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Preparation method of nanometer calcium hexaboride powder

A technology of calcium hexaboride and powder, applied in the field of preparation of calcium hexaboride, can solve problems such as particle hard agglomeration

Inactive Publication Date: 2013-08-28
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, CaB prepared by boron carbide method and boron thermal reduction method 6 Due to the high reaction temperature and the limitation of raw material size, the obtained CaB 6 The powder particle size is relatively large, all in the micron scale, and the particle hard agglomeration phenomenon is serious

Method used

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  • Preparation method of nanometer calcium hexaboride powder
  • Preparation method of nanometer calcium hexaboride powder
  • Preparation method of nanometer calcium hexaboride powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation method of nano calcium hexaboride:

[0023] (1) Weigh calcium chloride and sodium borohydride at a molar ratio of 1:6, grind and mix them evenly and put them into the crucible, not exceeding 2 / 3 of the crucible;

[0024] (2) Place the crucible in a vacuum resistance furnace and keep the working vacuum at 6.67×10 -2 P a , heating at a heating rate of 15°C / min to 530°C and holding for 1 hour;

[0025] (3) After the reactant is taken out and ground, first wash away Na in the product with absolute ethanol, and then use three-stage purified deionized water to wash away NaCl and other products. The number of washings is not less than six times. Ultrasonic vibration equipment was used to accelerate the dissolution of by-products during washing, and finally the obtained gray-black powder was placed in a vacuum drying oven at 60°C for 8 hours to heat and dry to obtain the purified final product.

Embodiment 2

[0027] The preparation method of nano calcium hexaboride:

[0028] (1) Weigh calcium chloride and sodium borohydride according to the chemical molar ratio of 1:12, grind and mix them evenly and put them into the crucible, not exceeding 2 / 3 of the crucible;

[0029] (2) Place the crucible in a vacuum resistance furnace and keep the working vacuum at 6.67×10 -2 P a , heating at a heating rate of 15°C / min to 490°C and holding for 4 hours;

[0030] (3) After the reactant is taken out and ground, first wash away Na in the product with absolute ethanol, and then use three-stage purified deionized water to wash away NaCl and other products. The number of washings is not less than six times. Ultrasonic vibration equipment was used to accelerate the dissolution of by-products during washing, and finally the obtained gray-black powder was placed in a vacuum drying oven at 70°C for 6 hours to heat and dry to obtain the purified final product.

Embodiment 3

[0032] The preparation method of nano calcium hexaboride:

[0033] (1) Weigh calcium chloride and sodium borohydride according to the chemical molar ratio of 1:9, grind and mix them evenly and put them into the crucible, not exceeding 2 / 3 of the crucible;

[0034] (2) Place the crucible in a vacuum resistance furnace and keep the working vacuum at 6.67×10 -2 P a , heating at a heating rate of 10°C / min to 500°C and holding for 2 hours;

[0035] (3) After the reactant is taken out and ground, first wash away Na in the product with absolute ethanol, and then use three-stage purified deionized water to wash away NaCl and other products. The number of washings is not less than six times. Ultrasonic vibration equipment was used to accelerate the dissolution of by-products during washing, and finally the obtained gray-black powder was placed in a vacuum drying oven at 60°C for 10 hours to heat and dry to obtain the purified final product.

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Abstract

The invention relates to a preparation method of nanometer calcium hexaboride powder. The preparation method comprises the steps of: weighing calcium chloride and sodium borohydride according to the chemical mole ratio of 1:(6-12), grinding, and evenly mixing to place in a crucible; placing the crucible in a vacuum resistance furnace, keeping the working vacuum degree of 6.67*10<-2>Pa, heating to increase the temperature up to 480 DEG C-550 DEG C, preserving heat for 1-4 hours, and carrying out furnace cooling; taking out reactant and grinding, washing, purifying and drying to finally obtain final product. The grain size of the CaB6 prepared is distributed within 20nm to 30nm, the particle size is smaller than 100nm, the CaB6 is shaped like a cube, and the yield rate approaches 100%.

Description

technical field [0001] The invention relates to a preparation method of calcium hexaboride, which belongs to the technical field of functional ceramics. Background technique [0002] Calcium Hexaboride (CaB 6 ) is an alkaline earth boride ceramic material composed of alkaline earth element calcium (Ca) and non-metallic element (B), with a gray-black appearance. At room temperature, CaB 6 There are three states: powder, polycrystalline and single crystal. CaB 6 Insoluble in hydrochloric acid, hydrofluoric acid, but soluble in nitric acid, sulfuric acid and molten alkali. In recent years, in the research field of borides and non-metallic boron-containing compound functional ceramic materials, in order to reduce the sintering temperature and enhance the high-temperature mechanical properties, the requirements for nanometerization of powder materials have been put forward. With the miniaturization of high-speed integrated circuits, microwave and millimeter wave devices, qua...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626B82Y30/00
Inventor 张琳闵光辉于化顺冯刚
Owner SHANDONG UNIV
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