Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal

A rare earth boride, single crystal technology, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problems of high current density, unavailable, poor substrate adhesion, etc., and achieve large growth size and good symmetry , good quality effect

Inactive Publication Date: 2012-12-05
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the strong yield strength between rare earth boride powders, it is difficult to prepare high-density polycrystalline blocks by traditional sintering methods, which directly affects the emission performance of the material and is difficult to meet the requirements of practical applications.
Afterwards, the research direction of hexaboride turned to the preparation and application of single crystals. One-dimensional nanowires and two-dimensional thin film materials were prepared by vapor deposition and laser deposition. Absorb water, affect the reaction rate and reaction products
The existence of thin film materials and poor substrate adhesion cannot achieve high current densities

Method used

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  • Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal
  • Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal
  • Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) the CeB 6 Powder, PrB 6 The powder was ball milled and mixed according to the atomic ratio of 9:1, and then loaded into a graphite mold. Place the mold in the SPS sintering cavity, evacuate until the total pressure reaches 5 Pa, raise the temperature to 1150 °C at a heating rate of 100 °C / min, keep it for 5 min, and cool to room temperature with the furnace to obtain (Ce 0.9 PR 0.1 )B 6 polycrystalline rod;

[0019] 2) Using an optical zone melting furnace, with a diameter of 8mm (Ce 0.9 PR 0.1 )B 6 The polycrystalline rod is the first zone melting for seed crystal and material rod. After the equipment is evacuated to below 1Pa, flow argon gas into it until the pressure rises to 0.5MPa, the gas flow rate is 2L / min, and the power of the furnace in the 30min zone is increased until both the seed crystal and the material rod are melted and a stable melting zone is formed. During the crystal growth process The rotation speed is 30rpm, and the unit of crystal grow...

Embodiment 2

[0022] 1) the CeB 6 Powder, PrB 6 The powder was ball milled and mixed according to the atomic ratio of 9:1, and then loaded into a graphite mold. Place the mold in the SPS sintering cavity, evacuate until the total air pressure reaches 5Pa, raise the temperature to 1100°C at a heating rate of 80°C / min, keep the temperature for 3min, and cool to room temperature with the furnace to obtain (Ce 0.9 PR 0.1 )B 6 polycrystalline rod;

[0023] 2) Using an optical zone melting furnace, with a diameter of 6mm (Ce 0.9 PR 0.1 )B 6 The polycrystalline rod is the first zone melting for seed crystal and material rod. After the equipment is evacuated to below 1Pa, flow argon gas into it until the pressure rises to 0.5MPa, the gas flow rate is 1.5L / min, and the power of the furnace in the 30min zone is increased until both the seed crystal and the material rod are melted and a stable melting zone is formed, and the crystal growth process The medium speed is 30rpm, and the unit of cry...

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Abstract

The invention discloses a preparation method of a multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal, and belongs to the technical field of rare earth boride hot cathode materials. At present, the research about the multi-element rare earth boride single crystal is little; further, the prepared single crystal is small in dimension and low in purity; and the requirement of actual application cannot be met. By using the preparation method, the high-quality and large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal is prepared by adopting a method for combining discharge plasma sintering with floating zone melting. The (Ce0.9Pr0.1)B6 single crystal prepared by using CeB6 and PrB6 powder as raw materials is a phi4.5 mm*40 mm cylinder, and the test result of a single-crystal diffractometer shows that the single crystal is favorable in quality and a twin crystal phenomenon does not occur.

Description

technical field [0001] The invention belongs to the technical field of rare earth boride hot cathode materials, and in particular relates to the preparation of high-quality, large-size multi-element rare earth boride (Ce 0.9 PR 0.1 )B 6 single crystal. Background technique [0002] Rare earth hexaboride (ReB 6 , Re is a rare earth element) is a class of borides with a special crystal structure, which has the characteristics of high melting point, high hardness, low work function, high emission current density, good chemical stability, and strong ion bombardment resistance. hot cathode material. Since the discovery of lanthanum hexaboride with excellent electron emission properties in the 1960s, a boom in research on rare earth borides has started. Due to the strong yield strength between rare earth boride powders, it is difficult to prepare high-density polycrystalline blocks by traditional sintering methods, which directly affects the emission performance of the materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B13/00C30B29/10C30B13/28
Inventor 张久兴李晓娜张忻包黎红张宁张繁星
Owner BEIJING UNIV OF TECH
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