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Preparation method of high purity CeB6 nano powder

A nano-powder, high-purity technology, applied in the field of preparation of high-purity CeB6 nano-powder, can solve the problems of harsh process requirements, high energy consumption of electrolysis, high production cost, etc., achieve low process conditions, avoid secondary pollution, reduce The effect of production costs

Active Publication Date: 2012-02-01
NORTHEASTERN UNIV LIAONING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Currently, CeB 6 The preparation methods of powder mainly include molten salt electrolysis, boron thermal reduction, boron carbide and chemical vapor deposition, etc. All of the above methods have the disadvantages of high energy consumption and complicated process, and are still far away from industrial production.
For example, the borothermic reduction method is the CeO 2 After mixing with boron powder, synthesize CeB at a high temperature above 1400°C 6 Powder, because the raw material is high-purity boron powder, so the production cost is high, and the process requirements are harsh and difficult to control
Electrolysis also has the disadvantages of high energy consumption, high cost, and low output

Method used

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  • Preparation method of high purity CeB6 nano powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take CeO 2 , B 2 o 3And the Mg powder is proportioned according to 100:120:162 mass percentage, that is, the excess of Mg powder is 5%, the high-energy ball mill is mixed, the raw material is ground to 0.5 microns, and pressed into a cylindrical block blank, the pressure of the sample is 40MPa, and the blank is placed in In the spreading 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 triggered. Stop heating, cool naturally 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 15%, and 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 ...

Embodiment 2

[0027] Take CeO 2 , B 2 o 3 And the Mg powder is batched according to 100:110:170 mass percentage, that is, the excess of Mg powder is 10%, the high-energy ball mill is mixed, the raw material is ground to 0.4 microns, and pressed into a cylindrical block blank. The pressure of the sample is 50MPa. 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 700 ° C. Until the self-propagating reaction is triggered, 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 the filtere...

Embodiment 3

[0029] Take CeO 2 , B 2 o 3 , Mg is batched according to 100:130:185 mass percentage, the excess of Mg powder is 20%, the high-energy ball mill is mixed, the raw material is ground to 0.2 micron, pressed into a block billet, the pressure of the sample is 70MPa, and the pressed billet is placed in a self-propagating reaction In the furnace, the billet is heated under the air atmosphere, that is, it is directly detonated until the self-propagating reaction is triggered, the heating is stopped, and the intermediate product is naturally cooled to room temperature, and the intermediate product is collected; 60% dilute sulfuric acid is used as the leaching agent. % dosage, the intermediate product is directly leached without crushing, leached in a closed autoclave, the leaching temperature is 70°C, and the leaching time is 30h, and 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 relates to a preparation method of high purity CeB6 nano powder, including the following steps: (1) CeO2, B2O3 and magnesium powder are mixed, high energy ball grinding is carried out, and then blank is obtained by pressing; (2) the blank is placed into an automatic spreading reaction furnace, heating in air atmosphere is carried out to initiate automatic spreading reaction, intermediate product is leached out in a hermetically sealed high pressure autoclave, so as to obtain leachate, filtering is carried out to obtain residue, and washing and drying are carried out to obtain the high purity CeB6 nanopowder. The invention has available raw material, simple operation and low requirement on technological condition; and the obtained CeB6 powder has the advantages of high purity, small granularity and high powder activity.

Description

technical field [0001] The present invention relates to the preparation method of boride powder, particularly a kind of high-purity CeB 6 Preparation method of nanopowder. Background technique [0002] CaB 6 It has the structural characteristics of typical rare earth metal hexaborides, and belongs to the cubic structure. It has the advantages of low work function, good chemical stability, high melting point, high hardness, strong anti-poisoning ability, and strong ion bombardment resistance. It is an ideal heat sink. Cathode materials are widely used in high-brightness point electron source equipment, such as electron microscopes such as SEM and TEM, and high current density electron source application equipment, such as microwave tubes, plasma sources, lithography, electron beam welding machines, free electron lasers, etc. in the device. For example, CeB 6 As a hot cathode material with a ratio of LaB 6 More superior performance, first, strong anti-carbon pollution; se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/04
Inventor 张廷安豆志河刘燕郭永楠赫冀成吕国志
Owner NORTHEASTERN UNIV LIAONING