CN111424319B - Preparation method of large-size kilogram-level silicon carbide single crystal - Google Patents
Preparation method of large-size kilogram-level silicon carbide single crystal Download PDFInfo
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- CN111424319B CN111424319B CN202010396973.7A CN202010396973A CN111424319B CN 111424319 B CN111424319 B CN 111424319B CN 202010396973 A CN202010396973 A CN 202010396973A CN 111424319 B CN111424319 B CN 111424319B
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Abstract
The invention discloses a preparation method of a large-size kilogram-level silicon carbide single crystal, which comprises the following steps: arranging a gas inlet at the center of the bottom of the crucible, and introducing raw material gas containing silicon and carbon elements and carrier gas; an exhaust hole is formed in the upper side wall of the crucible, an upper cover at the top of the crucible has no air hole, and seed crystals are fixed on the inner wall of the upper cover; heating the crucible, introducing the raw material gas into a gas inlet in the center of the bottom of the crucible, flowing to the position of the seed crystal under the carrying of the carrier gas, and simultaneously carrying out a chemical reaction on the raw material gas, wherein the chemical reaction generates silicon carbide molecules by controlling the temperature, the pressure and the concentration ratio and the flow of the raw material gas and deposits on the surface of the seed crystal; the reaction byproduct gas and the incompletely reacted raw material gas are exhausted through an exhaust hole on the side wall of the crucible under the carrying of carrier gas; and finally obtaining the silicon carbide crystal at the seed crystal. The method successfully solves the problem that the prior art can not realize the growth of the silicon carbide crystals with large size, kilogram level and high quality at the same time, increases the output, reduces the cost and improves the crystal quality.
Description
Technical Field
The invention relates to the field of preparation of silicon carbide single crystals, in particular to a preparation method of large-size kilogram-level silicon carbide single crystals.
Background
The silicon carbide single crystal has unique properties of large forbidden bandwidth, high breakdown electric field, large thermal conductivity, small dielectric constant, stable physical and chemical properties and the like, and is considered as an ideal semiconductor material for manufacturing high-temperature, high-voltage, high-frequency and high-power devices and the like. Since silicon carbide crystals are too costly to limit their practical application, an effective way to reduce the cost of the crystals is to enlarge the size and length of the crystals.
The silicon carbide single crystal growth methods currently used commercially are mainly classified into a physical vapor transport method (PVT) and a high temperature chemical vapor deposition method (HTCVD).
The physical vapor transport method (PVT) adopts solid silicon carbide powder as a raw material, quantitative powder is placed in a closed crucible, then the crucible is placed in a high-temperature vacuum heating cavity for growth, then the reaction cavity is opened by cooling and inflating, and the crucible is taken out to obtain crystals. The length of PVT growing silicon carbide crystal is limited because the amount of the powder is fixed and the powder cannot be added in the growing process. Meanwhile, the solid powder contains impurities, and C particles are included in crystals due to unbalance of Si/C ratio in the sublimation process. The method can not realize the preparation of kilogram-grade, high-thickness and high-quality silicon carbide crystals at present.
The High Temperature Chemical Vapor Deposition (HTCVD) method uses gas as a raw material, the raw material enters through a gas inlet at the bottom of a crucible, deposits on the surface of a seed crystal under the growth temperature and pressure to grow a crystal, and residual gas flows out through a pore at the top of the crucible. Although the method can continuously feed materials in the growth process, because the gas inlet hole of the crucible is arranged at the bottom and the gas outlet hole is arranged at the top of the crucible, all gases in the growth process, including residual incompletely reacted gases, gases generated after chemical reaction and carrier gases, are discharged out of the crucible through the top gas hole, namely the side edge of the crystal due to the buoyancy effect, and disturbance is caused to the crystal growth interface, especially etching gases (such as hydrogen) newly generated in the chemical reaction process have a strong etching effect on the grown silicon carbide crystal under a high-temperature environment, especially the edge of the crystal with the largest gas flow rate, and finally the diameter of the grown crystal is smaller than that of the seed crystal, namely the growth of the large-size silicon carbide crystal is difficult to realize.
In the prior art, the growth of large-size, kilogram-level and high-quality silicon carbide crystals cannot be realized simultaneously. How to grow large-size, kilogram-level and high-quality silicon carbide crystals in actual production, increase output, reduce cost and improve quality is a technical problem which needs to be solved urgently in the technical field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a silicon carbide crystal growth method, which solves the problems of limited length and quality of the silicon carbide crystal grown by a PVT method and the problem of undersize of the silicon carbide crystal grown by an HTCVD method, can realize the growth of the large-size, kilogram-level and high-quality silicon carbide crystal at the same time, and is a brand new innovative method.
In order to achieve the above object, the present invention provides a method for preparing large-size kilogram-scale silicon carbide crystals, comprising:
arranging a gas inlet at the center of the bottom of the crucible, and introducing raw material gas containing silicon and carbon elements and carrier gas; an exhaust hole is formed in the upper side wall of the crucible, an upper cover at the top of the crucible has no air hole, and seed crystals are fixed on the inner wall of the upper cover. Heating the crucible, introducing the raw material gas into a gas inlet in the center of the bottom of the crucible, flowing to the position of the seed crystal under the carrying of the carrier gas, and simultaneously carrying out a chemical reaction on the raw material gas, wherein the chemical reaction generates silicon carbide atoms and deposits on the surface of the seed crystal by controlling the temperature, the pressure, the concentration ratio and the flow of the raw material gas. The reaction byproduct gas and the incompletely reacted raw material gas are exhausted through the exhaust hole on the side wall of the crucible under the carrying of the carrier gas. And finally obtaining the silicon carbide crystal at the seed crystal.
Further, the crucible comprises an upper cover and a crucible body, the upper cover is 5-40 mm thick and has no opening, and the upper cover and the crucible body are connected in a threaded manner, a clamping groove and a nut.
Further, the crucible body is round platform form, cavity, and lateral wall thickness 5 ~ 30mm, end thickness 5 ~ 40mm, the contained angle of crucible lateral wall and bottom is 45 ~ 85.
Furthermore, a hole is formed in the center of the bottom of the crucible, and the size of the hole is 5-30 mm.
Furthermore, an air hole is reserved in the side wall of the crucible, and the distance between the position of the air hole and the upper edge of the crucible body is 1-10 mm.
Furthermore, the diameter of the side wall air hole is 0.5-10 mm.
Further, the row number of the side wall air holes is 1-10 rows, the distance between every two rows is 1-10 mm, the number of each air vent is 1-10, and the distribution of each air vent is uniform and axisymmetric.
Furthermore, the exhaust hole of the crucible is plated with a high-temperature-resistant corrosion-resistant coating comprising tantalum carbide and tungsten carbide, and the thickness of the coating is 1-500 mu m.
11. Further, the raw material gas is SiH4And CmHnThe SiH4And CmHnThe concentration ratio is (m-0.5) to (m +0.5), and the purity is 4N to 7N.
Further, the carrier gas is helium (He) or hydrogen (H)2) The purity is 4N-7N, and the flow rate is the raw material reaction gas SiH4And CmHnOf the total flow30 to 100 times.
In the invention, gas is used as a raw material, and the raw material can be continuously supplied in the crystal growth process through the opening at the bottom of the crucible, so that the possibility of the growth of kilogram-level silicon carbide crystals is ensured; in order to prevent the etching gas from etching the crystal growth, the invention opens the exhaust holes on the side wall of the graphite crucible instead of the top, and avoids the etching of the gas on the crystal through different sizes, quantities and gaps; and the crucible structure is designed into a truncated cone shape, so that the diameter of the crystal is expanded and grown, the problem that the diameter of the grown crystal is difficult to be larger than that of the seed crystal is solved, and the growth of the large-size kilogram-level silicon carbide crystal is successfully realized.
Drawings
FIG. 1 is a schematic view of the inventive structure and silicon carbide crystal growth.
Description of the reference numerals
1. Quartz tube
2. Induction coil
3. Crucible cover
4. Seed crystal
5. Thermal insulation felt
6. Exhaust hole on side wall of crucible
7. Grown crystal
8. Round platform shaped crucible
9. Crucible bottom
10. Crucible air inlet
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for accurately setting temperature, which comprises a preparation method of a large-size kilogram-level silicon carbide single crystal, and the preparation method comprises the following steps: arranging a gas inlet at the center of the bottom of the crucible, and introducing raw material gas containing silicon and carbon elements and carrier gas; an exhaust hole is formed in the upper side wall of the crucible, an upper cover at the top of the crucible has no air hole, and seed crystals are fixed on the inner wall of the upper cover. Heating the crucible, introducing the raw material gas into a gas inlet in the center of the bottom of the crucible, flowing to the position of the seed crystal under the carrying of the carrier gas, and simultaneously carrying out a chemical reaction on the raw material gas, wherein the chemical reaction generates silicon carbide atoms and deposits on the surface of the seed crystal by controlling the temperature, the pressure, the concentration ratio and the flow of the raw material gas. The reaction byproduct gas and the incompletely reacted raw material gas are exhausted through the exhaust hole on the side wall of the crucible under the carrying of the carrier gas. And finally obtaining the silicon carbide crystal at the seed crystal.
In the invention, preferably, the seed crystal is a high-quality silicon carbide substrate, and the seed crystal is fixed by bonding or a clamping ring; the traditional bonding mode needs heat treatment, so that the preparation process is long, the cost is high, the crystal taking process is complicated after the crystal growth is finished, and the risk of damaging the crystal is caused; preferably, snap ring fixation is advantageous.
In the invention, the single crystal furnace is preferably a medium-frequency induction heating system, and a quartz tube is preferably arranged in the single crystal furnace to serve as a reaction cavity.
In the invention, preferably, the crucible is coated with a heat insulation material on the outer wall, the heat insulation material is resistant to high temperature of not less than 2600 ℃, and preferably, the graphite felt is prepared from silicon carbide crystals.
In the invention, preferably, the temperature is measured by a bicolor thermometer, and the temperature is measured by focusing on the top of the crucible and the center of the outer side of the top of the crucible.
In the present invention, preferably, the pressure refers to a pressure inside the quartz tube and outside the crucible, the pressure is controlled by a conventional butterfly valve that can be used for controlling the pressure, and preferably, He gas is introduced into the reaction chamber during the crystal growth process, the pressure in the reaction chamber is controlled by adjusting the introduction amount of He gas, and the flow rate of He gas is calculated and set according to the target pressure and the adjustment time.
In the present invention, preferably, hydrogen (H)2) Or helium (He) gas as a carrier gas, has a small molecular weight and does not participate in chemical reactionsIt should be preferred that helium (He) be non-etching, as compared to hydrogen (H)2) Has better effect.
Example one
1. Preparing materials:
the diameter of the seed crystal used in the embodiment is 100mm, the thickness is 0.5mm, and the conductivity type is n type; and chemically cleaning, namely fixing the silicon surface and the crucible surface in seamless contact by using a snap ring structure at the center of the inner wall of the top of the crucible.
A graphite crucible is selected, the thickness of a truncated cone-shaped upper cover is 10mm, 7 rows of open air holes are reserved in the side wall, a first row of open air holes are arranged at the position of 10mm from the top of the crucible, the hole center distance of each row of open air holes is 10mm, the open air holes are round holes with the aperture of 4mm, and 10 open air holes are formed in each row of open air holes in an axial symmetry mode. The included angle between the side wall and the bottom cover is 60 degrees.
Selecting raw material Silane (SiH)4) Methane (CH) as a source of Si species4) As a source of C species, raw Silane (SiH)4) And methane (CH)4) Purity 5N, carrier gas helium (He) purity 4N5, Silane (SiH)4) With methane (CH)4) The concentration ratio was 1.1.
2. And (3) crystal growth process:
charging: the whole crucible wrapped with the graphite heat preservation felt is placed in a quartz cavity in a single crystal furnace, the three axes are concentric through centering adjustment, and a double-color temperature measuring instrument is struck to the center of the outer wall of the top of the crucible.
Washing the furnace: setting parameters, executing a furnace washing program (1), and vacuumizing until the pressure is 0.1 mbar; (2) opening a helium valve, introducing carrier gas helium with the flow of 7slm and the pressure of 950mbar, and keeping for 10 min; (3) pumping until the pressure is 0.1 mar; (4) repeating the processes of (2) and (3) for 2 times.
Temperature rise and crystal growth: (1) under the condition that the flow rate of He gas in the reaction cavity is 1slm, reducing the pressure in the reaction cavity to a target pressure value of 100mbar, and heating a graphite crucible in the reaction cavity to 2250 ℃; (2) after the temperature reaches 2250 ℃, SiH of reaction gas is opened4And CH4Valve for regulating SiH of reaction gas4At a flow rate of 100sccm and a concentration of 0.33mol/m3Adjusting the reaction gas CH4Flow velocity ofIs 40sccm and has a concentration of 0.30mol/m3. The flow rate of He was adjusted to 6 slm. The pressure control butterfly valve is opened and the pressure in the reaction chamber is kept at 100 mbar. In the process of crystal growth, the chemical reaction equation is as follows:
by-product H2And the carrier gas is exhausted from the air holes on the side wall of the crucible along with the carrier gas. The crystal growth is carried out for 150h by maintaining the parameters.
Cooling: and after the crystal growth procedure is finished, stopping heating, and slowly cooling along with the furnace.
Opening the furnace and taking crystals: charging air to atmospheric pressure, taking out of the furnace and taking the crystal down. A silicon carbide crystal having a maximum crystal diameter of 151mm and a weight of 2.06 kg was obtained.
Example two
1. Preparing materials:
the diameter of the used seed crystal selected in the embodiment is 76.2mm, the thickness is 1mm, and the conductive type is semi-insulating; chemical cleaning, fixing the crucible top inner wall center by adhesive and bonding process, wherein the silicon surface is tightly bonded with the crucible surface.
The method comprises the steps of selecting a tantalum carbide crucible, wherein the thickness of an upper cover in a circular truncated cone shape is 20mm, 5 rows of open air holes are reserved in the side wall, a first row of open air holes are formed in the position 5mm away from the top of the crucible, the hole center distance of each row of open air holes is 5mm, the open air holes are round holes with the aperture of 3mm, and 8 open air holes are formed in each row of open air holes in an axial symmetry mode. The included angle between the side wall and the bottom cover is 45 degrees.
Raw Silane (SiH)4) And ethane (C)2H6) Purity of 6N, carrier gas hydrogen (H)2) Purity of 5N, Silane (SiH)4) With ethane (C)2H6) The concentration ratio was 2.3.
2. And (3) crystal growth process:
charging: the whole crucible wrapped with the graphite heat preservation felt is placed in a quartz cavity in a single crystal furnace, the three axes are concentric through centering adjustment, and a double-color temperature measuring instrument is struck to the center of the outer wall of the top of the crucible.
Washing the furnace: setting parameters, executing a furnace washing program (1), and vacuumizing until the pressure is 0.1 mbar; (2) opening a hydrogen valve, introducing carrier gas with the flow rate of 5slm, raising the pressure to 950mbar, and keeping the pressure for 10 min; (3) pumping until the pressure is 0.1 mar; (4) repeating the processes of (2) and (3) for 3 times.
Temperature rise and crystal growth: (1) in the reaction chamber H2Reducing the pressure in the reaction chamber to a target pressure value of 120mbar under the condition that the flow rate of the gas is 2slm, and heating the graphite crucible in the reaction chamber to 2200 ℃; (2) after reaching 2200 deg.C, the reaction gas SiH is turned on4And C2H6Valve for regulating SiH of reaction gas4At a flow rate of 103sccm and a concentration of 0.42mol/m3Adjusting the reaction gas C2H6At a flow rate of 31sccm and a concentration of 0.18mol/m3. Adjusting H2The flow rate of (2) was 7 slm. And opening a pressure control butterfly valve, keeping the pressure in the reaction chamber at 120mbar, and maintaining the parameters to perform crystal growth for 100 hours in the crystal growth process.
Cooling: and after the crystal growth procedure is finished, stopping heating, and slowly cooling along with the furnace.
Opening the furnace and taking crystals: charging air to atmospheric pressure, taking out of the furnace and taking the crystal down. A silicon carbide crystal having a maximum crystal diameter of 100mm and a weight of 1.32 kg was obtained.
EXAMPLE III
1. Preparing materials:
the diameter of the seed crystal used in the embodiment is 150mm, the thickness is 0.5mm, and the conductivity type is n type; chemical cleaning; the silicon surface is fixed at the center of the inner wall of the top of the crucible by using an adhesive and an adhesion process, wherein the silicon surface is tightly adhered with the crucible surface.
The graphite crucible with the high-temperature coating is selected, the thickness of the upper cover in the shape of a circular truncated cone is 40mm, 10 rows of open air holes are reserved in the side wall, a first row of open air holes are formed in the position 10mm away from the top of the crucible, the hole center distance of each row of open air holes is 8mm, the open air holes are round holes with the aperture of 3mm, and 10 open air holes are formed in each row of open air holes in an axial symmetry mode. The included angle between the side wall and the bottom cover is 80 degrees.
Raw Silane (SiH)4) And methane (C)3H8) Purity 5N5, carrier gas helium (He) purity 5N, Silane (SiH)4) With methane (C)3H8) The concentration ratio was 2.95.
2. And (3) crystal growth process:
washing the furnace: setting parameters, executing a furnace washing program (1), and vacuumizing until the pressure is 0.1 mbar; (2) opening a helium valve, introducing carrier gas helium with the flow of 10slm and the pressure rising to 950mbar, and keeping for 13 min; (3) pumping until the pressure is 0.1 mar; (4) repeating the processes of (2) and (3) for 3 times.
Temperature rise and crystal growth: (1) under the condition that the flow rate of He gas in the reaction cavity is 5slm, reducing the pressure in the reaction cavity to a target pressure value of 150mbar, and heating the graphite crucible in the reaction cavity to 2300 ℃; (4) after the temperature reaches 2300 ℃, SiH of reaction gas is opened4And C3H8Valve for regulating SiH of reaction gas4At a flow rate of 115sccm and a concentration of 0.41mol/m3Adjusting the reaction gas C3H8At a flow rate of 33sccm and a concentration of 0.14mol/m3. The flow rate of He was adjusted to 10 slm. The pressure control butterfly valve was opened and the pressure in the reaction chamber was kept at 150 mbar. During the crystal growth, the crystal growth is carried out for 135h while maintaining the parameters.
Cooling: and after the crystal growth procedure is finished, stopping heating, and slowly cooling along with the furnace.
Opening the furnace and taking crystals: charging air to atmospheric pressure, taking out of the furnace and taking the crystal down. A silicon carbide crystal having a maximum crystal diameter of 185mm and a weight of 3.1 kg was obtained.
TABLE 1
As can be seen from the results in Table 1, a large-size kilogram-scale silicon carbide crystal can be obtained by the preparation method of the invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A preparation method of a large-size kilogram-level silicon carbide single crystal comprises the following steps: a gas inlet is arranged at the center of the bottom of the crucible, and raw material gas containing silicon and carbon elements and carrier gas are introduced; an exhaust hole is formed in the upper side wall of the crucible, an upper cover at the top of the crucible has no air hole, and seed crystals are fixed on the inner wall of the upper cover; heating the crucible, introducing the raw material gas into a gas inlet in the center of the bottom of the crucible, flowing to the position of the seed crystal under the carrying of the carrier gas, and simultaneously carrying out a chemical reaction on the raw material gas, wherein the chemical reaction generates silicon carbide molecules by controlling the temperature, the pressure, the concentration ratio and the flow of the raw material gas and deposits on the surface of the seed crystal; the reaction byproduct gas and the incompletely reacted raw material gas are exhausted through an exhaust hole on the side wall of the crucible under the load of the carrier gas; and finally obtaining the silicon carbide crystal at the seed crystal.
2. A preparation method of a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the crucible is composed of an upper cover and a crucible body, the upper cover is 5-40 mm thick and has no opening, and the upper cover and the crucible body are connected in a screw thread mode, a clamping groove mode and a nut mode.
3. A preparation method of a large-size kilogram-level silicon carbide single crystal according to claim 1, wherein the crucible body is truncated cone-shaped and hollow, the side wall thickness is 5-30 mm, the bottom thickness is 5-40 mm, and an included angle between the side wall and the bottom of the crucible is 45-85 degrees.
4. A method for preparing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the bottom of the crucible is provided with a hole at the center, and the size of the hole is 5-30 mm.
5. A method for preparing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein air holes are formed in the upper side wall of the crucible, and the positions of the air holes are 1-10 mm away from the upper edge of the crucible body.
6. A method for preparing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the diameter of the side-wall pores is 0.5-10 mm.
7. A method for preparing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the number of rows of side wall air holes is 1-10, the distance between each row is 1-10 mm, the number of each exhaust hole is 1-10, and the distribution of each exhaust hole is uniform and axisymmetric.
8. A preparation method of large-size kilogram-scale silicon carbide single crystals as claimed in claim 1, wherein the exhaust hole of the crucible is plated with a high-temperature-resistant and corrosion-resistant coating comprising tantalum carbide and tungsten carbide, and the coating thickness is 1-500 μm.
9. The method for producing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the source gas is SiH4And CmHnThe SiH4And CmHnThe concentration ratio is (m-0.5) to (m +0.5), and the purity is 4N to 7N.
10. A method for preparing a large-size kilogram-scale silicon carbide single crystal according to claim 1, wherein the carrier gas is helium (He) or hydrogen (H)2) The purity is 4N-7N, and the flow rate is the raw material reaction gas SiH4And CmHn30-100 times of the total flow.
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| CN112458532A (en) * | 2020-11-30 | 2021-03-09 | 山西烁科晶体有限公司 | Device and method for preparing silicon carbide single crystal through high-temperature chemical deposition |
| CN113026099A (en) * | 2021-03-05 | 2021-06-25 | 广州爱思威科技股份有限公司 | Silicon carbide single crystal growth control device and control method |
| CN113136622A (en) * | 2021-04-22 | 2021-07-20 | 中国电子科技集团公司第四十六研究所 | PVT method airflow-oriented silicon carbide single crystal growth device and using method |
| CN113502542A (en) * | 2021-09-10 | 2021-10-15 | 江苏超芯星半导体有限公司 | Growth control system and method for silicon carbide crystal by HTCVD method |
| CN113957534A (en) * | 2021-09-22 | 2022-01-21 | 广州爱思威科技股份有限公司 | Preparation method of 8-inch silicon carbide single crystal |
| CN115287749B (en) * | 2022-08-30 | 2023-09-12 | 江苏集芯先进材料有限公司 | Silicon carbide crystal growth apparatus capable of suppressing polycrystalline edge |
| CN117867648A (en) * | 2024-01-03 | 2024-04-12 | 杭州乾晶半导体有限公司 | Silicon carbide crystal expanding growth device and silicon carbide crystal expanding growth method |
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| CN106435735A (en) * | 2016-12-09 | 2017-02-22 | 河北同光晶体有限公司 | Method for optimizing growth of silicon carbide single crystals |
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