Method for preparing superfine zirconium boride powder

A technology of zirconium diboride and zirconium dioxide is applied in the field of preparing ultra-fine zirconium diboride powder, which can solve the problems of coarse particle size, large energy consumption and many impurity phases, and achieves simple equipment and operation process, and high reaction efficiency. Simple mechanism and low cost of raw materials

Inactive Publication Date: 2011-05-11
SHANGHAI UNIV
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Problems solved by technology

The self-propagating high-temperature synthesis method is simple, fast in reaction, short in time, low in energy consumption, and high in activity of the synthesized powder, which is beneficial to later sintering and processing. The reaction process is not easy to control
The mechanical synthesis method is to prepare ZrB by long-term mechanical ball milling of zirconia, boron oxide, metal aluminum or metal magnesium. 2 method, this method not only consumes a lot of energy, but also easily introduces impurities, which are difficult to remove
The traditional carbothermal reduction method in H 2 It needs to be heated to 1800°C in the atmosphere, or heated to 1700-1800°C under vacuum conditions, the particle size of the product is coarse, and it is difficult to remove impurities

Method used

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Embodiment 1

[0016] This embodiment provides a method for preparing ultrafine zirconium diboride powder, and its specific preparation steps are as follows:

[0017] A. Mix the raw materials according to a certain molar ratio: Zr0 2 :B 2 o 3 :B 4 C:C 12 h 22 o 11 =3:4:2:1, where Zr0 2 It is nano-sized zirconia powder, which is fully ground by adding alcohol, dried, and the mixture is pressed into a green body.

[0018] B. Put the green body into a corundum crucible, embed analytically pure activated carbon around the green body, put it into a high-temperature electric furnace, and carry out reaction synthesis under the protection of flowing high-purity argon gas. The synthesis temperature is 1500 ° C, and the temperature is kept for 3 hours. After cooling with the furnace, the body is taken out and fully ground to ultra-fine powder.

[0019] The ultrafine zirconium diboride prepared by the method has only the zirconium diboride phase through XRD analysis, and the average grain size ...

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Abstract

The invention relates to a method for preparing superfine zirconium boride powder, belonging to the technical field of ceramic materials. The method is as follows: burdening raw materials at a certain mole ratio, namely, the mole ratio of ZrO2 to B2O3 to B4C to C12H2O11 is 3: (2-4): (1-3):1; adding alcohol in the burdened raw materials for abundantly grinding; drying; pressing the mixed materials to a green body; placing the green body in a graphite or corundum crucible, embedding analytical pure activate carbon at the periphery of the green body, and putting in a high-temperature electric resistance furnace; reacting and synthesizing under the protection of flow high-pure argon, wherein the synthesis temperature is 1450-1550 DEG C and kept for 1-6 hours; and after cooling along with the furnace, taking the green body out, and fully grinding the green body to the superfine powder. In the invention, the cost of the used raw material is low, and a device and an operation flow process are simple; and by analysis of X-ray diffraction (XRD), only zirconium boride exists in the superfine powder, the average crystallite dimension of the zirconium boride is less than 100nm, and a result obtained by observation of scanning electron microscope (SEM) indicates that the average particle dimension is less than 500nm.

Description

technical field [0001] The invention relates to a method for preparing ultrafine zirconium diboride powder, which belongs to the technical field of ceramic materials. Background technique [0002] Zirconium diboride has the dual characteristics of ceramics and metals, because of its high melting point, high strength, high hardness, good electrical and thermal conductivity, good flame retardancy, heat resistance, oxidation resistance, corrosion resistance, neutron capture, etc. It has been widely used in the fields of high-temperature structural ceramic materials, composite materials, electrode materials, thin film materials, refractory materials, and nuclear control materials. [0003] At present, the preparation methods of zirconium diboride powder mainly include: direct synthesis method, reducing agent reduction method, electrolytic oxide method, self-propagating high temperature synthesis method, gas phase method and mechanical synthesis method. The raw materials of meta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/58
Inventor 甄强高林李榕孙凌云马杰
Owner SHANGHAI UNIV
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