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Method for preparing high-purity rare earth boride 6 (REB6) nano-powder

A nano-powder, high-purity technology, applied in the field of preparation of high-purity REB6 nano-powder, can solve the problems of restricting the application and research of REB6, difficult to prepare, difficult preparation method, etc. The effect of high self-propagating reaction rate and temperature gradient, guaranteed conversion and product yield

Active Publication Date: 2010-11-24
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all have the disadvantages of high energy consumption, high cost and complicated process.
Due to the low current efficiency, the electrolysis method also has the disadvantages of low yield, high energy consumption, high cost and small output.
Because of the difficulties in the preparation method, REB is severely limited 6 applications and research
And the REB prepared by the above method 6 The powder has defects such as low purity, large particle size, and poor activity, and it is difficult to prepare high-purity nanoscale REB 6 Material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take La 2 o 3 、B 2 o 3 And the Mg powder is batched according to the mass ratio of 100: 129: 160, that is, the excess of Mg powder is 5%, mixed by high-energy ball milling, the raw material is ground to 0.5 micron, and pressed into a cylindrical block blank with a pressure of 40 MPa; the blank is placed in an automatic In the spreading reaction furnace, heat the billet at constant temperature (constant temperature detonation) under the air atmosphere, the temperature is controlled at 750 ° C, until the self-propagating reaction is triggered, stop heating, naturally cool to room temperature, and collect intermediate products; use 40% dilute sulfuric acid as the leaching According to the theoretical requirements, the amount of excess acid is 20%, the intermediate product is directly leached without crushing, leached in a closed autoclave, the leaching temperature is 50°C, the leaching time is 40h, and the filter residue is obtained by filtration, and the cycle dynamic w...

Embodiment 2

[0040] Take La 2 o 3 、B 2 o 3 And the Mg powder is batched according to the mass ratio of 100: 120: 170, that is, the Mg powder is over 10%, mixed by high-energy ball milling, the raw material is ground to 0.4 micron, and pressed into a cylindrical block blank with a pressure of 55 MPa; put the pressed blank In the self-propagating reaction furnace, the billet is heated at a constant temperature (constant temperature detonation) under the air atmosphere, and the temperature is controlled at 900 ° C. Until the self-propagating reaction is initiated, the heating is stopped, naturally cooled to room temperature, and the intermediate product is collected; with 50% dilute sulfuric acid As a leaching agent, according to the theoretical requirement of an excess of 20% of acid, the intermediate product is leached directly without crushing, leached in a closed autoclave, the leaching temperature is 80°C, the leaching time is 24h, and the filter residue is obtained by filtration, and ...

Embodiment 3

[0042] Take La 2 o 3 、B 2 o 3, Mg is batched according to the mass ratio of 100: 135: 185, the excess of Mg powder is 20%, the high-energy ball mill is mixed, the raw material is ground to 0.2 microns, and pressed into a block billet with a pressure of 70MPa; the pressed billet is placed in a self-propagating reaction In the furnace, heat the sample in the air atmosphere, that is, directly detonate until the self-propagating reaction is triggered, stop heating, naturally cool to room temperature, and collect the intermediate product; use 60% dilute sulfuric acid as the leaching agent, and the amount of acid is excessive according to the theoretical requirements 20% dosage, the intermediate product is directly leached without crushing, leached in a closed autoclave, the leaching temperature is 70°C, the leaching time is 30h, the filter residue is obtained by filtration, and the filter product is dried in a drying oven , the temperature of the oven is controlled at about 150°...

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Abstract

The invention discloses a method for preparing high-purity rare earth boride 6 (REB6) nano-powder. The method comprises the following steps of: (1) mixing rare earth oxide, boric oxide and magnesium powder, performing high-energy ball-milling on the mixture, pressing the mixture into a block blank, putting the blank into a self-propagation reaction furnace for heating and triggering a self-propagation reaction so as to obtain an intermediate product, which is dispersed in an MgO substrate, of REB6; and (2) leaching the intermediate product in an enclosed autoclave by taking dilute sulphuric acid as a leaching agent to obtain leacheate, removing lixivium to obtain filter residue and washing and drying the filter residue to obtain the high-purity REB6 nano-powder. The method has the advantages of low raw material cost, simple operation, low requirement on technological conditions and capability of laying the foundation for industrial production. The obtained REB6 powder has the advantages of high purity, small particle size, high powder activity and the like.

Description

technical field [0001] The present invention relates to a REB 6 The preparation method of powder, particularly a kind of high-purity REB 6 Preparation method of nanopowder. Background technique [0002] Rare earth metal hexaboride REB 6 (LaB 6 , PrB 6 、NdB 6 , PmB 6 , SmB 6 、EuB 6 、GdB 6 , TbB 6 、DyB 6 , YbB 6 、HoB 6 ) has special crystal structure characteristics, therefore, it has the advantages of good chemical stability, high melting point, high hardness, etc. It is an ideal special ceramic material, which is widely used in the fields of national defense, military industry, nuclear industry and electronic information. , but due to its harsh preparation process conditions, currently only LaB 6 etc. have been better applied, but there are still defects such as poor product quality and unstable performance, especially high-purity REB 6 The preparation and application research of nanomaterials is almost a blank. [0003] Currently, REB 6 The preparation meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
Inventor 豆志河张廷安刘燕吕国志赫冀成
Owner NORTHEASTERN UNIV
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