CN112226815A - Pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT (physical vapor transport) method - Google Patents
Pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT (physical vapor transport) method Download PDFInfo
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- CN112226815A CN112226815A CN202011276502.9A CN202011276502A CN112226815A CN 112226815 A CN112226815 A CN 112226815A CN 202011276502 A CN202011276502 A CN 202011276502A CN 112226815 A CN112226815 A CN 112226815A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
Abstract
A pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT method relates to pretreatment technology of silicon carbide powder. The method aims to solve the technical problem that gas transportation is influenced by powder sintering in the growth process of the existing PVT method silicon carbide single crystal. The method comprises the following steps: putting the silicon carbide powder into a vacuum induction furnace with stirring, and heating the silicon carbide powder to be treated in a vacuum-pumping state; then argon is charged again, and heating treatment is continued while stirring; then cooling to room temperature to finish the pretreatment of the silicon carbide powder. A layer of relatively loose graphite isolation layer is formed on the surface of the silicon carbide powder, the stable isolation layer prevents the silicon carbide particles from contacting with each other, the sintering of the silicon carbide under the high-temperature condition is reduced, and the defects are reduced when the PVT method silicon carbide single crystal grows. The method can be used in the field of silicon carbide single crystal growth.
Description
Technical Field
The invention relates to a pretreatment method of silicon carbide powder.
Background
The PVT method is a commonly used method for growing silicon carbide single crystals, and the specific process can be divided into the following four steps:
firstly, putting a silicon carbide powder raw material into a graphite crucible, mounting a seed crystal on a crucible cover, wherein the seed crystal is used as a seed for growth of a silicon carbide crystal, and then putting the graphite crucible into a reaction furnace;
secondly, vacuumizing the crucible reaction system to exhaust air, silicon carbide powder and gas adsorbed by the container;
thirdly, heating to 1800-2000 ℃, and filling argon with certain pressure during the heating; heating to sublimate and decompose the silicon carbide into gas containing carbon and silicon elements, wherein the gas can be transported upwards along with the temperature gradient and generate a silicon carbide crystal on the seed crystal;
and fourthly, naturally cooling to obtain the silicon carbide single crystal.
During the growth process of the PVT method silicon carbide crystal, the gas transportation has important influence on the growth of the crystal, and the defects such as polytype, stacking faults, micropipes and the like can be generated due to the uneven gas distribution or unstable gas transportation. In the growth process of the silicon carbide crystal by the PVT method at present, the silicon carbide powder gradually generates an inevitable sintering phenomenon in a raw material area due to high temperature, relatively large crystal grains continuously generated by sintering interfere with the transportation of gas, and further the growth condition of a crystal growth area is unstable and defects are generated.
Disclosure of Invention
The invention provides a pretreatment method of silicon carbide powder for growing silicon carbide single crystals by a PVT method, aiming at solving the technical problem that gas transportation is influenced by powder sintering in the existing PVT method silicon carbide single crystal growing process.
The pretreatment method of the silicon carbide powder for growing the silicon carbide single crystal by the PVT method comprises the following steps:
firstly, putting silicon carbide powder into a vacuum induction furnace with stirring, and vacuumizing to 10 DEG-3-10-5Pa, heating to 500-800 deg.C and maintaining for 10-30 min while maintaining vacuum degree at 10-3-10-6Pa；
Secondly, filling argon into the vacuum induction furnace until the pressure in the furnace reaches 0.1-1 atm, then starting stirring, and continuously heating to 1400-1600 ℃ at a heating rate of 1000-1500 ℃/h while stirring and keeping for 5-15 min;
and thirdly, turning off heating, naturally cooling, turning off stirring after cooling to 1000-900 ℃, and continuing naturally cooling to room temperature to finish the pretreatment of the silicon carbide powder.
Furthermore, the grain size of the silicon carbide powder in the step one is 0.1-100 microns;
furthermore, the heating rate in the step one is 1000-1500 ℃/h;
furthermore, the stirring speed in the second step is 20-100 r/min;
furthermore, the heating rate in the second step is 1000 to 1500 ℃/h.
According to the invention, a relatively loose graphite isolation layer is formed on the surface of the silicon carbide powder by stirring and heating treatment by utilizing the property that the silicon carbide can be decomposed into graphite when heated at a proper temperature in an inert atmosphere. Because of the stability of graphite at high temperature, the isolating layer can prevent silicon carbide particles from contacting with each other, and further reduces the sintering of silicon carbide under high-temperature conditions. When the pretreated silicon carbide is used for growing the silicon carbide single crystal by a PVT method, the gas transportation is more stable, and the defects generated during the growth of the silicon carbide single crystal are reduced.
The silicon carbide powder material of the method can be used in the field of growing silicon carbide single crystals by a PVT method after pretreatment.
Drawings
FIG. 1 is a Raman spectrum of the silicon carbide powder after pretreatment in example 1;
FIG. 2 is a photograph of the morphology of the pretreated silicon carbide powder after crystal growth by the PVT method in example 1;
FIG. 3 is a photograph of the morphology of untreated silicon carbide powder in comparative example 1 after PVT process growth.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention.
Example 1: the pretreatment method of the silicon carbide powder for growing the silicon carbide single crystal by the PVT method in the embodiment comprises the following steps:
firstly, putting silicon carbide powder with the particle size of 100 microns into a vacuum induction furnace with stirring, and vacuumizing to 10 DEG-3Pa, then heating to 600 deg.C at a heating rate of 1000 deg.C/h for 15min to remove adsorbed gas on the powder surface, while maintaining trueThe void degree is 10-3；
Secondly, filling argon into the vacuum induction furnace until the pressure in the furnace reaches 0.5atm, then starting stirring, stirring at a stirring speed of 50r/min, and simultaneously continuously heating to 1500 ℃ at a heating rate of 1500 ℃/h and keeping for 10 min;
and thirdly, turning off heating, naturally cooling, turning off stirring after cooling to 1000 ℃, and continuing to naturally cool to room temperature to finish the pretreatment of the silicon carbide powder.
The raman spectrum of the silicon carbide powder material and the pretreated silicon carbide powder material of example 1 was measured, and the obtained raman spectrum is shown in fig. 1. As can be seen from FIG. 1, the silicon carbide powder raw material is 792cm-1And 963cm-1The absorption peak of the silicon carbide appears, and the pretreated silicon carbide powder is at 792cm-1And 963cm-1The absorption peak of silicon carbide is substantially disappeared by covering the surface with a graphite layer and is 1375cm-1And 1581cm-1The characteristic absorption band of graphite appears. The description shows that a layer of relatively loose graphite isolating layer is formed on the surface of the silicon carbide powder through stirring and heating treatment.
The pretreated silicon carbide powder obtained in example 1 and the untreated silicon carbide powder were simultaneously used for single crystal growth by the PVT method. The morphology of the residual sintered body in the crucible after the pretreated silicon carbide powder is subjected to single crystal growth is shown in figure 2, the morphology of the residual sintered body in the crucible after the untreated silicon carbide powder is subjected to single crystal growth is shown in figure 3, and comparing the figures 2 and 3, it can be known that the crystal sintering phenomenon is obviously inhibited in the crystal growth process of the treated silicon carbide powder by the PVT method.
The treatment of the embodiment 1 improves the quality of the PVT method silicon carbide single crystal growth, and has low cost and easy implementation.
Example 2: the pretreatment method of the silicon carbide powder for growing the silicon carbide single crystal by the PVT method in the embodiment comprises the following steps:
firstly, putting silicon carbide powder with the particle size of 100 microns into a vacuum induction furnace with stirring, and vacuumizing to 10 DEG-4Pa, then at 1200 ℃/hHeating to 800 deg.C at a heating rate for 10min to remove gas adsorbed on the powder surface, and maintaining vacuum degree at 10-4；
Secondly, filling argon into the vacuum induction furnace until the pressure in the furnace reaches 1atm, then starting stirring, stirring at a stirring speed of 80r/min, and simultaneously continuously heating to 1200 ℃ at a heating rate of 1500 ℃/h and keeping for 10 min;
and thirdly, turning off heating, naturally cooling, turning off stirring after cooling to 1000 ℃, and continuing to naturally cool to room temperature to finish the pretreatment of the silicon carbide powder.
The surface of the pretreated silicon carbide powder of the embodiment forms a relatively loose graphite isolation layer, and when the graphite isolation layer is used for growing crystals by a PVT method, the sintering of the crystals can be inhibited, so that the growth quality of the single crystals is improved.
Claims (5)
1. A pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT method is characterized in that the method comprises the following steps:
firstly, putting silicon carbide powder into a vacuum induction furnace with stirring, and vacuumizing to 10 DEG-3-10-5Pa, heating to 500-800 deg.C and maintaining for 10-30 min while maintaining vacuum degree at 10-3-10-6Pa；
Secondly, filling argon into the vacuum induction furnace until the pressure in the furnace reaches 0.1-1 atm, then starting stirring, and continuously heating to 1400-1600 ℃ at a heating rate of 1000-1500 ℃/h while stirring and keeping for 5-15 min;
and thirdly, turning off heating, naturally cooling, turning off stirring after cooling to 1000-900 ℃, and continuing naturally cooling to room temperature to finish the pretreatment of the silicon carbide powder.
2. The pretreatment method of silicon carbide powder for PVT process growth of silicon carbide single crystal according to claim 1, wherein the particle size of the silicon carbide powder in the first step is 0.1-100 μm.
3. The method of claim 1 or 2, wherein the heating rate in the first step is 1000 to 1500 ℃/hr.
4. The method for pretreating silicon carbide powder for growing silicon carbide single crystals by the PVT method according to claim 1 or 2, wherein the stirring speed in the second step is 20 to 100 r/min.
5. The method of claim 1 or 2, wherein the heating rate in the second step is 1000 to 1500 ℃/hr.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725895A (en) * | 2021-01-29 | 2021-04-30 | 芯璨半导体科技(山东)有限公司 | Method for growing silicon carbide single crystal |
| CN112744816A (en) * | 2021-01-29 | 2021-05-04 | 芯璨半导体科技(山东)有限公司 | Preparation method of silicon carbide powder for silicon carbide single crystal growth |
| CN113026095A (en) * | 2021-03-15 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
| CN113481603A (en) * | 2021-08-02 | 2021-10-08 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of PVT method silicon carbide crystal growth raw material |
| CN113479888A (en) * | 2021-06-01 | 2021-10-08 | 中科汇通(内蒙古)投资控股有限公司 | Core-shell structure powder for SiC single crystal growth and preparation process thereof |
| CN115261977A (en) * | 2022-08-04 | 2022-11-01 | 福建北电新材料科技有限公司 | Silicon carbide pretreatment method and device |
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| CN113479888A (en) * | 2021-06-01 | 2021-10-08 | 中科汇通(内蒙古)投资控股有限公司 | Core-shell structure powder for SiC single crystal growth and preparation process thereof |
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Application publication date: 20210115 |