CN110592673A - High-quality large-size silicon carbide crystal growth method - Google Patents
High-quality large-size silicon carbide crystal growth method Download PDFInfo
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- CN110592673A CN110592673A CN201811534979.5A CN201811534979A CN110592673A CN 110592673 A CN110592673 A CN 110592673A CN 201811534979 A CN201811534979 A CN 201811534979A CN 110592673 A CN110592673 A CN 110592673A
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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
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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
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Abstract
The invention provides a high-quality large-size silicon carbide crystal growth method, and aims to improve the quality of a grown SiC crystal and eliminate the defect of a planar hexagonal cavity. The method comprises the following steps: and (2) placing the crucible filled with the silicon carbide raw material and the seed crystal in a single crystal growth furnace, wherein the quick pushing-up distance range of the crucible is 5-50mm, the crucible is far away from a high-temperature region, the crucible is slowly descended under the condition of certain temperature and pressure, the descending distance is consistent with the pushing-up distance of the crucible, then the silicon carbide raw material is sublimated and crystallized on the seed crystal under the condition of certain temperature and pressure, and the crystal is cooled to obtain the silicon carbide single crystal. The invention has the advantages that: in the initial stage of crystal growth, the seed crystal is far away from a high-temperature region, and the ablation of the seed crystal caused by high temperature is eliminated, so that the defect of a plane hexagonal cavity is eliminated; meanwhile, the full utilization of the SiC raw material is ensured, so that the high-quality large-size silicon carbide crystal is obtained.
Description
Technical Field
The invention belongs to the field of silicon carbide crystal growth, and particularly relates to a high-quality large-size silicon carbide crystal growth method.
Background
Silicon carbide as a third-generation semiconductor material has excellent physical and chemical properties and has wide application in the fields of high-end photoelectricity, high power, microwave radio frequency and the like.
The most mature and effective way to grow silicon carbide crystals is currently the physical vapor transport method (Journal of crystal growth 43 (1978) 209-212), which has the following basic principles: the silicon carbide raw material is placed in a crucible, a seed crystal is fixed on the top of an upper cover of the crucible, the raw material is sublimated at high temperature and low pressure, the sublimated gas is transported to the seed crystal by taking the temperature gradient provided by a crystal growth thermal field as power for mass transmission, and finally the gas is transported to the seed crystal for crystal growth. The temperature gradient in the thermal field includes an axial temperature gradient and a radial temperature gradient.
Various defects in the silicon carbide single crystal substrate are one of the factors that affect the main performance of various types of silicon carbide-based devices. Research shows that defect generation in the growth of silicon carbide single crystals has a close relationship with the state of the seed crystal. The state of the seed crystal includes defects of the seed crystal itself (e.g., micropipes, polytypes, dislocations, etc.), damage to the seed crystal processing process (e.g., scratches, etc.), and defects introduced at the early stage of growth. Aiming at the defects and processing damages of the seed crystal, a better method is provided for processing at present. However, no effective method is available for treating the defects in the early growth stage.
Generally, a growth interface of a silicon carbide crystal is a convex interface, the silicon carbide single crystal grows at a position with a seed crystal, and a spontaneously nucleated polycrystal grows at a seed-crystal-free position outside the seed crystal, so that the grown polycrystal at the edge of the crystal is ensured to invade into a single crystal area through the convex growth interface, and the single crystal area of the crystal cannot be reduced, and the size requirement is met. Thus, the temperature at the edge position of the seed crystal is significantly higher than the center position of the seed crystal. While silicon carbide seeds are typically 350 microns to 500 microns thick, too thick a seed can add significant cost to the production. Therefore, the temperature of the edge of the seed crystal is obviously higher than that of the central position of the seed crystal during the initial growth, and the ablation phenomenon of the edge area of the seed crystal can often occur, so that the quality of the grown crystal can not meet the requirement. As the diameter of the silicon carbide crystal becomes larger, the temperature difference between the edge and the center of the seed crystal becomes larger, so that the edge of the seed crystal is easier to be corroded by high temperature in the early growth stage, and the problem is more obvious.
In the actual crystal growth process, especially in the 6-inch single crystal growth process, ablation often occurs at the initial stage of seed crystal growth, then a large number of plane hexagonal cavity defects occur in the crystal growth, and even the edge position of the seed crystal is burnt through to grow into polycrystal, so that the overall quality of the crystal is reduced. Therefore, there is a need for a growing method for improving the quality of the crystal to avoid the adverse effect on the quality of the crystal.
Disclosure of Invention
The invention provides a high-quality silicon carbide crystal growth method aiming at the problems of plane hexagonal cavities and the like caused by seed crystal ablation in the initial growth stage. Compared with the conventional silicon carbide crystal growth method, the method can greatly reduce the problems of plane hexagonal cavities and the like caused by seed crystal ablation in the initial growth stage, obtain high-quality silicon carbide crystals, and obviously improve the crystal qualification rate and the wafer quality. In order to achieve the above object, the present invention is characterized in that a crucible containing silicon carbide raw material and seed crystal is placed in a single crystal growth furnace, the crucible is rapidly pushed up by a distance ranging from 5mm to 50mm, the seed crystal is far away from a high temperature region, the silicon carbide raw material is sublimated and crystallized on the seed crystal under certain conditions of temperature, pressure and crucible movement, and the crystal is cooled to obtain silicon carbide single crystal. Wherein the temperature, pressure and crucible movement conditions are the following processes performed in sequence: (1) under the condition that the pressure is 20-80kPa, the temperature is raised to 2100-2400 ℃, the crucible is quickly pushed upwards by 5-50mm to ensure that the seed crystal is far away from the high-temperature region and is maintained for 1-10 h; (2) keeping the power of the heating power supply unchanged on the basis of the step (1), reducing the pressure to 100-3000Pa, and starting the crystallization growth of the SiC crystal on the seed crystal for 1-5 h; (3) keeping the pressure constant and the power of a heating power supply constant, and slowly descending the crucible for 5-50mm within 10-30 hours; (4) keeping the pressure constant, keeping the temperature at 2100-2400 ℃, keeping the temperature close to the growth temperature in the step (1) and keeping the difference not more than 50 ℃, and continuing to grow the crystal for 40-100 h; (5) raising the pressure to 20-80kPa, and cooling. The temperature is the temperature of the silicon carbide raw material in the crucible, and the pressure is the pressure in the growth chamber.
Therefore, the seed crystal is prevented from being ablated in a high-temperature area, and the appearance of a plane hexagonal cavity in the growth process is reduced. And meanwhile, in the crystal growth stage in the step (3), the crucible moves at a higher speed, so that different positions of the upper part, the lower part and the like of the raw material can be ensured to pass through a high-temperature region, the SiC raw material is fully utilized, the Si/C ratio of the growth atmosphere is ensured to be maintained stable, the generation of defects such as polytype, micropipe and the like is inhibited, and the high-quality silicon carbide crystal is grown.
Specifically, the method comprises the following steps:
and (2) placing the crucible filled with the silicon carbide raw material and the seed crystal in a single crystal growth furnace, quickly pushing the crucible upwards by a distance range of 5-50mm, keeping the seed crystal away from a high-temperature region, sublimating the silicon carbide raw material and crystallizing the silicon carbide raw material on the seed crystal under certain conditions of temperature, pressure and crucible movement, and cooling the crystal to obtain the silicon carbide single crystal.
Wherein, in the process (1), the pressure condition is 20 to 80kPa, preferably the pressure is 30 to 60kPa, and more preferably the pressure is 40 to 50 kPa.
Wherein, in the process (1), the crucible pushing-up distance is 5-50mm, preferably the crucible pushing-up distance is 10-40mm, and further preferably the crucible pushing-up distance is 20-30 mm.
Wherein, in the process (1), the speed of quickly pushing up the crucible is 1mm/min-20mm/min, preferably the speed of quickly pushing up the crucible is 5mm/min-15mm/min, and further preferably the speed of quickly pushing up the crucible is 8mm/min-12 mm/min.
Wherein, in the processes (1) to (4), the temperature condition is 2100-.
Wherein, in the process (1), the maintaining time is 1-10h, preferably 3-8h, and more preferably 4-7 h.
Wherein, in the processes (2) to (4), the pressure condition is 100-3000Pa, preferably the pressure is 300-2500Pa, and further preferably the pressure is 500-1500 Pa.
Wherein, in the process (2), the maintaining time is 1-5h, and preferably 2-4 h.
Wherein, in the process (3), the descending speed of the crucible is in the range of 0.5mm/h-2mm/h, and preferably in the range of 1.0mm/h-1.5 mm/h.
Wherein, in the process (4), the crystal continuous growth time is 40-100h, preferably the crystal continuous growth time is 50-90 h. It is further preferred that the crystals continue to grow for a period of 60 to 80 hours.
The invention has the following beneficial effects:
the invention provides a method for eliminating seed crystal ablation in the initial growth stage. The constant input heat is ensured by controlling the constant power of the heating power supply in the initial growth stage. The temperature of the seed crystal will not change if the crucible is not moved. According to the invention, the crucible is moved at the initial growth stage, and the seed crystal is far away from the high-temperature region, so that the problem of seed crystal ablation at the initial growth stage due to the fact that the seed crystal is thin at the same time of high temperature is solved. And then, when the crystal grows to a certain thickness, the interface shape of the surface of the crystal basically forms a convex interface which is basically matched with the shape of an isothermal line of a temperature field, so that the temperature of the edge of the crystal growth interface is basically the same as that of the central position of the crystal growth interface, the problem of preferential ablation of the crystal growth interface due to inconsistent temperature does not exist, and the ablation of seed crystals is avoided and the generation of hexagonal cavities is eliminated.
The invention provides a crystal growth method, which solves the problem of seed crystal ablation during initial growth of the seed crystal, and simultaneously, the temperature of the upper part of the SiC raw material is increased by moving the high-temperature reduction region upwards after the growth is finished, so that the temperature of the upper part of the SiC raw material is increased, the SiC raw material can be effectively sublimated and supplied to form meteorological components, and the raw material is fully utilized. Specifically, in the crystal growth stage in the step (3), the crucible moves at a relatively high speed, so that different positions of the upper part, the lower part and the like of the raw material can be ensured to pass through a high-temperature region, the SiC raw material is fully utilized, the Si/C ratio of the growth atmosphere is ensured to be maintained stable, defects such as polytype, micropipe and the like are inhibited, and high-quality silicon carbide crystals are grown.
Drawings
FIG. 1 is a schematic diagram showing temperature and pressure and crucible movement during SiC single crystal growth according to an embodiment of the present invention.
FIG. 2 is a schematic view showing temperature and pressure and crucible movement during the growth of a SiC single crystal according to a comparative example of the present invention.
FIG. 3 example 1 shows the non-growth surface condition of the seed crystal after completion of the growth of a silicon carbide crystal.
FIG. 4 example 2 shows the non-growth surface condition of the seed crystal after completion of the growth of the silicon carbide crystal.
FIG. 5 example 3 shows the non-growth surface condition of the seed crystal after completion of the growth of the silicon carbide crystal.
FIG. 6 shows the non-growth surface condition of the seed crystal after completion of the growth of the silicon carbide crystal of comparative example 1.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the method for eliminating seed crystal ablation at the initial growth stage and the method for growing silicon carbide crystal provided by the present invention are described in detail below with reference to the accompanying drawings.
The temperature pressure and crucible movement schematic diagram in the SiC single crystal growth process of the invention is shown in figure 1 and figure 2, and the invention is characterized in that in the crystal growth process, the crucible is pushed upwards to make the seed crystal far away from a high temperature region, so as to prevent the seed crystal from ablation and further eliminate the plane hexagonal cavity defect of the crystal. The high temperature reducing region moves upwards after the growth is finished, so that the temperature of the upper part of the SiC raw material is increased, the SiC raw material can be effectively sublimated and supplied to form meteorological components, the raw material is fully utilized, the silicon-carbon ratio of the gas-phase components is ensured to be relatively stable in the growth process, and the defects of other polytypes, microtubules and the like in the crystal are favorably reduced.
Example 1
A4H-SiC seed crystal is adopted, and a C surface is used as a crystal growth surface and is bonded on a graphite crucible cover. Filling enough SiC powder raw material at the bottom of the crucible, placing the crucible cover adhered with the seed crystal on the upper part of the crucible, and placing the crucible cover into a single crystal growth furnace after assembly. Pushing up the crucible by 20mm at the speed of 8mm/h, vacuumizing the single crystal furnace until the pressure is less than 10Pa, and sequentially carrying out the following processes: (1) filling mixed gas of argon and nitrogen into the growth furnace until the pressure reaches 30kPa, keeping the pressure unchanged, heating by adopting medium-frequency induction heating, setting the temperature of the raw materials at 2200-; (2) reducing the pressure to 1200Pa through a pressure control system of the growth furnace, and keeping the pressure for 2 hours; (3) maintaining the pressure at 1200pa for 20h, and lowering the crucible by 20mm at the speed of 1 mm/h; (4) continuously maintaining the pressure at 1200Pa for 100 h; (5) the pressure was raised to 30kPa, and cooling was carried out to obtain a 6-inch 4H-SiC conductive single crystal. And taking down the crystal, and observing the seed crystal ablation condition of the non-growth surface of the crystal. FIG. 3 shows the non-growth surface condition of the crystal after growth. As can be seen in fig. 3, the seed crystal is not ablated.
Example 2
A4H-SiC seed crystal is adopted, and a C surface is used as a crystal growth surface and is bonded on a graphite crucible cover. Filling enough SiC powder raw material at the bottom of the crucible, placing the crucible cover adhered with the seed crystal on the upper part of the crucible, and placing the crucible cover into a single crystal growth furnace after assembly. Pushing the crucible upwards by 30mm at the speed of 10mm/h, vacuumizing the single crystal furnace until the pressure is less than 10Pa, and sequentially carrying out the following processes: (1) inflating the growth furnace with mixed gas of argon and nitrogen until the pressure reaches 40kPa, keeping the pressure unchanged, heating by adopting medium-frequency induction heating, setting the temperature of the raw materials at 2100-2200 ℃, preserving the heat for 5 hours after the temperature reaches, and keeping the temperature in the furnace unchanged; (2) reducing the pressure to 800Pa through a pressure control system of the growth furnace, and keeping the pressure for 2 hours; (3) the pressure is maintained at 500pa for 20h, and the crucible is lowered by 30mm at the speed of 1.5 mm/h; (4) continuously maintaining the pressure at 500Pa for 80 h; (5) the pressure was raised to 40kPa, and cooling was carried out to obtain a 6-inch 4H-SiC conductive single crystal. And taking down the crystal, and observing the seed crystal ablation condition of the non-growth surface of the crystal. FIG. 4 shows the non-growth surface condition of the crystal after growth. As can be seen in fig. 4, the seed crystal is not ablated.
Example 3
A4H-SiC seed crystal is adopted, and a C surface is used as a crystal growth surface and is bonded on a graphite crucible cover. Filling enough SiC powder raw material at the bottom of the crucible, placing the crucible cover adhered with the seed crystal on the upper part of the crucible, and placing the crucible cover into a single crystal growth furnace after assembly. Pushing the crucible upwards by 40mm at the speed of 12mm/h, vacuumizing the single crystal furnace until the pressure is less than 10Pa, and sequentially carrying out the following processes: (1) filling mixed gas of argon and nitrogen into the growth furnace until the pressure reaches 60kPa, keeping the pressure unchanged, heating by adopting medium-frequency induction heating, setting the temperature of the raw materials at 2200-; (2) reducing the pressure to 1000Pa through a pressure control system of the growth furnace, and keeping the pressure for 5 hours; (3) the pressure is maintained at 1000pa for 10h, and the crucible is lowered by 30mm at the speed of 1.2 mm/h; (4) continuously maintaining the pressure at 1000Pa for 80 h; (5) the pressure was raised to 60kPa, and cooling was carried out to obtain a 6-inch 4H-SiC conductive single crystal. And taking down the crystal, and observing the seed crystal ablation condition of the non-growth surface of the crystal. FIG. 5 shows the non-growth surface condition of the crystal after growth. As can be seen in fig. 5, the seed crystal is not ablated.
Comparative example 1
A4H-SiC seed crystal is adopted, and a C surface is used as a crystal growth surface and is bonded on a graphite crucible cover. Filling enough SiC powder raw material at the bottom of the crucible, placing the crucible cover adhered with the seed crystal on the upper part of the crucible, and placing the crucible cover into a single crystal growth furnace after assembly. Vacuumizing the single crystal furnace until the pressure is less than 10Pa, and sequentially carrying out the following processes: (1) filling mixed gas of argon and nitrogen into the growth furnace until the pressure reaches 30kPa, keeping the pressure unchanged, heating by adopting medium-frequency induction heating, setting the temperature of the raw materials at 2200-; (2) reducing the pressure to 1000Pa through a pressure control system of the growth furnace, and keeping the pressure for 2 hours; (3) maintaining the pressure at 500pa for 20 h; (4) continuously maintaining the pressure at 1000Pa for 100 h; (5) the pressure was raised to 30kPa, and cooling was carried out to obtain a 6-inch 4H-SiC conductive single crystal. And taking down the crystal, and observing the seed crystal ablation condition of the non-growth surface of the crystal. FIG. 6 shows the non-growth surface condition of the crystal after growth. As can be seen in fig. 6, seed ablation occurs.
It should be noted that the above-mentioned embodiments are only illustrative of the present invention, and should not be construed as limiting the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the claims and that such changes are encompassed within the scope of the invention.
Claims (5)
1. A method for growing high-quality large-size silicon carbide crystals, which comprises the following steps: placing a crucible filled with silicon carbide raw materials and seed crystals in a single crystal growth furnace, quickly pushing the crucible upwards for a distance range of 5-50mm, keeping away from a high-temperature region, sublimating the silicon carbide raw materials and crystallizing the silicon carbide raw materials on the seed crystals under certain conditions of temperature, pressure and crucible movement, and cooling the crystals to obtain silicon carbide single crystals; the specific process comprises the following steps: (1) under the condition that the pressure is 20-80kPa, the temperature is raised to 2100-2400 ℃, the crucible is quickly pushed upwards by 5-50mm to ensure that the seed crystal is far away from the high-temperature region and is maintained for 1-10 h; (2) keeping the power of the heating power supply unchanged on the basis of the step (1), reducing the pressure to 100-3000Pa, and starting the crystallization growth of the SiC crystal on the seed crystal for 1-5 h; (3) keeping the pressure constant and the power of a heating power supply constant, and slowly descending the crucible for 5-50mm within 10-30 hours; (4) keeping the pressure constant, keeping the temperature at 2100-2400 ℃, keeping the temperature close to the growth temperature in the step (1) and keeping the difference not more than 50 ℃, and continuing to grow the crystal for 40-100 h; (5) raising the pressure to 20-80kPa, and cooling; the temperature is the temperature of the silicon carbide raw material in the crucible, and the pressure is the pressure in the growth chamber.
2. A method for growing high quality large size silicon carbide crystals according to claim 1 wherein: the seed crystal is a seed crystal which forms a certain angle with the basal plane (0001), and the angle range is 0-8 degrees.
3. A high quality large size silicon carbide crystal growth method according to claim 1 wherein the rate of crucible fast push-up from process (1) is 1mm/min to 20 mm/min.
4. The method as claimed in claim 1, wherein the pressure in the process (2) is controlled within the range of 500-1500Pa and the time is controlled within the range of 1-5 h.
5. A high quality large size silicon carbide crystal growth method according to claim 1 wherein the crucible lowering speed is controlled in the process (3) in the range of 0.5mm/h to 2 mm/h.
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| CN116905088B (en) * | 2023-09-12 | 2024-01-19 | 苏州优晶光电科技有限公司 | Control method and device for quality of silicon carbide crystal grown by resistance method and growth method |
| 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 |
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Application publication date: 20191220 Assignee: Shenzhen Reinvested Tianke Semiconductor Co.,Ltd. Assignor: TANKEBLUE SEMICONDUCTOR Co.,Ltd.|XINJIANG TANKEBLUE SEMICONDUCTOR Co.,Ltd. Contract record no.: X2023990000679 Denomination of invention: A High Quality Growth Method for Large Size Silicon Carbide Crystals Granted publication date: 20200925 License type: Common License Record date: 20230725 |
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