High-purity gadolinium hexaboride polycrystal and preparation method thereof

A technology of hexaboride and gadolinium boride, which is applied in the polycrystalline field of gadolinium hexaboride, can solve the problems of impurities and low density

Active Publication Date: 2020-10-20
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of low density and impurities in the existing polycrystalline gadolinium hexaboride samples, the present invention aims to provide a high-purity polycrystalline gadolinium hexaboride and its preparation method

Method used

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  • High-purity gadolinium hexaboride polycrystal and preparation method thereof
  • High-purity gadolinium hexaboride polycrystal and preparation method thereof
  • High-purity gadolinium hexaboride polycrystal and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] In the first step, weigh GdH in the glove box according to the molar ratio of 1:6 2 Mix well with boron powder (GdH 2 Both the purity of boron powder and boron powder are 99.5-99.9%, and the particle size is 360 mesh, both purchased from Hunan Institute of Rare Earth Metal Materials). Use the QM-QX2 planetary high-energy ball mill to mill for 3 hours at a rotational speed of 350r / min, wherein every 30 minutes of ball milling, stop for 5 minutes and rotate in reverse to refine the powder and fully mix it.

[0036] The second step: the mixed powder was loaded into a graphite mold in a glove box, followed by spark plasma sintering (SPS) (LABOX-350, Sinter Land Inc., Japan) in-situ reaction sintering.

[0037] Among them, the sintering process is divided into four stages.

[0038] The first stage is the dehydrogenation reaction stage, at a temperature of 973K, GdH 2 The powder is dehydrogenated to form Gd metal element, wherein the pressure is 3MPa, the reaction time is ...

Embodiment 2

[0044] In the first step, weigh GdH in the glove box according to the molar ratio of 1:6 2 Mix well with boron powder (GdH 2 Both the purity of boron powder and boron powder are 99.5-99.9%, and the particle size is 360 mesh, both purchased from Hunan Rare Earth Metal Material Research Institute), the atmosphere of the glove box is high-purity argon with a purity ≥ 99.99%, and the oxygen content is lower than 10ppm; using QM -QX2 planetary high-energy ball mill ball mill for 3 hours, rotating speed 350r / min, among which every 30 minutes of ball milling, stop for 5 minutes and reverse rotation, so that the powder is refined and fully mixed.

[0045] The second step: the mixed powder was loaded into a graphite mold in a glove box, followed by spark plasma sintering (SPS) (LABOX-350, Sinter Land Inc., Japan) in-situ reaction sintering.

[0046] The sintering process is divided into four stages.

[0047] The first stage is the dehydrogenation reaction stage, at a temperature of 1...

Embodiment 3

[0053] In the first step, weigh GdH in the glove box according to the molar ratio of 1:6 2 Mix well with boron powder (GdH 2 Both the purity of boron powder and boron powder are 99.5-99.9%, and the particle size is 360 mesh, both purchased from Hunan Institute of Rare Earth Metal Materials). Use the QM-QX2 planetary high-energy ball mill to mill for 3 hours at a rotational speed of 350r / min, wherein every 30 minutes of ball milling, stop for 5 minutes and rotate in reverse to refine the powder and fully mix it.

[0054] The second step: the mixed powder was loaded into a graphite mold in a glove box, followed by spark plasma sintering (SPS) (LABOX-350, Sinter Land Inc., Japan) in-situ reaction sintering.

[0055] The sintering process is divided into four stages.

[0056] The first stage is the dehydrogenation reaction stage, at a temperature of 1173K, GdH 2 The powder is dehydrogenated to form a Gd metal element, wherein the pressure is 5 MPa, the reaction time is 5 minute...

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Abstract

The invention discloses a high-purity gadolinium hexaboride polycrystal and a preparation method thereof. The gadolinium hexaboride polycrystal does not contain gadolinium tetraboride impurities; andpreferably, the density of the gadolinium hexaboride polycrystal exceeds 80%, and the diameter of the gadolinium hexaboride polycrystal is 15 mm or above.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth boride materials, and in particular relates to a method for preparing high-purity gadolinium hexaboride polycrystal by using spark plasma sintering technology, and the gadolinium hexaboride polycrystal prepared therefrom. Background technique [0002] Due to the advantages of high melting point, low work function, high temperature and low volatility, high resistance to ion bombardment, and good physical and chemical stability, rare earth hexaborides have very good applications in the fields of high-energy optics, high-resolution sensors, and cathodes. prospect. Among them, the high emission efficiency of gadolinium hexaboride, the low-temperature magnetic transition and the strong light absorption characteristics in the near-infrared field have attracted widespread interest from scholars. However, the current research on gadolinium hexaboride is slow, mainly because gadolinium he...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/10C30B1/10
CPCC30B29/10C30B1/10
Inventor 杨新宇宁舒羽张久兴王衍
Owner HEFEI UNIV OF TECH
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