Method for preparing highly-pure beta-Sialon ceramic powders

A ceramic powder, high-purity technology, applied in the field of ceramic materials, can solve problems such as high content, high requirements, and inevitable impurities

Inactive Publication Date: 2010-04-28
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

At present, the common methods of synthesizing β-Sialon ceramic powder are: (1) high-temperature solid-state reaction method, the preparation process of this method is relatively complicated, and the required synthesis temperature is high (about 1700 ° C)
(2) Self-propagating high-temperature synthesis method, which is a rapid milling method, but the process equipment is complicated, the requirements are high, and the reaction process is difficult to control
(3) Carbothermal reduction nitriding method, this method has a wide range of applications, mainly due to relatively low requirements for equipment and processes, but there are many influencing factors in the synthesis process, and the impurity content in the product is relatively high
[0006] The Chinese invention patent application with the publication number CN1168872A also provides a preparation method of Sialon ceramic powder, which uses a high-temperature self-propagating process. The process equipment is complex, the requirements are high, and the reaction process is difficult to control.
[0007] Furthermore, the Chinese invention patent application with the publication number CN1270153A provides a preparation method of Sialon combined with SiC powder, which mainly uses river sand as a raw material, and there is a large amount of SiC in the synthesis product phase. 2 O (2.9%), Na 2 O (3.5%) content is high, not suitable for high temperature industrial applications
[0008] In short, the initial raw materials used in the method of preparing β-Sialon ceramic powder provided by published patents and literatures are all mechanically mixed, and uneven mixing of raw materials leads to high synthesis temperature and inevitable impurity phases.
In addition, there is no published invention patent about the preparation of β-Sialon ceramic powder by nano-casting using ordered mesoporous silica as raw material

Method used

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  • Method for preparing highly-pure beta-Sialon ceramic powders
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  • Method for preparing highly-pure beta-Sialon ceramic powders

Examples

Experimental program
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Effect test

Embodiment 1

[0041]The molar ratio of silicon and aluminum in the initial proportion is 1:1, and the molar ratio of silicon and sucrose is 1:0.42. First dissolve 4.45g of anhydrous aluminum trichloride into 10g of deionized water, then add 3.0g of sucrose, stir for a while to completely dissolve the sucrose, then add 0.34g of sulfuric acid, then slowly add 2.0g of SBA-15 to the above solution, stir Evenly, the obtained product was dried at 80°C for 6 hours to allow the water to evaporate completely, and then the temperature was raised to 160°C for 6 hours of heat treatment for pre-carbonization. In the second step, continue to add a solution consisting of 1.8g of sucrose, 0.2g of sulfuric acid and 10g of deionized water to the above-mentioned pre-carbonized product, and repeat the drying at 80°C and heat treatment at 160°C. The third step is to calcine at 800°C for 6 hours under the protection of argon with an argon flow rate of 0.2 L / min to complete the entire carbonization process and ob...

Embodiment 2

[0043] The molar ratio of silicon and aluminum in the initial proportion is 1:1, and the molar ratio of silicon and sucrose is 1:0.5. First dissolve 4.45g of anhydrous aluminum trichloride into 10g of deionized water, then add 3.6g of sucrose, stir for a while to completely dissolve the sucrose, then add 0.4g of sulfuric acid, then slowly add 2.0g of SBA-15 to the above solution, stir Evenly, the obtained product was dried at 80°C for 6 hours to allow the water to evaporate completely, and then the temperature was raised to 160°C for 6 hours of heat treatment for pre-carbonization. In the second step, continue to add a solution consisting of 2.16g of sucrose, 0.24g of sulfuric acid and 10g of deionized water to the above-mentioned pre-carbonized product, and repeat the drying at 80°C and heat treatment at 160°C. The third step is to calcine at 800°C for 6 hours under the protection of argon with an argon flow rate of 0.2 L / min to complete the entire carbonization process and o...

Embodiment 3

[0045] The molar ratio of silicon and aluminum in the initial proportion is 1:1, and the molar ratio of silicon and sucrose is 1:0.58. First dissolve 4.45g of anhydrous aluminum trichloride into 10g of deionized water, then add 4.2g of sucrose, stir for a while to completely dissolve the sucrose, then add 0.48g of sulfuric acid, then slowly add 2.0g of SBA-15 to the above solution, stir Evenly, the obtained product was dried at 80°C for 6 hours to allow the water to evaporate completely, and then the temperature was raised to 160°C for 6 hours of heat treatment for pre-carbonization. In the second step, continue to add a solution consisting of 2.52g of sucrose, 0.3g of sulfuric acid and 10g of deionized water to the above-mentioned pre-carbonized product, and repeat the drying at 80°C and heat treatment at 160°C. The third step is to calcine at 800°C for 6 hours under the protection of argon with an argon flow rate of 0.2 L / min to complete the entire carbonization process and ...

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Abstract

The invention provides a method for preparing highly-pure beta-Sialon ceramic powders, which combines a carbothermal reduction nitridation process and nano-pouring technology and comprises the following specific steps: firstly, taking ordered mesoporous silicon dioxide as a main raw material, taking soluble inorganic aluminum salt as an aluminum oxide precursor, taking an organic small molecular compound as a carbon source, and preparing a compound of mesoporous carbon/silicon oxide/aluminum oxide through nanometer pouring; then performing carbothermal reduction nitridation on the compound of the mesoporous carbon/the silicon oxide/the aluminum oxide to prepare a sample; and finally, calcining the sample in air to remove residual carbon, and cooling the sample after residual carbon is removed to prepare a product. The method has the advantages that the synthesis temperature of the preparation method is relatively low, and is favorable for reducing the required energy consumption in production; and the purity of the prepared beta-Sialon ceramic powders is high, and the particle shapes are mainly in a long rod-like shape. The preparation method can be widely used in fields of space flight, metallurgy, chemical industry and the like.

Description

technical field [0001] The invention belongs to the technical field of ceramic materials, and in particular relates to a preparation method for synthesizing high-purity β-Sialon ceramic powder by using a carbothermal reduction nitriding process combined with a nano-casting technology and the β-Sialon ceramic powder prepared by the method. Background technique [0002] and high performance nitride material Si 3 N 4 The structure is similar to that of Sialon as Si 3 N 4 The solid solution can also be divided into two crystal forms, the low-temperature phase α-Sialon and the high-temperature phase β-Sialon. Wherein β-Sialon is β-Si 3 N 4 Z Si-N bonds in the structure are replaced by Z Al-O bonds, and its composition can be expressed as Si 6-z Al z o z N 8-z (where 0<Z≤4.2). Since β-Sialon is easy to grow into a columnar shape, it produces a whisker-like toughening effect, which makes β-Sialon have higher fracture strength and fracture toughness than α-Sialon. Due ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/599
Inventor 刘茜颜强王明辉
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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