A kind of preparation method of superfine tantalum carbide niobium solid solution powder

A tantalum carbide and solid solution technology, applied in the field of new material preparation, can solve the problems of high carbonization temperature, agglomeration, slow diffusion speed, etc., and achieve the effects of low carbonization temperature, small particle size, and short process.

Active Publication Date: 2011-12-07
长沙伟徽高科技新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the NbC powder grains are coarse, the activity is low, the diffusion speed is slow, and the agglomeration phenomenon is serious during the alloy sintering process, which makes it difficult to meet the increasingly higher requirements of cemented carbide.
[0004] The traditional method of preparing NbC powder is to mix common Nb 2 o 5 The powder is mixed with solid carbon ball mill, carbonized once in carbon tube furnace or carbonized once in carbon tube furnace and twice in vacuum furnace. About 1~3μm

Method used

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  • A kind of preparation method of superfine tantalum carbide niobium solid solution powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] After compressing the purchased slurry-like niobium hydroxide and slurry-like tantalum hydroxide respectively and drying them in an oven at 200°C, 126 kilograms of nanoscale niobium hydroxide and 159 kilograms of nanoscale tantalum hydroxide were obtained; 20nm-90nm.

[0028] Get above-mentioned 14.07 kilograms of niobium hydroxide and 36.75 kilograms of tantalum hydroxide and mix with 8.99 kilograms of carbon black again, heat up to 1300 ℃ through slowly 3 hours, high temperature holding time is 11 hours, when vacuum degree reaches 10Pa, end carbonization. Cool with H2 for 14 hours. Ball mill after discharge. The particle size of the Fsss sample was measured to be 0.64 μm, and the chemical composition met the requirements. The specific composition is shown in Table 1.

Embodiment 2

[0030] After compressing the purchased slurry-like niobium hydroxide and slurry-like tantalum hydroxide respectively and drying them in an oven at 200°C, 126 kilograms of nanoscale niobium hydroxide and 159 kilograms of nanoscale tantalum hydroxide were obtained; 20nm-90nm.

[0031] Then 23.45 kg of niobium hydroxide and 28.82 kg of tantalum hydroxide were mixed with 9.95 kg of carbon black, and the temperature was slowly raised to 1320°C for 3 hours, and the high temperature holding time was 12 hours. When the vacuum reached 12Pa, the carbonization was completed. Cool with H2 for 13 hours. Ball mill after discharge. The Fsss particle size of the sample was measured to be 0.69 μm, and the chemical composition met the requirements. The specific composition is shown in Table 1.

Embodiment 3

[0033] After compressing the purchased slurry-like niobium hydroxide and slurry-like tantalum hydroxide respectively and drying them in an oven at 200°C, 126 kilograms of nanoscale niobium hydroxide and 159 kilograms of nanoscale tantalum hydroxide were obtained; 20nm-90nm.

[0034] Mix 5.92 kg of niobium hydroxide and 43.40 kg of tantalum hydroxide with 8.13 kg of carbon black, slowly heat up to 1280° C. for 3 hours, hold high temperature for 13 hours, and finish carbonization when the vacuum reaches 12 Pa. Pass H2 to cool, and the cooling time is 12 hours. Ball mill after discharge. The Fsss particle size of the sample was measured to be 0.65 μm, and the chemical composition met the requirements. The specific composition is shown in Table 1.

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Abstract

The invention belongs to the field of new material preparation and particularly provides a preparation method of superfine tantalum-niobium carbide solid solution powder. The preparation method comprises the following specific steps: a, separately compressing slurry-shaped niobium hydroxide and tantalum hydroxide, and then drying at the temperature of 180-250 DEG C for 6-12 hours to remove water, thus obtaining niobium hydroxide powder and tantalum hydroxide powder with the particle size of 20-90 nm; and b, uniformly mixing the niobium hydroxide powder and tantalum hydroxide powder with carbon black based on the condition that the mass ratio of carbon black to niobium hydroxide powder to tantalum hydroxide powder is 1:(0.72-2.75):(2.24-5.29), carbonizing in a vacuum furnace while controlling the carbonization temperature at 1250-1350 DEG C, continuously vacuumizing, and terminating the carbonization process when the vacuum degree reaches 10-12 Pa; and then cooling for 12-16 hours, and after discharging the material, ball-milling to obtain the tantalum-niobium carbide powder with the Fsss particle size less than 0.7 mu m. The preparation method provided by the invention has low carbonization temperature, the prepared niobium carbide powder has small particle size, and the operation process is simple and easy to implement.

Description

technical field [0001] The invention belongs to the field of new material preparation, and adopts a method combining low-temperature drying and vacuum smelting to prepare superfine tantalum-niobium carbide solid solution powder. Background technique [0002] The main application field of NbC is cemented carbide inserts. One of its functions: as a cemented carbide grain growth inhibitor, after adding NbC, it can prevent the growth of grains in the cemented carbide sintering process; its second function is Together with TiC, it forms the third dispersed phase except WC and Co, which significantly increases the thermal shock resistance, hot compression and oxidation resistance of cemented carbide and improves the hot hardness of cemented carbide. [0003] Due to the continuous improvement of application requirements and the harsh application environment, the metallographic structure of cemented carbide is more uniform and finer, which puts forward higher requirements for the pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C29/06C22C1/04
Inventor 郭伟
Owner 长沙伟徽高科技新材料有限公司
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