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Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof

A rare earth boride and cathode material technology, applied in the direction of boron/boride, metal boride, etc., can solve the problems of low product purity and density, high technical difficulty, affecting performance, etc., achieve high purity and density, and expand applications Field, the effect of easy operation

Inactive Publication Date: 2015-08-19
JINGGANGSHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the existing rare earth boride polycrystalline preparation method complex process, high technical difficulty, low product purity and density, affecting performance, and high cost, the invention provides a rare earth boride (La x Ce 1-x )B 6 Solid solution polycrystalline cathode material and preparation method thereof

Method used

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  • Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof
  • Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof
  • Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof

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Effect test

Embodiment 1

[0031] 1) Classified ball mill + hand mixing. LaB 6 and CeB 6 20g each of the raw material powder is placed in a stainless steel grinding tank, and stainless steel balls of φ12mm, φ10mm, φ8mm and φ6mm are selected as the grinding medium. The mass ratio of powder to powder is 10:1. In order to prevent the boron powder in the mixed powder from being oxidized, the above operations are all carried out in an argon atmosphere glove box with an oxygen content and a water vapor content of ≤0.5ppm. The ball mill jar was placed in a high-energy ball mill for ball milling at a speed of 500 r / min. After ball milling for 2 hours, samples were stored in a glove box. LaB obtained by ball milling in the glove box 6 and CeB 6 The powder is weighed respectively at a molar ratio of 9:1, the total mass of the powder is 10g, and the weighed LaB 6 and CeB 6 The powder is placed in an agate mortar for manual grinding and mixing. 2) Load the furnace. The above-mentioned mixed reaction materi...

Embodiment 2

[0034] 1) Classified ball mill + hand mixing. LaB 6 and CeB 6 The raw material powder is placed in a stainless steel grinding tank respectively, and stainless steel balls of φ12mm, φ10mm, φ8mm and φ6mm are selected as the grinding medium. The material mass ratio is 20:1. In order to prevent the boron powder in the mixed powder from being oxidized, the above operations were all carried out in an argon atmosphere glove box with oxygen content and water vapor content ≤ 6ppm. The ball mill jar was placed in a high-energy ball mill for ball milling at a speed of 700 r / min, and samples were stored in a glove box after ball milling for 1 hour. LaB obtained by ball milling in the glove box 6 and CeB 6 The powder is weighed respectively at a molar ratio of 4:1, the total mass of the powder is 10g, and the weighed LaB 6 and CeB 6 The powder is placed in an agate mortar for manual grinding and mixing. 2) Load the furnace. The above-mentioned mixed reaction materials were loaded ...

Embodiment 3

[0037] 1) Mixing ball milling. The LaB after weighing respectively with a molar ratio of 7:3 6 and CeB 6 A total of 20g of raw material powder is placed in a stainless steel grinding tank. Stainless steel balls of φ12mm, φ10mm, φ8mm and φ6mm are selected as grinding media. The mass ratio of stainless steel balls of φ12mm, φ10mm, φ8mm and φ6mm is 1:2:2:1 The mass ratio of the ball to the powder is 15:1; in order to prevent the boron powder in the mixed powder from being oxidized, the above operations are all carried out in an argon atmosphere glove box with an oxygen content and a water vapor content of ≤1ppm. The ball mill jar was placed in a high-energy ball mill for ball milling at a speed of 600r / min. After ball milling for 1.5h, samples were stored in a glove box. 2) Load the furnace. The above-mentioned mixed reaction materials were loaded into a φ20mm graphite mold in a glove box, and the mold was placed in a hot-press sintering furnace. 3) Heating and sintering. Va...

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Abstract

The invention provides a multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and a preparation method thereof, and belongs to the technical field of rare earth boride cathode materials. The method adopting LaB6 and CeB6 powder as raw materials comprises the following steps: carrying out ball milling, and carrying out vacuum hot pressing sintering at a highest sintering temperature of 1700-1900DEG C to synthesize (LaxCe1-x)B6 solid solution polycrystals, wherein x is not smaller than 0.1 and not greater than 0.9. The method combines a powder synthesis process with a sintering densification process, so the method has the advantages of preparation flow simplification, purity and density increase, and production cost reduction, and is suitable for industrial production and application. The (LaxCe1-x)B6 solid solution polycrystalline cathode material obtained through the preparation method has the characteristics of single phase and high density, and can be used in plasma sources, electron beam welding machines, electron beam exposure machines and field emission arrays.

Description

technical field [0001] The invention belongs to the technical field of rare earth boride cathode materials, in particular to a multi-element rare earth boride (La x Ce 1-x )B 6 Solid solution polycrystal and method for its preparation. Background technique [0002] The cathode is the heart device of various modern vacuum electronic devices, and it is widely used in the defense industry and civilian fields. Lanthanum hexaboride (LaB 6 ) and cerium hexaboride (CeB 6 ) represented by rare earth hexaboride (REB 6 ), is a hot cathode with excellent performance, which has the characteristics of low work function, low resistivity, low evaporation rate, high melting point, long life, etc., so it is widely used in various electron microscopes, plasma sources, electron beam welders, electron beam Exposure machine, field emission array and other equipment. Especially in some micro-processing equipment, it is necessary to obtain precise and controllable electron beams, requiring ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
Inventor 周身林叶子飘罗回雨余晓光罗小兵孙心瑗陈明源
Owner JINGGANGSHAN UNIVERSITY