Production process of hafnium disilicide

A production process, a technology of disilicidation, applied in the direction of metal silicide, etc., can solve the problems of poor fluidity, low degree of alloying, and insufficient combination, etc., and achieve the effect of reasonable process, high purity, and low cost

Active Publication Date: 2020-10-16
辽宁中色新材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods of hafnium disilicide mainly include the direct synthesis of hafnium sponge and the re-synthesis of metal silicon by carbon reduction of hafnium dioxide. The direct synthesis of hafnium sponge is the direct synthesis of hafnium sponge and silicon as raw materials. Remelting with hafnium is not good, silicon is in a liquid state, the fluidity is not good, it cannot be fully combined with silicon, the degree of alloying is not high, and there is elemental silicon
Carbon reduction of hafnium dioxide to produce metal silicon and resynthesis method is to use elemental carbon to reduce hafnium dioxide to produce metal hafnium. During the reduction process, in order to fully reduce hafnium dioxide, only excess carbon is required, so that free carbon exists in metal hafnium. Silicon carbide impurities will be produced during the process of compounding with silicon; if the amount of carbon is insufficient, there will be a small amount of hafnium oxide that has not been reduced. After compounding with silicon, there will be hafnium oxide, which will affect the purity of the product and cannot reach the high-purity standard.

Method used

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  • Production process of hafnium disilicide
  • Production process of hafnium disilicide
  • Production process of hafnium disilicide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Mixing

[0028] a. Hafnium dioxide powder has a purity of 99.9% and a fineness of 200 mesh;

[0029] b. Silicon powder is 325 mesh silicon powder, and the purity of silicon powder is 99.99%;

[0030] c. Add 8.8kg of zirconia powder and 1.2kg of silicon powder to 100g of carboxymethyl cellulose as a binder, put it into a vacuum ball mill and fill it with argon protection, and mix the materials by ball milling. The ball milling speed is 120 rpm, ensuring 10 hours, mix well, obtain mixed material;

[0031] (2) Briquetting

[0032] After mixing the materials in step (1), according to 600 grams per block, use a three-beam four-column hydraulic press to press into a round cake-shaped block, the pressing pressure is 20MPa, and the size of the briquetting block is φ80mm×25mm;

[0033] (3) Sintering reduction

[0034] Put the block material pressed in step (2) into the quartz crucible of a 200kg vacuum sintering furnace. The input amount of raw materials is 51kg, vacuumi...

Embodiment 2

[0040] (1) Mixing

[0041] a. Hafnium dioxide powder has a purity of 99.9% and a fineness of 200 mesh;

[0042] b. Silicon powder is 325 mesh silicon powder, and the purity of silicon powder is 99.99%;

[0043] c. Add 8.78kg of zirconia powder and 1.22kg of silicon powder to 100g of carboxymethyl cellulose as a binder, put it into a vacuum ball mill and fill it with argon protection, and mix the materials by ball milling. The ball milling speed is 120 rpm, ensuring 10 hours, mix well, obtain mixed material;

[0044] (2) Briquetting

[0045] After mixing the materials in step (1), according to 600 grams per block, use a three-beam four-column hydraulic press to press into a round cake-shaped block, the pressing pressure is 20MPa, and the size of the briquetting block is φ80mm×25mm;

[0046] (3) Sintering reduction

[0047] Put the block material pressed in step (2) into the quartz crucible of a 200kg vacuum sintering furnace. The input amount of raw materials is 51kg, vacuu...

Embodiment 3

[0053] (1) Mixing

[0054] a. Hafnium dioxide powder has a purity of 99.9% and a fineness of 200 mesh;

[0055] b. Silicon powder is 325 mesh silicon powder, and the purity of silicon powder is 99.99%;

[0056] c. Add 8.79kg of zirconia powder and 1.21kg of silicon powder to 100g of carboxymethyl cellulose as a binder, put it into a vacuum ball mill and fill it with argon protection, and mix the materials by ball milling. The ball milling speed is 120 rpm, ensuring 10 hours, mix well, obtain mixed material;

[0057] (2) Briquetting

[0058] After mixing the materials in step (1), according to 600 grams per block, use a three-beam four-column hydraulic press to press into a round cake-shaped block, the pressing pressure is 20MPa, and the size of the briquetting block is φ80mm×25mm;

[0059] (3) Sintering reduction

[0060] Put the block material pressed in step (2) into the quartz crucible of a 200kg vacuum sintering furnace. The input amount of raw materials is 51kg, vacuu...

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Abstract

The invention discloses a production process of hafnium disilicide. The production process comprises the following steps: ball-milling and mixing zirconium dioxide powder and silicon powder under a vacuum condition, briquetting by using a hydraulic machine, sintering and finishing in a vacuum sintering furnace, removing white silicon dioxide powder coated on the surface of hafnium, ball-milling ina vacuum ball mill, adding sodium hydroxide, adding distilled water with the temperature of 60 DEG C, and drying to obtain silicon-containing hafnium powder; detecting the content of silicon in the silicon-containing hafnium powder, adding silicon powder according to the content of silicon in the hafnium powder, carrying out ball milling for 5 hours in a vacuum ball mill under the protection of inert argon, putting into a vacuum self-propagating combustion furnace, vacuumizing, heating a thermal electrode, igniting the hafnium powder, making the hafnium powder and the silicon powder carry outa self-propagating combination reaction to obtain hafnium disilicide. Hafnium dioxide powder is used as a raw material, and the raw material cost is lower than sponge hafnium cost; according to the method, the whole process is reasonable in technology and suitable for industrial production, the obtained hafnium disilicide product is high in purity, and the alloying degree can reach 100%.

Description

technical field [0001] The invention relates to a production process of hafnium disilicide. Background technique [0002] Hafnium disilicide is a transition metal silicide. It has the characteristics of high melting point, high hardness, high wear resistance and oxidation resistance. It is used as ceramic material and various high temperature resistant parts and functional parts. Hafnium disilicide nanomaterials show special electrical and optical properties, and have potential application value in the field of optoelectronics. [0003] At present, the methods of hafnium disilicide mainly include the direct synthesis of hafnium sponge and the re-synthesis of metal silicon by carbon reduction of hafnium dioxide. The direct synthesis of hafnium sponge is the direct synthesis of hafnium sponge and silicon as raw materials. Remelting with hafnium is not good, silicon is in a liquid state, the fluidity is not good, it cannot be fully combined with silicon, the degree of alloying...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/06
CPCC01B33/06C01P2006/80C01P2002/72
Inventor 张洪涛
Owner 辽宁中色新材科技有限公司
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