powder and put it in a porcelain boat, and put it into a tubular resistance furnace with a glass three-way-quartz tube furnace. Turn on the three-way switch, and calcinate at 800°C for 1h in an air atmosphere, and the heating rate is 10°C / min, yellow-green ITO powder was obtained. The TEM observation results of the powder showed that the ITO grain morphology completely inherited the rod-like structure and high dispersion characteristics of the precursor, and the grain size was slightly smaller than the precursor. The grain is a polycrystal composed of many small grains with a size of 20-30nm closely packed, and the aspect ratio is 3-4.

Embodiment 3

[0022] Take 1.5g of precursor powder and put it in a porcelain boat, and put it into a tubular resistance furnace with a glass tee-quartz tube furnace. Close the glass tee at one end of the quartz tube, connect the three-way switch at the other end to a vacuum pump, reduce the air pressure in the quartz tube to below 1 Torr, then start the calcination heating program at a heating rate of 10°C / min, and calcine at 800°C for 1 hour in vacuum to obtain Yellow-green ITO powder. The powder TEM morphology observation results show that the ITO grains are equiaxed polyhedral grains, the grain size is between 40-80nm, and there is no hard agglomeration between the grains.

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Abstract

A preparation method of indium tin oxide nano-powder with controllable crystalline form is characterized in that the technological method comprises the following steps: (1) dissolving indium oxide and tin oxide in distilled water, using strong base aqueous solution as precipitant to prepare ITO precursor through two-step precipitation method; (2) washing the sedimentary precursor power with water, drying, grinding, screening to obtain indium tin oxide precursor power; and (3) calcining indium tin oxide precursor power under a certain atmosphere to prepare yellowgreen ITO nano-powder. The invention has the advantages that 1. no hard agglomeration exists among the ITO grains, the grain size is more uniform; 2. the calcining atmosphere can be selected to control the appearance of the ITO grains; 3. the preparation process of the precursor does not use any dispersant or surface complexing agent to inhibit the power agglomeration; and 4. the temperature and precipitation rate can be adjusted to change the grain size and length-diameter ratio of grains during the two-step precipitation process.

Description

technical field [0001] The invention relates to a preparation method of nano powder, in particular to a preparation method of indium tin oxide nano powder with controllable crystal form. Background technique [0002] ITO is a typical high-conductivity transparent semiconductor material with a resistivity as high as 10 -5 Ω·cm. Since the bandgap width of ITO semiconductor is 3.5-4.6eV, the light transmittance of this material in the visible light range reaches more than 90%, and it has been widely used in various displays such as computers, mobile phones, LCD TVs, ATM automatic teller machines, etc. . [0003] ITO materials are generally used as thin films, and are usually produced continuously using large-scale magnetron sputtering equipment. This method has the advantage of high conductivity and light transmittance, but its disadvantages are not only expensive equipment, but tens of millions of yuan for production equipment. , and due to the use of physical coating, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/02C01G15/00C03C17/245
Inventor 卢金山董伟李朔梅
Owner NANCHANG HANGKONG UNIVERSITY
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