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Technology for preparing spherical ultrafine zirconium boride powder by adopting liquid phase method and prepared zirconium boride powder

A kind of spherical, liquid-phase method, applied in the direction of boron/boride, metal boride, etc., can solve the problems of wide powder particle size distribution, high reaction temperature, etc., and achieve easy reaction process, high powder purity, and reaction process control. Effect

Inactive Publication Date: 2018-12-11
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesized powder has a wide particle size distribution and a high reaction temperature.

Method used

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  • Technology for preparing spherical ultrafine zirconium boride powder by adopting liquid phase method and prepared zirconium boride powder
  • Technology for preparing spherical ultrafine zirconium boride powder by adopting liquid phase method and prepared zirconium boride powder

Examples

Experimental program
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Effect test

Embodiment 1

[0026] a ZrB 2 The preparation process of the precursor conversion method of ceramic powder, the specific process is as follows:

[0027] (1) Step 1: According to the amount ratio of substances, it is boric acid: zirconium oxychloride octahydrate=3:1, glucose is calculated according to the carbon obtained after pyrolysis is complete, that is, C / (Zr+B)=6, take 1.6 respectively g zirconium oxychloride octahydrate, 4g boric acid, and 10g glucose for subsequent use.

[0028] (2) Step 2: Dissolve 1.6g of zirconium oxychloride in 20ml of absolute ethanol, add dropwise 2ml of hydrogen peroxide and 5ml of acetylacetone, and continue stirring for 1 hour to obtain a uniform and transparent solution, namely zirconium sol. Dissolve 4g of boric acid in 30g of absolute ethanol, heat in a water bath at 40°C until completely dissolved, and prepare a boric acid solution. Dissolve 10 g of glucose in 20 g of deionized water to prepare a glucose solution. In the case of continuous magnetic sti...

Embodiment 2

[0033] A single-component ZrB 2 The preparation process of the precursor conversion method of ceramic powder is the same as in Example 1 except that the following experimental raw material ratios are different.

[0034] In this embodiment: the amount ratio of the raw materials weighed is boric acid: zirconium oxychloride octahydrate=4:1, glucose is calculated according to the carbon obtained after pyrolysis is complete, that is, C / (Zr+B)=6.

Embodiment 3

[0036] a ZrB 2 The preparation process of the precursor conversion method of the ceramic powder is the same as in Example 1 except that the ratio of the following experimental raw materials and the heat treatment temperature are different.

[0037] In the present embodiment: the amount ratio of the raw material that weighs is boric acid: zirconium oxychloride octahydrate=3:1, and glucose calculates namely C / (Zr+B)=6 according to the carbon that obtains after pyrolysis is complete, heat treatment temperature It is 1600°C.

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Abstract

The invention provides a technology for preparing spherical ultrafine zirconium boride powder by adopting a liquid phase method. The technology is specifically charaterized in that ultrafine zirconiumboride powder is prepared through a sol-gel and heat treatment process, and the zirconium boride powder with controllable size can be obtained by regulating and controlling the process parameters inthe method. The technology comprises the following steps that zirconium oxychloride octahydrate, boric acid and glucose serve as starting materials, absolute ethyl alcohol and deionized water serve assolvents, a zirconium precursor solution, a boric acid solution and a glucose solution are prepared separately and are uniformly mixed so as to obtain boron-zirconium precursor sol, and in the process, acetylacetone and hydrogen peroxide are added so as to promote the formation of the precursor sol; and then drying is carried out, and calcining is carried out at high temperature in an argon atmosphere so as to prepare the ZrB2 ceramic powder with high purity and fine and uniform particle size. The technology is simple, the reaction raw material cost is low, the reaction process is easy to control, the synthesis temperature is low, and the prepared powder is high in purity, uniform and fine in particle size and less in agglomeration and can conveniently become a preferred material of a ceramic composite material and a ceramic coating.

Description

technical field [0001] The invention belongs to the technical field of inorganic non-metallic materials, and relates to a method for preparing ultra-high temperature ceramic raw material powder, in particular to a process for preparing spherical ultrafine zirconium boride powder by a liquid phase method and the prepared zirconium boride powder . Background technique [0002] ZrB 2 With strong ionic bonds and covalent bonds, boride-based ultra-high temperature ceramics have comprehensive characteristics such as high melting point, high modulus, high hardness, low saturated vapor pressure, high thermal conductivity and electrical conductivity, and good thermal shock resistance. It has become the most potential candidate material for ultra-high temperature ceramics, and has a wide range of applications in high-temperature structural materials, composite materials, refractory materials and other fields. [0003] At present, the commonly used methods for preparing zirconium bor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C01B35/04
CPCC01B35/04C01P2002/72C01P2004/03C01P2006/80C04B35/58078
Inventor 刘长青常小靖伍媛婷张露月李旭
Owner SHAANXI UNIV OF SCI & TECH
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