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High-purity silicon carbide powder and preparation method therefor

A high-purity silicon carbide powder, silicon carbide powder technology, applied in the direction of silicon carbide, carbide, etc., can solve the problems of high-purity silicon carbide powder particle size distribution range, difficult impurity content, high toxicity, etc., to achieve good decarbonization effect , low degree of oxidation, controllable particle size

Active Publication Date: 2019-09-10
SICC CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, in order to improve the purity of the prepared silicon carbide powder, impurities are often removed by hydrometallurgy or solvent pickling. This method of removing impurities is large in pollution and toxicity, and it is easy to introduce new impurities, and the effect of removing impurities is poor. It is difficult to further reduce the content, and it is difficult to produce high-purity silicon carbide powder with a purity greater than 99.999%; and the particle size distribution range of the high-purity silicon carbide powder prepared by the existing method is large, and it is difficult to control

Method used

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Embodiment approach

[0045] According to one embodiment of the present application, the preparation method of high-purity silicon carbide powder comprises the following steps:

[0046] 1) One-time synthesis: Mix high-purity carbon powder and high-purity silicon powder evenly under vacuum conditions at a molar ratio of 1:1, place them in a graphite crucible, and place them in a medium-frequency induction heating furnace; grow in a medium-frequency induction heating furnace The chamber is evacuated to 1 x 10 -2 to 1×10 -3 Pa and raise the temperature to 1000-1500°C, stabilize for 10-15h to obtain β-silicon carbide powder;

[0047] 2) Secondary synthesis: continue to heat up to 1900-2200°C, and fill with high-purity argon and / or high-purity helium until the pressure in the growth chamber is stable at 800-900mbar, and keep the temperature and pressure stable for 20-40h of conversion reaction, Obtain α silicon carbide powder;

[0048] 3) Recrystallization: Evacuate again until the pressure in the gr...

Embodiment 1

[0054] The preparation of embodiment 1 high-purity silicon carbide powder 1#

[0055] 1) One-time synthesis: Mix high-purity carbon powder and high-purity silicon powder evenly under vacuum conditions at a molar ratio of 1:1, place them in a graphite crucible, and place them in a medium-frequency induction heating furnace; grow in a medium-frequency induction heating furnace The chamber is evacuated to 1 x 10 - 2 Pa and raise the temperature to 1000°C, and stabilize for 10 hours to obtain β-silicon carbide powder;

[0056] 2) Secondary synthesis: continue to raise the temperature to 1900°C, and fill it with high-purity argon and / or high-purity helium until the pressure in the growth chamber is stable at 800mbar, and keep the temperature and pressure stable for 20 hours of conversion reaction to obtain α-silicon carbide powder;

[0057] 3) Recrystallization: Evacuate again until the pressure in the growth chamber is stable at 10mbar, and raise the temperature to 2800°C, maint...

Embodiment 2

[0060] Embodiment 2 Preparation of high-purity silicon carbide powder 1#-7#, comparative silicon carbide powder D1#-D3#

[0061] According to the preparation method of the high-purity silicon carbide powder 1# of Example 1, high-purity silicon carbide powder 1#-7# and contrast silicon carbide powder D1#-D3# were prepared respectively, which were compared with the preparation of high-purity silicon carbide powder 1# The differences in the methods are shown in Table 1.

[0062] Table 1

[0063]

[0064] Compared with the hydrometallurgical impurity removal in high-purity silicon carbide powder D3#, the mixed strong acid of hydrofluoric acid and hydrochloric acid is used to soak and then filter and wash.

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Abstract

The application discloses high-purity silicon carbide powder and a preparation method therefor and belongs to the field of preparation of semiconductor materials. The preparation method for the high-purity silicon carbide powder comprises the following steps: providing beta silicon carbide powder and / or alpha silicon carbide powder as an initial silicon carbide powder material; recrystallizing theinitial silicon carbide powder material, so as to prepare a silicon carbide polycrystalline block; and subjecting the silicon carbide polycrystalline block to decarburization purification, thereby preparing the high-purity silicon carbide powder, wherein a temperature of recrystallization is not low 2,500 DEG C. According to the high-purity silicon carbide powder and the preparation method therefor, the purity of the prepared high-purity silicon carbide powder is improved by a recrystallization method, impurity removal by a hydrometallurgy or pickling step is not required, and the high-puritysilicon carbide powder is light in pollution, low in toxicity and high in operability; by a decarburization purification step of introducing oxygen gas to pure silicon carbide powder at a temperatureof 600 DEG C to 799 DEG C, the decarburization effect of the carbonized polycrystalline block is good, the prepared high-purity silicon carbide powder is low in degree of oxidation, and the influenceon an oxygen impurity is low when the high-purity silicon carbide powder is applied to growth of silicon carbide monocrystals; and by the preparation method, the high-purity silicon carbide powder with purity not lower than 99.9999% can be prepared, and the particle size of the high-purity silicon carbide powder is controllable.

Description

technical field [0001] The application relates to a high-purity silicon carbide powder and a preparation method thereof, belonging to the field of semiconductor material preparation. Background technique [0002] With the development of third-generation semiconductor technology, the production scale of third-generation semiconductor silicon carbide materials is gradually expanding. At the same time, with the in-depth research on the application of silicon carbide materials, the market has higher and higher requirements for silicon carbide substrates. Resistivity, as one of the important parameters reflecting the performance of silicon carbide substrates, is mainly affected by the impurity content in silicon carbide wafers. The main sources of impurities in silicon carbide ingots include crucible insulation materials used for growth, protective gases used in the growth process, and silicon carbide powder used for growing ingots. Therefore, reducing the impurity content in s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/956
CPCC01P2004/60C01P2006/80C01B32/956
Inventor 靳婉琪耶夫亨·布乐琴科王超贾河顺王雅儒
Owner SICC CO LTD
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