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Preparation method of submicron transition metal boride powder with low oxygen content

A transition metal, sub-micron-level technology, applied in the direction of metal borides, boron/borides, etc., can solve the problems of many impurities, low activity, coarse powder particle size, etc., and achieve strong controllability, low agglomeration degree, and oxygen content low effect

Inactive Publication Date: 2012-04-18
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Currently, MB 2 The synthesis method mainly contains following several kinds: 1) direct synthesis method: take metal M simple substance and boron as raw material, directly synthesize in inert gas or vacuum high-temperature reaction, the synthetic powder purity of this method is high, and synthesis condition is relatively simple, but raw material is relatively expensive, synthetic MB 2 Coarse powder particle size and low activity are not conducive to powder sintering and post-processing
2) Self-propagating combustion synthesis method: This synthesis process is based on the reactant MO 2 , Mg and B 2 o 3 The huge heat released by the solid-state reaction of etc. maintains the spontaneous continuous progress of the reaction, so that the reactant is transformed into MB 2 ; This method is simple in process, fast in speed, short in time, extremely small in energy consumption, high in activity of the synthesized powder, and beneficial to sintering and post-processing; , product structure and performance are not easy to control is also its shortcoming
However, the traditional MO 2 There is a key problem in the reduction method - the reduction of particle size and the reduction of oxygen content are always contradictory: at low temperature, although ultrafine MB can be obtained 2 powder, but the oxygen content of the powder is high; at high temperature, although MB with low oxygen content can be obtained 2 Powder, but the particle size of the powder is relatively coarse, reaching above the micron level

Method used

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  • Preparation method of submicron transition metal boride powder with low oxygen content
  • Preparation method of submicron transition metal boride powder with low oxygen content
  • Preparation method of submicron transition metal boride powder with low oxygen content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First weigh 100mmol of ZrO 2 and 400mmol of elemental boron, with ethanol as solvent, Si 3 N 4 The balls were used as ball milling media, mixed on a roller mill for 24 hours, and dried by rotary evaporation to obtain ZrO 2 / B mixed powder; then ZrO 2 / B mixed powder is placed in a graphite crucible, heated to 1000°C in a graphite furnace at an air pressure lower than 200Pa and kept for 2 hours to obtain ZrB 2 / B 2 o 3 Powder.

[0027] The above ZrB 2 / B 2 o 3 Put the powder in a beaker, add deionized water, heat and stir, the water temperature is controlled at 80°C, stir for 6 hours, and centrifuge for 20 minutes to obtain ZrB 2 Powder.

[0028] ZrB will be obtained 2 The powder is placed in a graphite crucible, heated to 1500°C in a graphite furnace with an air pressure lower than 200Pa and kept at a temperature of 3 hours to obtain the submicron ZrB with low oxygen content 2 Powder.

[0029] Oxygen content was measured with an oxygen and nitrogen analyzer...

Embodiment 2

[0033] First weigh 100mmol of HfO 2 and 400mmol of elemental boron, with ethanol as solvent, Si 3 N 4 The balls are used as the ball milling medium, mixed on a roller ball mill for 24 hours, and dried by rotary evaporation to obtain HfO 2 / B mixed powder; then HfO 2 / B mixed powder is placed in a graphite crucible, heated to 1000°C in a graphite furnace at an air pressure lower than 200Pa and kept for 2 hours to obtain HfB 2 / B 2 o 3 Powder.

[0034] The above HfB 2 / B 2 o 3 Put the powder in a beaker, add deionized water, heat and stir, the water temperature is controlled at 80°C, stir for 6 hours, and centrifuge for 20 minutes to obtain HfB 2 Powder.

[0035] HfB will be obtained 2The powder is placed in a graphite crucible, heated to 1500°C in a graphite furnace with an air pressure lower than 200Pa and kept for 3 hours to obtain the low-oxygen content submicron HfB 2 Powder.

[0036] The measured oxygen content was 0.2 wt%.

[0037] image 3 The HfB prepared...

Embodiment 3

[0040] The difference between this example and Example 1 is that "400 mmol of elemental boron" is replaced with "300 mmol of elemental boron", and the rest of the content is the same as that of Example 1.

[0041] Know through detecting and analyzing: the ZrB that present embodiment makes 2 The average particle diameter of the powder is 400nm, and the oxygen content is 0.5wt%.

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Abstract

The invention discloses a preparation method of a submicron transition metal boride powder with low oxygen content. The method comprises the following steps: first carrying out ball milling mixing and drying on a transition metal oxide and elementary substance boron to obtain a MO2 / B mixed powder carrying out heat treatment on the MO2 / B mixed powder to obtain a MB2 / B2O3 powder; adding the obtained MB2 / B2O3 powder into water, heating and stirring to dissolve out B2O3 therein and centrifuging to obtain a MB2 powder; carrying out heat treatment on the obtained MB2 powder again. Compared with a prior art, the transition metal boride powder prepared by the method of the invention has advantages of a small particle size of 200-700 nm, low degree of aggregation and an oxygen content about 0.01-1.0wt%; besides the process of the preparation method of the present invention is simple and practical, has strong controllability and is easy for realization of large scale production.

Description

technical field [0001] The present invention relates to a kind of transition metal boride (MB 2 ) powder preparation method, specifically, relates to a low oxygen content submicron transition metal boride (MB 2 ) powder preparation method, which belongs to the technical field of powder preparation. Background technique [0002] Transition metal borides (MB 2 ) has excellent properties such as high melting point, hardness, thermal stability and corrosion resistance. It is widely used in the production of ultra-high temperature structural materials, and has important applications in the fields of mechanical processing, metallurgy and minerals, aerospace and aviation. [0003] Due to inherently strong covalent bonds and low diffusion coefficients, MB 2 It has poor sintering properties and is difficult to densify. From the perspective of raw materials, there are two main factors restricting MB 2 The sintering performance of the powder, one is the particle size of the powder...

Claims

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Application Information

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IPC IPC(8): C01B35/04
Inventor 张国军郭伟明阚艳梅
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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