CN112481699A - Preparation method of high-quality silicon carbide single crystal and silicon carbide single crystal - Google Patents
Preparation method of high-quality silicon carbide single crystal and silicon carbide single crystal Download PDFInfo
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- CN112481699A CN112481699A CN202011255128.4A CN202011255128A CN112481699A CN 112481699 A CN112481699 A CN 112481699A CN 202011255128 A CN202011255128 A CN 202011255128A CN 112481699 A CN112481699 A CN 112481699A
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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
The application provides a preparation method of a high-quality silicon carbide single crystal, which comprises the following steps: providing a crystal growth raw material into a crucible, and heating the crystal growth raw material to prepare a silicon carbide single crystal; the crystal growth raw material comprises a first silicon carbide powder layer, a carbon powder layer and a second silicon carbide powder layer which are sequentially paved from the bottom of the crucible upwards. The application provides a preparation method of high-quality carborundum single crystal, through the specific position in the long brilliant raw materials of carborundum add the carbon powder layer of certain thickness for the rich silicon atmosphere who sublimes from the crucible bottom fully reacts with the carbon particle in the carbon powder layer when the carbon powder layer, and then effectively alleviate the erosion to graphite crucible, prolong graphite crucible's life, reduce in the crystal polytype, the production of microtubule defect, and can also avoid the carbon particle to rise along with the air current, show the carbon inclusion in the reduction crystal, obtain high-quality carborundum single crystal.
Description
Technical Field
The application relates to the technical field of preparation of crystal materials, in particular to a preparation method of a high-quality silicon carbide single crystal and the silicon carbide single crystal.
Background
In the prior art, when the PVT method is used for preparing the silicon carbide single crystal, a silicon carbide seed crystal is usually fixed at the top in a graphite crucible, and a silicon carbide powder is used as a crystal growth raw materialPlaced inside a graphite crucible. The essence of the PVT method lies in the decomposition of silicon carbide powder, the gas phase component of which is mainly Si, Si2C and SiC2。
Therefore, the gas phase obtained after the silicon carbide powder is thermally decomposed is a silicon-rich gas phase, i.e., the partial pressure of the silicon atmosphere in the crucible is too high in the early stage of crystal growth, and the too high silicon atmosphere reacts with carbon in the graphite crucible to generate the gas phase. In the reaction process, on one hand, the graphite crucible is seriously corroded, so that the use frequency of the graphite crucible is limited, the inner wall of the crucible is sunken after being corroded, the shape of the crucible changes, a temperature field is changed, the change of the temperature field also influences the growth of crystals, and the defects of polytype and tube are easily caused; on the other hand, can produce a large amount of carbon particles in crystal growth's earlier stage and transmit to the growth surface, cause earlier stage carbon inclusion, in crystal growth's later stage, the carborundum raw materials of crucible bottom is because the silicon sublimation is too fast and the carbonization is serious, and the carborundum material after the carbonization easily transmits to the growth face along with the atmosphere, causes later stage carbon inclusion.
In the prior art, the generation of carbon inclusions is reduced by improving a crucible structure or supplementing a silicon atmosphere in a preparation process, so that the quality of the silicon carbide crystal is improved.
Disclosure of Invention
In order to solve the above problems, the present application aims to provide a method for preparing a high quality silicon carbide crystal, which can effectively reduce erosion of raw materials to the wall of a graphite crucible in the preparation process, and can also significantly reduce carbon inclusion defects in the silicon carbide crystal, the method comprising:
providing a crystal growth raw material into a crucible, and heating the crystal growth raw material to prepare a silicon carbide single crystal;
the crystal growth raw material comprises a first silicon carbide powder layer, a carbon powder layer and a second silicon carbide powder layer which are sequentially paved from the bottom of the crucible upwards.
The method for preparing the silicon carbide single crystal provided by the application comprises the step of charging silicon carbide powderThe carbon powder layer is added into the material, because the temperature of the crucible wall and the crucible bottom is highest, the silicon carbide powder nearby is most easy to sublimate, and the carbon powder layer is arranged to ensure that the silicon-rich atmosphere (such as containing Si, SiC and Si) sublimates from the crucible bottom2The gas phase of the C gas) fully reacts with carbon particles in the carbon powder layer when passing through the carbon powder layer, so that the corrosion to the graphite crucible is effectively reduced, and the service life of the graphite crucible is prolonged; and, the top on carbon powder bed still is provided with second carborundum powder, can effectively prevent the carbon particle in the carbon powder layer, and the carbon particle that the carborundum powder produced of long brilliant later stage rises along with sublimed air current and transmits to the growth surface and form the carbon inclusion, and the second carborundum powder on upper strata has played fine filter action promptly.
In addition, unstable Si/C ratio in the gas phase is liable to cause polytype defects, thereby increasing the number of micropipe defects. Compared with the existing distribution mode of only laying silicon carbide powder, on one hand, the corrosion to the graphite crucible is reduced, and the temperature field change caused by thinning the crucible wall can be avoided, so that the defects of polytype and microtubule in the crystal are reduced; on the other hand, the carbon-silicon ratio is properly increased by the material distribution mode, so that the supersaturation degree of the atmosphere in the gas phase is further maintained at a higher level, the growth of a 4H silicon carbide crystal form is facilitated, the occurrence of polytype is further avoided, and the number of micro-tubes is obviously reduced.
Alternatively, the above method may use an existing thermal field structure for charging and preparing a silicon carbide single crystal, such as a crystal growth furnace in which a graphite crucible is disposed, and a heating element, such as a graphite heater or an intermediate frequency induction heater, is disposed outside the graphite crucible, and a silicon carbide seed crystal is further fixed to the top of the inside of a crucible cover of the graphite crucible.
Further, the carbon powder layer is formed by laying carbon powder particles, and the particle size of the carbon powder particles is 150-300 meshes.
The proper particle size of the carbon powder particles in the carbon powder layer can not only ensure the full reaction with the sublimed atmosphere, but also accelerate the growth rate of the crystal. For example, when the particle size of the carbon powder particles is too small, the atmosphere channel in the carbon powder layer is too small, so that the atmosphere is prevented from rising, the atmosphere is retained in the powder, and the growth rate of the silicon carbide crystal is influenced; when the particle size of the carbon powder particles is too large, the atmosphere channel in the carbon powder layer is too large, and the atmosphere cannot fully react with the carbon powder particles after rising to the carbon powder layer.
Meanwhile, the carbon powder layer made of the carbon powder particles with the particle size and the mesh number is adopted, and the formed pores are the minimum limit of the necessary pores for the crystal growth of the silicon carbide, so that the consumed pores can not be obviously expanded in the crystal growth process although the carbon particles in the carbon powder layer are consumed by reaction.
Further, the distance between the top surface of the carbon powder layer and the top charge surface of the crystal growth raw material accounts for (1/10) - (3/10) of the total thickness of the crystal growth raw material. Preferably, the distance is (1.5/10) - (2/10) of the total thickness of the crystal growth raw material, and more preferably 1/5.
In one embodiment, the distance between the top surface of the carbon powder layer and the top charge surface of the crystal growth raw material is the thickness of the second silicon carbide powder. In the mode of feeding that this application provided, all react rather than through the carbon powder layer in order to make the carborundum powder as far as possible, consequently set up the carbon powder layer at the top that is close to long brilliant raw materials to when setting up in above-mentioned distance department, can also avoid long brilliant later stage carborundum raw materials produced carbon particle along with sublimed air current rise, avoid forming the carbon inclusion.
Further, the spreading thickness ratio of the carbon powder layer to the first silicon carbide powder layer is (5-20): (55-85).
In one embodiment, the thickness of the first silicon carbide powder layer is 60 to 80mm, and the thickness of the carbon powder layer is about 5 to 20 mm.
Furthermore, the particle size of the silicon carbide powder of the first silicon carbide powder layer is 200-1000 microns, preferably 300-800 microns, and more preferably 500 microns.
Furthermore, the particle size of the silicon carbide powder of the second silicon carbide powder layer is 200-1000 microns, preferably 300-800 microns, and more preferably 500 microns.
In a preferred embodiment, the first silicon carbide powder layer located below the carbon powder layer and the second silicon carbide powder layer located above the carbon powder layer use silicon carbide powders of the same particle size, i.e. the same silicon carbide powder. In another embodiment, the first silicon carbide powder layer and the second silicon carbide powder layer may be made of powder materials with different particle sizes, and in this case, the particle size of the second silicon carbide powder layer is preferably smaller than that of the first silicon carbide powder layer, and more preferably, the particle size of the second silicon carbide powder layer is the same as that of the carbon powder layer, so as to better perform the filtering function.
Further, the crucible is a graphite crucible.
Further, the method comprises a step of heating the crystal growth raw material by using a PVT method to carry out crystal growth so as to obtain the silicon carbide single crystal.
Further, the step of heating the crystal growth raw material by using the PVT method to perform crystal growth specifically comprises: and carrying out crystal growth for 80-120 h under the conditions that the pressure in the crystal growth furnace is 8-10 mbar and the temperature is 2200-2400 ℃. Preferably, the crystal is grown for 100 hours under the conditions that the furnace body pressure of the crystal growth furnace is 10mbar and the temperature is 2300 ℃.
On the other hand, the application also provides a silicon carbide single crystal prepared by the preparation method.
The following beneficial effects can be brought through the application:
the application provides a preparation method of high-quality carborundum single crystal, through the specific position in the long brilliant raw materials of carborundum add the carbon powder layer of certain thickness for the rich silicon atmosphere who sublimes from the crucible bottom fully reacts with the carbon particle in the carbon powder layer when the carbon powder layer, and then effectively alleviate the erosion to graphite crucible, prolong graphite crucible's life, reduce in the crystal polytype, the production of microtubule defect, and can also avoid the carbon particle to rise along with the air current, show the carbon inclusion in the reduction crystal, obtain high-quality carborundum single crystal.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a schematic view of the material distribution manner of the charging step in the preparation method provided by the present application;
FIG. 2 is a view under a microscope of a sliced silicon carbide single crystal obtained by the production method of example 1;
FIG. 3 is an enlarged view of a portion of the wafer shown in FIG. 2, at a magnification of 200;
FIG. 4 is a view under a microscope of a single crystal silicon carbide wafer obtained by the production method of comparative example 1;
FIG. 5 is an enlarged partial view of the wafer of FIG. 4, at a magnification of 200; (ii) a
In the figure: 1. a graphite crucible; 2. a silicon carbide powder layer; 3. a carbon powder layer; 4. silicon carbide seed crystals; 5. and (4) covering the crucible.
Detailed Description
In order to more clearly explain the overall concept of the present application, the following detailed description of the overall scheme of the present invention is made by way of example. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
Unless otherwise specified, each raw material powder in the following examples is commercially available.
The preparation method provided by the application can be prepared by adopting a crystal growth furnace as shown in figure 1. Wherein the crystal growth furnace is provided with a graphite crucible 1, and a heating element such as a graphite heater or a medium frequency induction heater for heating the crystal growth raw material can be further provided outside the graphite crucible 1, which is not shown in the figure. An upper crucible cover 5 is arranged at the top of the graphite crucible 1, and a silicon carbide seed crystal 4 is also fixed at the top of the inner side of the upper crucible cover 5.
The following examples are all distributed as shown in fig. 1, that is, in the graphite crucible 1, a first silicon carbide powder layer, a carbon powder layer 3 and a second silicon carbide powder layer are sequentially laid from bottom to top, and preferably, the same silicon carbide powder 2 can be used for the first silicon carbide powder layer and the second silicon carbide powder layer.
Example 1
The present embodiment provides a method for producing a high-quality silicon carbide single crystal, including the steps of:
step one, charging: putting about 3000g of crystal growth raw material into a graphite crucible, wherein a layer of silicon carbide powder with the mass of about 2211g and the granularity of 500 microns is paved at the bottom of the graphite crucible, and the paving height is about 70 mm; then, carbon powder particles with the mass of 158g and the granularity of 200 meshes are flatly paved on the silicon carbide powder to prepare a carbon powder layer, and the thickness of the carbon powder layer is about 10 mm; finally, about 631g of silicon carbide powder with the same granularity as that of the silicon carbide powder below the carbon powder layer is paved above the carbon powder layer, and the paving thickness is about 20 mm;
step two, after the charging is finished, covering the crucible upper cover with the silicon carbide seed crystal fixed on the inner side of the crucible upper cover on the crucible opening of the graphite crucible, enabling the silicon carbide seed crystal to be placed on the top charge level of the crystal growth raw material for about 100mm, and assembling the crystal growth furnace;
step three, heating and crystal growth: heating the crystal growth raw material by using a PVT method to grow crystals, controlling the furnace body pressure of a crystal growth furnace to be 10mbar, controlling the temperature to be 2300 ℃, and controlling the total growth time to be 100 h;
and step four, cooling after crystal growth is finished, and opening the crystal growth furnace to obtain the silicon carbide crystal with the weight of about 1500 g.
Example 2
The present embodiment provides a method for producing a high-quality silicon carbide single crystal, including the steps of:
step one, charging: placing 3066g of crystal growth raw material in a graphite crucible, wherein a layer of silicon carbide powder with the mass of about 2153g and the granularity of 300 microns is paved at the bottom of the graphite crucible, and the paving height is about 65 mm; then carbon powder particles with the mass of 251g and the granularity of 300 meshes are flatly paved on the silicon carbide powder to prepare a carbon powder layer with the thickness of 15 mm; finally, laying 662g of silicon carbide powder with the same granularity as that of the silicon carbide powder below the carbon powder layer above the carbon powder layer, wherein the laying thickness is about 20 mm;
step two, after the charging is finished, covering the crucible upper cover with the silicon carbide seed crystal fixed on the inner side of the crucible upper cover on the crucible opening of the graphite crucible, enabling the silicon carbide seed crystal to be placed on the top charge level of the crystal growth raw material for about 100mm, and assembling the crystal growth furnace;
step three, heating and crystal growth: heating the crystal growth raw material by using a PVT method to grow crystals, controlling the furnace body pressure of a crystal growth furnace to be 10mbar, controlling the temperature to be 2300 ℃, and controlling the total growth time to be 100 h;
and step four, cooling after crystal growth is finished, and opening the crystal growth furnace to obtain the silicon carbide crystal with the weight of 1550 g.
Example 3
The present embodiment provides a method for producing a high-quality silicon carbide single crystal, including the steps of:
step one, charging: placing 2835g of crystal growth raw material into a graphite crucible, wherein a layer of silicon carbide powder with the mass of 2272g and the granularity of 800 microns is paved at the bottom of the graphite crucible, and the paving height is about 77 mm; then carbon powder particles with the mass of about 120g and the granularity of 150 meshes are flatly paved on the silicon carbide powder to prepare a carbon powder layer with the thickness of about 8 mm; finally, 443g of silicon carbide powder with the same granularity as that of the silicon carbide powder below the carbon powder layer is paved above the carbon powder layer, and the paving thickness is 15 mm;
step two, after the charging is finished, covering the crucible upper cover with the silicon carbide seed crystal fixed on the inner side of the crucible upper cover on the crucible opening of the graphite crucible, enabling the silicon carbide seed crystal to be placed on the top charge level of the crystal growth raw material for about 100mm, and assembling the crystal growth furnace;
step three, heating and crystal growth: heating the crystal growth raw material by using a PVT method to grow crystals, controlling the furnace body pressure of a crystal growth furnace to be 10mbar, controlling the temperature to be 2300 ℃, and controlling the total growth time to be 100 h;
and step four, cooling after crystal growth is finished, and opening the crystal growth furnace to obtain the silicon carbide crystal with the weight of 1550 g.
Examples 4 to 5
Examples 4 to 5 were substantially the same as example 1 in terms of the material distribution method and the preparation method, except that the carbon powder particles in the carbon powder layer were 100 mesh and 400 mesh, respectively, and the remaining steps and parameters were the same.
Examples 6 to 7
Examples 6 to 7 are substantially the same as example 1 in the material distribution manner and the preparation method, except that under the condition that the total thickness of the crystal growth raw material is 100mm, the thicknesses of the second silicon carbide powder layer located above the carbon powder layer are 8mm and 40mm, respectively, and the thickness of the second silicon carbide powder layer can be understood as the distance from the carbon powder layer to the top material surface of the crystal growth raw material.
Comparative example 1
Comparative example 1 charging was carried out by the conventional batch method, i.e., by charging a pure silicon carbide powder having a mass of 3000g and a particle size of 500 μm into the same graphite crucible, and the remaining process parameters, such as temperature, pressure and time for heating for crystal growth, were the same as those of example 1.
The silicon carbide single crystal obtained by the above-described preparation method of each example was subjected to characterization of quality defects such as carbon inclusion, micropipe, polytype, and the like, and the graphite crucible was weighed before and after preparation, respectively, to measure the amount of loss of the graphite crucible, and the results are shown in table 1, wherein the characterization graphs obtained by microscopic observation after slicing example 1 and comparative example 1 are shown in fig. 2 and fig. 3.
TABLE 1
As can be seen from the data in table 1 and the results observed in fig. 2 to 5, compared with comparative example 1 in which only silicon carbide powder is used, the preparation method provided in the embodiments of the present application can significantly reduce or even eliminate the quality defects of carbon inclusions, micropipes and polytypes in a single crystal, and effectively reduce the loss amount of the graphite crucible, and the particle size of the carbon powder particles in the carbon powder layer and the laying position of the carbon powder layer in the silicon carbide powder have a certain effect on further improving the quality of the silicon carbide crystal. Meanwhile, when the silicon carbide crystals obtained in comparative example 1 and comparative example 1 were observed, respectively, it was found that the silicon carbide crystals obtained in example 1 were high in transparency, had no significant micropipes and no significant granular inclusions in the wafers, while the crystals obtained in comparative example 1 had very significant granular inclusions inside and had dispersed micropipes penetrating the inside of the crystals. Therefore, the method provided by the application can reduce the erosion of the gas relative to the graphite crucible in the crystal growth process, further maintain the stability of the temperature field, reduce the rising of the carbon inclusion along with the gas flow, and prepare the high-quality silicon carbide crystal.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A method for producing a high-quality silicon carbide single crystal, characterized by comprising:
providing a crystal growth raw material into a crucible, and heating the crystal growth raw material to prepare a silicon carbide single crystal;
the crystal growth raw material comprises a first silicon carbide powder layer, a carbon powder layer and a second silicon carbide powder layer which are sequentially paved from the bottom of the crucible upwards.
2. The preparation method according to claim 1, wherein the carbon powder layer is prepared by laying carbon powder particles, and the particle size of the carbon powder particles is 150-300 meshes.
3. The method according to claim 1, wherein a distance between a top charge level of the carbon powder layer and a top charge level of the growth raw material accounts for (1/10) - (3/10) of a total thickness of the growth raw material.
4. The preparation method according to claim 1, wherein the spreading thickness ratio of the carbon powder layer to the first silicon carbide powder layer is (5-20): (55-85).
5. The method according to claim 1, wherein the first silicon carbide powder layer has a silicon carbide powder particle size of 200 to 1000 μm.
6. The preparation method according to claim 1, wherein the silicon carbide powder particle size of the second silicon carbide powder layer is 200 to 1000 μm.
7. A production method according to claim 1, wherein the crucible is a graphite crucible.
8. The production method according to any one of claims 1 to 7, comprising a step of heating a growth raw material by a PVT method to perform growth to obtain a silicon carbide single crystal.
9. The preparation method according to claim 8, wherein the step of heating the crystal growth raw material by the PVT method to perform crystal growth is specifically as follows: and carrying out crystal growth for 80-120 h under the conditions that the pressure in the crystal growth furnace is 8-10 mbar and the temperature is 2200-2400 ℃.
10. A silicon carbide single crystal produced by the production method according to any one of claims 1 to 9.
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| CN114182348A (en) * | 2021-10-28 | 2022-03-15 | 江苏吉星新材料有限公司 | Preparation method of silicon carbide single crystal with reduced carbon coating |
| CN114182348B (en) * | 2021-10-28 | 2023-09-19 | 江苏吉星新材料有限公司 | Preparation method of silicon carbide single crystal with reduced carbon coating |
| CN115142133A (en) * | 2022-06-24 | 2022-10-04 | 江苏集芯半导体硅材料研究院有限公司 | Control system and control method for growth speed of silicon carbide crystal and crystal growth furnace |
| CN115261991A (en) * | 2022-07-08 | 2022-11-01 | 江苏芯恒惟业电子科技有限公司 | Method for reducing defect density of carbon inclusion in silicon carbide single crystal |
| CN117265664A (en) * | 2023-09-26 | 2023-12-22 | 江苏超芯星半导体有限公司 | Growth method of silicon carbide crystal and silicon carbide crystal |
| CN117265664B (en) * | 2023-09-26 | 2024-04-30 | 江苏超芯星半导体有限公司 | Growth method of silicon carbide crystal and silicon carbide crystal |
| CN117535788A (en) * | 2024-01-10 | 2024-02-09 | 乾晶半导体(衢州)有限公司 | Single crystal growth method |
| CN117535788B (en) * | 2024-01-10 | 2024-04-05 | 乾晶半导体(衢州)有限公司 | Single crystal growth method |
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