CN113479888A - Core-shell structure powder for SiC single crystal growth and preparation process thereof - Google Patents
Core-shell structure powder for SiC single crystal growth and preparation process thereof Download PDFInfo
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Abstract
The invention provides core-shell structure powder for SiC single crystal growth and a preparation process thereof. The powder material comprises a core, an intermediate layer and a shell, wherein the core is SiC-Si mixed powder of large-particle-size Si particles and small-particle-size SiC particles, the intermediate layer is large-particle-size SiC powder, the shell is carbon-rich SiC powder, and the carbon-rich SiC powder of the shell is obtained by heating the SiC powder in a graphite crucible at 2000-2400 ℃. When the silicon carbide single crystal is prepared by adopting a physical vapor transport method, the core-shell structure powder can realize effective isolation of silicon carbide particles of different powders, and can realize reasonable adjustment of carbon and silicon components in different heating sublimation stages, so that the problems of sintering and uneven heating in the heating sublimation process of the existing silicon carbide powder are effectively solved, and finally, the silicon carbide single crystal with high quality can be obtained.
Description
Technical Field
The invention relates to SiC powder for growing silicon carbide single crystals, in particular to core-shell structure powder for growing SiC single crystals and a preparation process thereof.
Background
Silicon carbide is a typical representative of third-generation semiconductors, and is widely used in the fields of power electronics, radio frequency devices, optoelectronic devices, and the like. The method for growing the silicon carbide single crystal by adopting a physical vapor transport method (PVT method) is one of the most promising preparation methods at present, and the silicon carbide single crystal grows on the surface of a seed crystal under the action of temperature gradient and concentration gradient by heating and sublimating silicon carbide powder in a graphite crucible.
In the process of growing silicon carbide single crystals by the PVT method, the properties of silicon carbide powder in a graphite crucible are key factors influencing the growth quality and efficiency of the silicon carbide powder. Generally, the granularity of the silicon carbide powder is in the micron level, the powder is in close contact, heat conduction of the powder is facilitated, the powder at different positions in the graphite crucible can be heated quickly and uniformly, and good heating effect and sublimation effect are achieved; however, the sublimation temperature of the silicon carbide powder is up to more than 2000 ℃, and in the heating process of keeping such high temperature for a long time, the powder may have a phenomenon of large-area sintering, on one hand, the gas transmission channel is obstructed, which is not beneficial to conveying the sublimed gas to the growth chamber, on the other hand, the heating uniformity and sublimation condition inside the silicon carbide powder can be influenced, and further, the proportion of carbon and silicon in the sublimed gas is influenced, which can bring adverse effects to the growth of the silicon carbide single crystal. In addition, the prior sublimation of silicon causes the problems of carbon enrichment and silicon depletion of the silicon carbide powder in the middle and later growth stages, and further influences the growth of the silicon carbide single crystal.
Therefore, for the growth of the silicon carbide single crystal, the silicon carbide powder with a specific structure is prepared, so that the silicon carbide powder does not undergo powder sintering in the heating process, can be normally sublimated and smoothly output, can realize a certain regulation effect on the components of the silicon carbide powder, and has very important value.
Disclosure of Invention
The invention provides a core-shell structure powder for SiC single crystal growth and a preparation process thereof, aiming at the problems of sintering, uneven heating, carbon-rich tendency of powder in the middle and later periods and the like in the heating sublimation process of the existing silicon carbide powder.
In order to achieve the purpose, the invention provides core-shell structure powder for SiC single crystal growth, which adopts the following main technical scheme:
the powder material comprises a core, an intermediate layer and a shell, wherein the core is SiC-Si mixed powder of large-particle-size Si particles and small-particle-size SiC particles, the intermediate layer is large-particle-size SiC powder, the shell is carbon-rich SiC powder, and the carbon-rich SiC powder of the shell is obtained by heating the SiC powder in a graphite crucible at 2000-2400 ℃.
The technical scheme of the invention also comprises the following subsidiary schemes:
the large-particle-size Si particles are spherical, the purity of the silicon powder is not lower than 99.999%, and the particle size of the silicon powder is not lower than 50 microns; the grain size of the small-grain SiC grains is not more than 1 micron; the grain size of the large-grain SiC powder of the middle layer is not less than 10 microns; the particle size of the carbon-rich SiC powder does not exceed 50 microns.
Calculated by mass percentage, the ratio of the Si particles to the SiC particles in the powder core is 3: 1-5: 1.
the coverage area ratio of the powder shell to the powder core is 50-90%. The proportion not only realizes the isolation of the silicon carbide powder of the middle layer and other silicon carbide powder, but also leaves a certain space or gap, and is convenient for the sublimed gas component to be conveyed in time.
The surface coverage ratio of SiC particles to Si particles in the SiC-Si mixed powder is not less than 80%. The setting of the coverage ratio can ensure good bonding to the intermediate layer silicon carbide powder.
The thickness of the intermediate layer is not less than 100 microns, and the silicon carbide powder of the intermediate layer is the main part for sublimation in the initial growth stage of the silicon carbide single crystal.
The invention also provides a preparation process of the core-shell structure powder for SiC single crystal growth, which comprises the following steps:
(1) preparation of carbon-rich SiC powder: heating SiC powder with the particle size not more than 50 micrometers in a graphite crucible at 2000-2400 ℃ to obtain carbon-rich SiC powder;
(2) preparing a powder core: mechanically mixing large-particle-size Si particles with the particle size not less than 50 micrometers and small-particle-size SiC particles with the particle size not more than 1 micrometer to obtain SiC-Si mixed powder, and heating the SiC-Si mixed powder at the temperature not more than 1000 ℃ for not more than 1 hour to ensure that the particles in the SiC-Si mixed powder are locally melted to generate good combination, thereby forming a powder core;
(3) preparing a powder intermediate layer: mechanically mixing the powder core obtained in the second step with large-particle-size high-purity SiC powder with the particle size of not less than 10 microns; heating the obtained mixed powder at the temperature of not more than 1000 ℃, and then naturally cooling to finish the preparation of the powder intermediate layer;
(4) preparing a powder shell: c, paving the carbon-rich SiC powder obtained in the first step on the surface to form a pre-laid layer, then covering the powder obtained in the third step on the paved pre-laid layer to form a main powder layer, and finally paving the carbon-rich SiC powder on the main powder layer again to obtain a composite layer; heating the obtained composite layer at the temperature of not more than 1000 ℃, and then naturally cooling to finish the preparation of the powder shell;
(5) shaping powder: and (3) shaping the powder shell obtained in the last step in a vibrating screen, and removing the carbon-rich SiC powder loosely bonded on the surface of the powder to obtain the core-shell structure powder for SiC single crystal growth.
And in the heating preparation process, the carbon-rich SiC powder is protected by inert gas.
The thickness of the powder shell is not less than 100 microns.
Pores are present between the carbon-rich SiC powder on the surface of the shell.
When the silicon carbide single crystal is prepared by adopting a physical vapor transport method, the powder is directly used for growing the silicon carbide single crystal, or the powder is added into the conventional silicon carbide powder according to the mass percentage of not less than 30% and is uniformly mixed for use.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) in the technical scheme, the core-interlayer-shell structure is adopted, so that the performances of different positions of the silicon carbide powder are effectively divided and cooperated, and the silicon carbide powder with a special structure and suitable for growing silicon carbide single crystals by a PVT method is obtained. The core is SiC-Si mixed powder, the core is designed into large-diameter Si particles, and the core is positioned in the center and blocked by the intermediate layer in the heating and sublimation process, so that silicon in the core at the initial growth stage of the silicon carbide single crystal is difficult to effectively convey after sublimation, and the sublimated silicon can be emitted from the powder later. And in the middle and later growth stages, the silicon at the core can be effectively conveyed to the growth atmosphere to realize the supplement of silicon components, so that the silicon carbide powder in the middle layer does not have the tendency of graphitization due to preferential sublimation of the silicon. Meanwhile, the small-particle-size SiC particles coat the large-particle-size Si particles, and the large-particle-size Si particles and the SiC powder in the middle layer are well combined under the action of the transition layer. In addition, the silicon sublimation in the core needs to pass through the intermediate layer and the outer shell layer to enter into the growth atmosphere, and secondary heating can be realized to the intermediate layer and the outer pit in the gas conveying process, so that the sublimation of carbon-containing components is accelerated, and the carbon-silicon ratio in the growth atmosphere is adjusted to be within a reasonable range. The shell adopts the carborundum powder of rich carbon, and its aim at, on the one hand can well combine with the SiC powder of intermediate level, and on the other hand, its itself can appear graphitized thin layer on the top layer after high temperature heating to effectively realize the isolation between the carborundum powder, avoid the appearance of sintering phenomenon.
(2) In the aspect of powder preparation process, the advantages of the invention are reflected in two aspects. Firstly, the high-temperature heating required by the growth of the silicon carbide single crystal is directly adopted to obtain the carbon-rich silicon carbide powder as the shell of the powder, on one hand, the good adhesion with the silicon carbide in the middle layer can be realized, and on the other hand, the secondary utilization of the silicon carbide powder can also be realized by using part of used silicon carbide powder. Secondly, the preparation process adopts short-time heating at the temperature of not more than 1000 ℃, so that limited fusion bonding at local contact points among the powder can be obtained, obvious sintering can not occur, the core-shell structure powder is favorably formed, and the core-shell structure powder has excellent effect in practical application.
Detailed Description
The technical scheme of the invention is explained in detail by combining specific embodiments.
The core-shell structure powder for SiC single crystal growth comprises a core, an intermediate layer and a shell, wherein the core is SiC-Si mixed powder of large-particle-size Si particles and small-particle-size SiC particles, the intermediate layer is large-particle-size SiC powder, the shell is carbon-rich SiC powder, and the carbon-rich SiC powder of the shell is obtained by heating the SiC powder in a graphite crucible at 2000-2400 ℃.
The powder material is used in the preparation of the silicon carbide single crystal by the PVT method, and the core, the middle layer and the shell structure of the powder material fully utilize the components and the structures of different layers of powder, so that the sintering phenomenon can be avoided in the powder material at the initial growth stage and the middle and later growth stages, the heating uniformity is improved, and the proportion of carbon and silicon is effectively adjusted to be within a reasonable range.
The large-particle-size Si particles are spherical, the purity of the silicon powder is not lower than 99.999%, and the particle size of the silicon powder is not lower than 50 microns; the grain size of the small-grain SiC grains is not more than 1 micron; the grain size of the large-grain SiC powder of the middle layer is not less than 10 microns; the particle size of the carbon-rich SiC powder does not exceed 50 microns. The SiC particles with small particle size are easy to adhere and cover the Si particles with large particle size.
Calculated by mass percentage, the ratio of the Si particles to the SiC particles in the powder core is 3: 1-5: 1.
the coverage area ratio of the powder shell to the powder core is 50-90%. The determination of the proportion can effectively isolate different powder particles by the shells of the powder particles, avoid the sintering of silicon carbide from generating blocks with larger areas, and specially reserve a certain uncovered proportion on the other hand, thereby further providing a smooth gas conveying channel on the basis of a gas conveying pore channel in the carbon-rich SiC powder and being beneficial to the gas conveying of the middle layer.
The surface coverage ratio of SiC particles to Si particles in the SiC-Si mixed powder is not less than 80%. The ratio is a result of comprehensive consideration on the basis of the particle diameters and the coverage ratio of Si and SiC particles, and gives consideration to both the effective coverage of Si particles and the bonding effect to the intermediate layer powder.
The thickness of the intermediate layer is not less than 100 microns. The silicon carbide powder of the intermediate layer is a main body part of the powder sublimed in the early growth stage, and the thickness of the silicon carbide powder needs to be ensured.
A preparation process of core-shell structure powder for SiC single crystal growth comprises the following steps:
(1) preparation of carbon-rich SiC powder: the method comprises the following steps of heating SiC powder with the particle size not more than 50 microns at 2000-2400 ℃ in a graphite crucible to obtain carbon-rich SiC powder, wherein the heating time can be determined according to the actual amount and specific temperature of the SiC powder, and the phenomenon that the SiC powder is obviously carbon-rich is taken as the standard; the powder particle size is defined by the median particle size of the powder, preferably, the median particle size of the SiC powder used to prepare the carbon-rich SiC powder is selected to be 45 microns, 40 microns, 30 microns, 20 microns or 10 microns;
(2) preparing a powder core: mixing large-particle-size Si particles and small-particle-size SiC particles by using a ball mill, mechanically mixing the large-particle-size Si particles with the particle size not less than 50 micrometers and the small-particle-size SiC particles with the particle size not more than 1 micrometer to obtain SiC-Si mixed powder, and heating the SiC-Si mixed powder at the temperature not more than 1000 ℃ for not more than 1 hour to ensure that local contact points among the particles in the SiC-Si mixed powder are fused to generate good combination, thereby forming a powder core; preferably, the large-size Si particles have a median particle size of 60 microns or 70 microns or 80 microns or 100 microns or 300 microns or 500 microns; preferably, the small particle size SiC particles have a median particle size of 0.8 microns or 0.7 microns or 0.6 microns or 0.5 microns or 0.4 microns or 0.3 microns or 0.2 microns or 0.1 microns or 0.07 microns or 0.05 microns or 0.03 microns;
(3) preparing a powder intermediate layer: mechanically mixing the powder core obtained in the second step with large-particle-size high-purity SiC powder with the particle size of not less than 10 microns; heating the obtained mixed powder for less than 1 hour at the temperature of not more than 1000 ℃, then naturally cooling, and adopting inert gas for protection in the cooling process to finish the preparation of the powder intermediate layer; preferably, the large-particle-size high-purity SiC powder has a median particle size of 300 microns or 100 microns or 80 microns or 50 microns or 30 microns or 20 microns or 15 microns;
(4) preparing a powder shell: c, paving the carbon-rich SiC powder obtained in the first step on the surface to form a pre-laid layer, then covering the powder obtained in the third step on the pre-laid layer to form a main powder layer, and finally paving the carbon-rich SiC powder on the main powder layer again to obtain a composite layer; heating the obtained composite layer for less than 1 hour at the temperature of not more than 1000 ℃, and then naturally cooling to finish the preparation of the powder shell; in the powder spreading process, the layer number and the thickness of the powder can be accurately controlled by adopting mechanical adjustment of powder sieving force, times and the like;
(5) shaping powder: and (3) shaping the powder shell obtained in the last step in a vibrating screen, and removing the carbon-rich SiC powder loosely bonded on the surface of the powder by using the vibration of the vibrating screen to obtain the core-shell structure powder for the SiC single crystal growth by the PVT method.
And in the heating preparation process, the carbon-rich SiC powder is protected by inert gas.
Heating in steps (2) - (4) in a high-purity graphite crucible at a temperature not higher than 1000 deg.C, introducing argon gas for protection to prevent oxidation, and keeping the pressure at 1 × 104 Pa~1×105Pa, the time is controlled within 1 hour, the time is adjusted according to the granularity of the powder, and the heating time which is a little longer can be selected for the large-diameter powder. By heating at a higher temperature for a short time, local adhesive bonds are formed at the contact points of the powder particles of different powder layers, the adhesive bond strength is higher than that of physical adsorption when the powder particles are not heated, but the sintering phenomenon is far from occurring.
During the heating process of steps (1) - (4), the powder is loosely laid in a single layer or thin layer, so as to ensure sufficient contact and coating between different powders.
The thickness of the powder casing is not less than 100 microns to ensure effective isolation between different powder particles.
Pores exist among the carbon-rich SiC powder on the surface of the shell, on one hand, the pores are conveying gaps caused by preferential sublimation of Si components in the high-temperature heating process of the original silicon carbide powder, and on the other hand, larger pore channels for gas conveying are reserved due to the specially controlled coverage ratio.
When the silicon carbide single crystal is prepared by adopting a physical vapor transport method, the powder is directly used for growing the silicon carbide single crystal, or the powder is added into the conventional silicon carbide powder according to the mass percentage of not less than 30% and is uniformly mixed for use. In the process of preparing the silicon carbide single crystal selected powder by the PVT method, parameters such as heating temperature, speed and the like, particularly temperature gradient and concentration gradient in a growth chamber can be combined to adjust the powder with different adding proportions.
The core-shell structure design provided by the invention particularly utilizes the characteristic that silicon powder is easy to sublimate preferentially and the coating obstruction of silicon carbide on the outer layer by the combination of the central large-particle-size silicon powder and the small-particle-size silicon carbide powder, and fully exerts the characteristics of different layers of powder. The Si particles at the core are blocked by the intermediate layer because the Si particles are positioned at the core part in the heating and sublimation process of the silicon carbide powder, so that the sublimated silicon can be diffused from the powder in the middle and later growth stages. The silicon component of the silicon carbide powder in the middle layer is supplemented, so that the silicon carbide powder in the middle layer does not have the graphitization tendency caused by the preferential sublimation of silicon. In addition, the silicon sublimation process of core department needs to pass through intermediate level and shell layer, can realize the secondary heating to intermediate level and outer hole, helps accelerating the sublimation of carbonaceous component, and then adjusts the carbon-silicon ratio in the growth atmosphere and be in reasonable range. In the powder material, due to the existence of the Si particles with large core particle size, the carbon-silicon ratio of the silicon carbide powder material can be in a reasonable range in different growth stages, and the silicon carbide powder material is favorable for obtaining high-quality silicon carbide single crystals.
The embodiments of the present invention have been described above, but many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments, and the corresponding modifications and variations are within the scope of the invention.
Claims (10)
1. The core-shell structure powder for SiC single crystal growth is characterized by comprising a core, an intermediate layer and a shell, wherein the core is SiC-Si mixed powder of large-particle-size Si particles and small-particle-size SiC particles, the intermediate layer is large-particle-size SiC powder, the shell is carbon-rich SiC powder, and the carbon-rich SiC powder of the shell is obtained by heating the SiC powder in a graphite crucible at 2000-2400 ℃.
2. The core-shell structure powder for SiC single crystal growth according to claim 1, wherein the particle size of the large-particle size Si particles is not less than 50 μm; the grain size of the small-grain SiC grains is not more than 1 micron; the grain size of the large-grain SiC powder of the middle layer is not less than 10 microns; the particle size of the carbon-rich SiC powder does not exceed 50 microns.
3. The core-shell structure powder for SiC single crystal growth according to claim 1, wherein the ratio of Si particles to SiC particles in the core of the powder is 3: 1-5: 1.
4. the core-shell structure powder for SiC single crystal growth according to claim 1, wherein the ratio of the coverage area of the powder shell to the powder core is 50-90%.
5. The core-shell structure powder for SiC single crystal growth according to claim 1, wherein a surface coverage ratio of SiC particles to Si particles in the SiC-Si mixed powder is not less than 80%.
6. The core-shell structure powder for SiC single crystal growth according to claim 1, wherein the thickness of the intermediate layer is not less than 100 μm.
7. The preparation process of the core-shell structure powder for SiC single crystal growth comprises the following steps:
(1) preparation of carbon-rich SiC powder: heating SiC powder with the particle size not more than 50 micrometers in a graphite crucible at 2000-2400 ℃ to obtain carbon-rich SiC powder;
(2) preparing a powder core: mechanically mixing large-particle-size Si particles with the particle size not less than 50 micrometers and small-particle-size SiC particles with the particle size not more than 1 micrometer to obtain SiC-Si mixed powder, and heating the SiC-Si mixed powder at the temperature not more than 1000 ℃ for not more than 1 hour to ensure that the particles in the SiC-Si mixed powder are locally melted to generate good combination;
(3) preparing a powder intermediate layer: mechanically mixing the powder core obtained in the second step with large-particle-size high-purity SiC powder with the particle size not less than 10 microns, heating at the temperature not more than 1000 ℃, and naturally cooling;
(4) preparing a powder shell: c, paving the carbon-rich SiC powder obtained in the first step on the surface to form a pre-laid layer, then covering the powder obtained in the third step on the paved pre-laid layer to form a main powder layer, and finally paving the carbon-rich SiC powder on the main powder layer again to obtain a composite layer; heating the obtained composite layer at the temperature of not more than 1000 ℃ and then naturally cooling;
(5) shaping powder: and (3) shaping the powder obtained in the last step in a vibrating screen, and removing the carbon-rich SiC powder loosely bonded on the surface of the powder.
8. The process for preparing core-shell structure powder for SiC single crystal growth according to claim 7, wherein the carbon-rich SiC powder is protected with an inert gas during the heating preparation.
9. The process for preparing core-shell structure powder for SiC single crystal growth according to claim 7, wherein the thickness of the powder shell is not less than 100 μm.
10. The process for preparing core-shell structure powder for SiC single crystal growth according to claim 7, wherein when the silicon carbide single crystal is prepared by a physical vapor transport method, the powder is directly used for the growth of the silicon carbide single crystal, or the powder is added to conventional silicon carbide powder in a proportion of not less than 30% by mass and is uniformly mixed for use.
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