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Method for preparing high-purity nano hafnium boride from molten salt through electrolysis

A technology of molten salt electrolysis and nano-boron, applied in the field of electrolytic metallurgy, can solve the problems of difficult control of C element content, large-scale production difficulty, and expensive metal hafnium, and achieve simple equipment, easy industrial continuous production, and low price Effect

Inactive Publication Date: 2018-06-29
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Chinese patents CN103754891A and CN101428812A use hafnium dioxide, boron carbide, graphite, etc. as raw materials, heat them to about 1500°C, and perform high-temperature reduction in an inert atmosphere or a hydrogen atmosphere; the reaction temperature of this method is high, and the C element content in the product Difficult to control, so get high purity HfB 2 The product is more difficult
Other methods such as self-propagating high-temperature synthesis and chemical vapor deposition have high energy consumption, difficult control of impurity content, and difficulty in large-scale production
Currently commercially available HfB 2 The powder mostly uses high-purity metal hafnium and boron powder to react directly, and the HfB obtained by this method 2 The powder has high purity, but metal hafnium is expensive, the cost is high, and the particle size of the obtained powder is relatively large

Method used

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  • Method for preparing high-purity nano hafnium boride from molten salt through electrolysis
  • Method for preparing high-purity nano hafnium boride from molten salt through electrolysis
  • Method for preparing high-purity nano hafnium boride from molten salt through electrolysis

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Experimental program
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Effect test

Embodiment 1

[0023] HfO with a purity of 99.9% 2 The powder and boron powder are uniformly mixed at a molar ratio of 1:2, and formed by mechanical pressure to form a rectangular block with a length of 70mm, a width of 50mm, and a thickness of 10mm.

[0024] The rectangular block is combined with a conductive cathode current collector as the cathode, the graphite rod is used as the anode, and the CaCl 2 As an electrolyte, in an argon environment, 950°C, and a cell voltage of 3.0V, use a regulated power supply to control the voltage and perform constant voltage electrolysis;

[0025] After electrolysis, the electrolysis product is washed with 1% by volume dilute hydrochloric acid and pure water in turn, dried in vacuum and sieved to obtain high-purity HfB 2 powder.

[0026] The resulting product is subjected to purity analysis and XRD characterization, see Table 1 and attached figure 1 , the product purity reaches 99.96wt%.

Embodiment 2

[0028] HfO with a purity of 99.9% 2 The powder and boron powder are uniformly mixed at a metering ratio of 1:2, and formed by mechanical pressure to form a rectangular block with a length of 70mm, a width of 50mm, and a thickness of 10mm.

[0029] Combining a rectangular block with a conductive cathode current collector as the cathode, using a graphite rod as the anode, and using NaCl as the electrolyte, in an argon environment, 700°C, and a cell voltage of 2.9V, use a regulated power supply to control the voltage to perform constant voltage electrolysis ;

[0030] After electrolysis, the electrolysis product is washed with 1% by volume dilute hydrochloric acid and pure water in turn, dried in vacuum and sieved to obtain high-purity HfB 2 powder.

[0031] The resulting product is subjected to purity analysis and XRD characterization, see Table 1 and attached figure 2 , the product purity reaches 99.95wt%.

Embodiment 3

[0033] HfO with a purity of 99.9% 2 The powder and boron powder are uniformly mixed at a metering ratio of 1:2, and formed by mechanical pressure to form a rectangular block with a length of 70mm, a width of 50mm, and a thickness of 10mm.

[0034] The rectangular block is combined with a conductive cathode current collector as the cathode, the graphite rod is used as the anode, and the NaCl:CaCl 2 The mixed molten salt electrolyte with a molar ratio of 1:1 is used as the electrolyte. In an argon environment, 600°C, and a cell voltage of 2.9V, the voltage is controlled by a regulated power supply to perform constant voltage electrolysis;

[0035] After electrolysis, the electrolysis product is washed with 1% by volume dilute hydrochloric acid and pure water in turn, dried in vacuum and sieved to obtain high-purity HfB 2 powder.

[0036] The resulting product was analyzed for purity, see Table 1 for details, and the product purity reached 99.92wt%.

[0037] Gained product imp...

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Abstract

The invention belongs to the technical field of electrolytic metallurgy, and particularly relates to a method for preparing high-purity nano hafnium boride from molten salt through electrolysis. The preparation method comprises the steps of taking hafnium oxide and boron as raw materials, and mixing and compressing hafnium oxide powder and the boron into porous blocks; compounding the porous blocks and a cathode collector to be regarded as a cathode, and taking graphite as an anode; and electrolyzing the molten salt by taking one or more of CaCl2 and NaCl as molten salt electrolytes to directly generate the hafnium boride, and the prepared hafnium boride product is high-purity nano powder. The preparation method provided by the invention has the advantages of lower reaction temperature, easy operation, and low price of the raw materials, and is environmentally friendly and beneficial to industrial continuous production.

Description

technical field [0001] The invention belongs to the technical field of electrolytic metallurgy, in particular to a method for preparing high-purity nano hafnium boride by electrolysis of molten salt. Background technique [0002] Hafnium diboride (HfB 2 ) high melting point, high hardness, good chemical stability, strong electrical and thermal conductivity, good thermal shock resistance, and is widely used in thin film resistors and microelectronics industries. Additionally, to HfB 2 Adding other materials such as SiC, etc., can greatly improve its oxidation resistance and ablation, and is widely used in high-demand fields such as aerospace. 2 The purity and particle size requirements are also getting higher and higher. [0003] Currently, HfB 2 The preparation methods mainly include carbothermal / borothermic reduction method, self-propagating high-temperature synthesis, sol-gel method, etc. For example, Chinese patents CN103754891A and CN101428812A use hafnium dioxide, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00B82Y40/00
CPCC25B1/00B82Y40/00
Inventor 石志霞孙静彭程张碧田段华英王星明
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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