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Preparation method of high-purity YB4 powder body

A technology of YB4 and powder, applied in the field of preparation of YB4 powder, can solve the problems of high price, inability to realize large-scale production, complicated process, etc.

Inactive Publication Date: 2011-11-30
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently preparing YB 4 There are four main methods: the first method is to use pure metal Y and simple substance B, and obtain it by direct reaction at high temperature. The advantage of this method is that the synthesized YB 4 The purity is very high, and other impurities will not be introduced in the reaction process. The disadvantage is that the raw materials used in this method are very expensive and difficult to obtain, so large-scale production cannot be realized; the second method is boron thermal method, that is, Y 2 o 3 Powder and simple substance B are used as raw materials, and YB is synthesized at high temperature 4 , this method synthesizes YB 4 The purity is high, but it is expensive to use B as a raw material; the third method is to prepare larger-sized YB by controlling the ratio of Y, B, and Al 4 crystal, but this method is not only expensive in raw materials, but also complex in process, difficult to achieve practical application; the fourth method is based on yttrium halide YCl 3 ·7H 2 O, elemental B and Al are used as raw materials and directly synthesized at high temperature, but the disadvantage of this method is that the raw materials are expensive and the reaction process is relatively complicated.

Method used

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  • Preparation method of high-purity YB4 powder body
  • Preparation method of high-purity YB4 powder body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) put Y 2 o 3 and B 4 C powder was dried at 200°C for 5h, and then Y 2 o 3 and B 4 C two kinds of raw material powder by mole ratio Y 2 o 3 : B 4 C=1: 2.0 Weigh 4.47g, and mix and grind 3h in agate mortar;

[0017] (2) Press the mixed raw material powder into a cylinder of Φ10×10mm under a pressure of about 3MPa on a powder tablet press, and put it into a graphite mold. Using a spark plasma sintering system (SPS), vacuum Under the conditions (the vacuum degree used in the examples is the initial vacuum degree, and the vacuum pump has been running to evacuate during the reaction process), from room temperature to 1700 ° C, keep it warm for 30 minutes, and then cool to room temperature with the furnace;

[0018] (3) Take out the obtained block, grind it in an agate mortar, then place it in 2mol / L dilute hydrochloric acid, heat it to 60°C, stir it with a stirrer for 120min, then filter it dry, and repeat it with deionized water. Rinse to neutral;

[0019] (4) ...

Embodiment 2

[0021] (1) put Y 2 o 3 and B 4 C powder was dried at 200°C for 5h, and then Y 2 o 3 and B 4 C two kinds of raw material powder by mole ratio Y 2 o 3 : B 4 C=1: 2.1 Weigh 4.54g, put it into an agate mortar and mix and grind for 3h;

[0022] (2) Press the mixed raw material powder into a cylinder of Φ10×10mm under a pressure of about 3MPa on a powder tablet press, and put it into a graphite mold. Using a spark plasma sintering system (SPS), vacuum Under the conditions, rise from room temperature to 1700°C, keep it warm for 30 minutes, and then cool down to room temperature with the furnace;

[0023] (3) Take out the obtained block, grind it in an agate mortar, then place it in 2mol / L dilute hydrochloric acid, heat it to 60°C, stir it with a stirrer for 120min, then filter it dry, and repeat it with deionized water. Rinse to neutral;

[0024] (4) Place the prepared powder in a drying oven and dry at 100°C for 2 hours to obtain high-purity YB 4 Powder.

Embodiment 3

[0026] (1) put Y 2 o 3 Powder and B 4 C powder was dried at 200°C for 5h, and then Y 2 o 3 and B 4 C two kinds of raw material powder by mole ratio Y 2 o 3 : B 4 C=1: 2.3 weighs 4.69g, adds it in the agate mortar and grinds 3h;

[0027] (2) Put the mixed raw material powder directly into the graphite mold, use the spark plasma sintering system (SPS), under the vacuum condition of 20Pa, rise from room temperature to 1700°C, keep it warm for 30min, and then cool to room temperature with the furnace;

[0028] (3) Take out the obtained block, grind it in an agate mortar, then place it in 2mol / L dilute hydrochloric acid, heat it to 60°C, stir it with a stirrer for 10min, then filter it dry, and repeat it with deionized water. Rinse to neutral;

[0029] (4) Place the prepared powder in a drying oven and dry at 100°C for 2 hours to obtain high-purity YB 4 Powder.

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Abstract

The invention relates to a preparation method of YB4 powder body, which comprises the following steps of: 1) taking Y2O3 and B4C raw material powder and uniformly mixing; 2) pressing the uniformly mixed raw material powder into block bodies; then, putting the block bodies into a die; under a vacuum condition, raising the temperature to 1700 DEG C to 2000 DEG C; preserving the temperature for 15 to 120 minutes; then, cooling with a stove to room temperature; 3) taking out the obtained block bodies; grinding; putting the block bodies into hydrochloric acid; heating; stirring; filtering to be dry; washing with deionized water to be natural; and 4) drying the obtained powder body. According to the invention, commercially available Y2O3 and B4C powder is used as raw material, is easy to obtainand has low price; in the reaction process, element C and element O are combined for generating CO gas for volatilization; element Y and element B are combined for generating YB4; the introduction ofother foreign matter is effectively avoided; high-purity YB4 powder body is obtained; the prepared YB4 has single phase; the size of crystal grain is from 3 to 10 mu m; and the product purity is higher than 99.5%.

Description

technical field [0001] The present invention relates to YB 4 The preparation method of the powder belongs to the material synthesis method, and the prepared YB 4 Powder can be used in fields such as ceramic materials and electronic materials. Background technique [0002] In recent years, a lot of research has been done on borides at home and abroad. Since borides usually have excellent electrical conductivity, high hardness and melting point, they can be used as electronic materials and ceramic materials. [0003] Currently preparing YB 4 There are four main methods: the first method is to use pure metal Y and simple substance B, and obtain it by direct reaction at high temperature. The advantage of this method is that the synthesized YB 4 The purity is very high, and other impurities will not be introduced in the reaction process. The disadvantage is that the raw materials used in this method are very expensive and difficult to obtain, so large-scale production cannot ...

Claims

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Application Information

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IPC IPC(8): C01B35/04
Inventor 李俊国何勇袁辉平郭启龙张联盟
Owner WUHAN UNIV OF TECH