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Preparation method of hafnium carbide nano-powder

A nano-powder, hafnium carbide technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of lower reaction temperature, large particle size, high equipment requirements, etc., to achieve lower reaction temperature , Uniform grain distribution and good repeatability

Inactive Publication Date: 2015-06-03
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are not many reports on the synthesis methods of hafnium carbide at home and abroad. The reported methods mainly include: (1) direct carbothermal reduction method, which generally needs to be reacted above 1900°C, which has high energy consumption and high equipment requirements, and grows out The particle size is large, and it is necessary to use other methods to assist in reducing the reaction temperature

Method used

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  • Preparation method of hafnium carbide nano-powder
  • Preparation method of hafnium carbide nano-powder
  • Preparation method of hafnium carbide nano-powder

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Weigh 15g HfCl 4 , 9.84g C 6 h 8 o 7 ·H 2 O(HfCl 4 and C 6 h 8 o 7 ·H 2 (2 molar ratio is 1:1) is put into 1000mL beaker, adds 65mL deionized water, stirs constantly with glass rod, makes HfCl 4 and C 6 h 8 o 7 ·H 2 O is fully dissolved in deionized water, and then an appropriate amount of NH is added with a burette 3 ·H 2 O solution (mass concentration 25%) adjusts the pH of the solution to 2-3, and performs magnetic stirring treatment at a constant temperature of 80° C., the magnetic stirring speed is 60 r / min, and the stirring time is 30 min to obtain a hafnium-containing gel. Put the hafnium-containing gel in an alumina crucible and put it into a low-temperature tube furnace for heat treatment to obtain a precursor powder. The annealing process is to raise the temperature to 800°C at a rate of 4°C / min at room temperature, keep it for 2 hours, and the atmosphere is high-purity Ar , the Ar flow rate is 0.5L / min. The precursor powder obtained after the ...

Embodiment 2

[0035] Weigh 15g HfCl 4 , 6.27g C 6 h 8 o 7 ·H 2 O(HfCl 4 and C 6 h 8 o 7 ·H 2 (2 molar ratio is 1:0.64) is put into 1000mL beaker, adds 60mL deionized water, stirs constantly with glass rod, makes HfCl 4 and C 6 h 8 o 7 ·H 2 O is fully dissolved in deionized water, and then an appropriate amount of NH is added with a burette 3 ·H 2 The O solution adjusts the pH of the solution to 2-3, and performs magnetic stirring treatment at a constant temperature of 60°C, the magnetic stirring speed is 60r / min, and the stirring time is 30min, to obtain a hafnium-containing gel. Put the hafnium-containing gel in an alumina crucible and put it into a low-temperature tube furnace for heat treatment to obtain a precursor powder. The annealing process is to raise the temperature to 800°C at a rate of 3°C / min at room temperature, keep it for 1 hour, and the atmosphere is high-purity Ar , the Ar flow rate is 0.5L / min. The precursor powder obtained after the annealing treatment wa...

Embodiment 3

[0038] Weigh 15g HfCl 4 , 14.7g C 6 h 8 o 7 ·H 2 O(HfCl 4 and C 6 h 8 o 7 ·H 2 (2 molar ratio is 1:1.5) is put into 1000mL beaker, adds 70mL deionized water, stirs constantly with glass rod, makes HfCl 4 and C 6 h 8 o 7 ·H 2 O is fully dissolved in deionized water, and then an appropriate amount of NH is added with a burette 3 ·H 2 The O solution adjusts the pH of the solution to 2-3, and performs magnetic stirring treatment at a constant temperature of 80° C., the magnetic stirring speed is 80 r / min, and the stirring time is 60 min to obtain a hafnium-containing gel. Put the hafnium-containing gel in an alumina crucible and put it into a low-temperature tube furnace for heat treatment to obtain a precursor powder. The annealing process is to raise the temperature to 800°C at a rate of 10°C / min at room temperature, keep it for 3 hours, and the atmosphere is high-purity Ar , the Ar flow rate is 0.4L / min. The precursor powder obtained after the annealing treatmen...

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Abstract

The invention relates to a preparation method of hafnium carbide nano-powder. The preparation method comprises steps as follows: 1) preparing hafnium-containing gel: dissolving HfCl4 and C6H8O7*H2O in deionized water, continuously stirring the mixture to fully dissolve the HfCl4 and the C6H8O7*H2O, then adjusting the pH value to range from 2 to 3 with an ammonia water solution, and performing magnetic stirring treatment at the constant temperature of 60-80 DEG C to obtain the hafnium-containing gel; 2) preparing precursor powder: placing the hafnium-containing gel into a low-temperature tube furnace for heat treatment to obtain the precursor powder; (3) preparing the hafnium carbide nano-powder: placing the precursor powder into a planetary ball-milling tank for high-energy ball milling, and placing obtained powder into a discharge plasma sintering furnace for reactions to obtain the hafnium carbide nano-powder. The method is simple in technology, low in energy consumption, good in repeatability and good in industrial prospect, and the prepared hafnium carbide nano-powder is a high-activity nano-scale product with hafnium carbide distributed evenly and is even in crystal grain distribution, high in purity and good in degree of crystallinity.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and relates to a preparation method of hafnium carbide nano powder. Background technique [0002] HfC is a non-stoichiometric carbide formed by the transition element Hf and C, namely HfC x (0.5≤x≤1), it belongs to a superhard material. According to the JCPDF card, its structure is a NaCl-type face-centered cubic structure, and its lattice constant is 0.46375nm. Hf atoms form a compact cubic lattice, and C atoms are in the octahedral interstitial position of the lattice. HfC crystals are connected by carbon-hafnium bonds with a bond distance of a / 2, and the bonds are symmetrically distributed. In the HfC crystal structure, the adjacent metal atomic planes between the (111) planes and the C atomic planes are connected by the strongest bond energy atomic bonds. When slipping, the strongest bonds must be destroyed, so the slipping is very difficult. Macroscopically, it exhibits...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30B82Y30/00
Inventor 王为民方志朋王吉林夏睿王阳达奥运傅正义
Owner WUHAN UNIV OF TECH