CN115029782B - Silicon carbide epitaxial growth method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 72
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 41
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- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 141
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 36
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 29
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 11
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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Abstract
The application discloses a silicon carbide epitaxial growth method. The growth method comprises a substrate in-situ etching stage, a buffer layer growth stage, a transition layer growth stage and a main body layer growth stage, wherein a pure and smooth surface beneficial to epitaxial growth is obtained through the substrate in-situ etching; introducing a C source gas and a Si source gas with the initial carbon-silicon ratio of less than 1 into the reaction cavity based on the spraying assembly in the buffer layer growth stage, gradually increasing the flow rate of the C source gas and the Si source gas, simultaneously heating the reaction cavity based on the heater to adjust the growth rate of the lateral growth of the buffer layer to improve the microtube, and growing the buffer layer with the thickness of 0.5-1.5 mu m on the surface of the substrate; and smoothly transitioning the C/Si ratio of the introduced C source gas and the introduced Si source gas to the C/Si ratio of the high-speed growth mode of the main body layer growth stage in the transition layer stage, and keeping the flow rate of the introduced gas at the end of the transition layer in the main body layer growth stage until the growth of the main body layer is finished. The growing method can obtain high-quality silicon carbide epitaxial wafer.
Description
Technical Field
The application relates to the technical field of epitaxial growth, in particular to a silicon carbide epitaxial growth method.
Background
In the epitaxial growth process of the silicon carbide, a substrate is placed on a graphite tray in a reaction cavity, a heater is used for heating, gas containing C element and gas containing Si element are introduced into the reaction cavity under the condition of proper temperature, and the gas containing C element and the gas containing Si element react on the surface of the substrate to grow the SiC single crystal film. The obtained SiC single crystal thin film is used for manufacturing electronic devices, and in order to improve the yield of electronic devices, it is necessary to reduce defects in the SiC single crystal thin film. Defects of the SiC single crystal film obtained by the existing epitaxial growth process mainly comprise micropipes, triangular dislocation, screw dislocation, basal plane dislocation, carrot defect, falling object defect, edge dislocation, micro pits, stacking faults and the like, and most of the defects can cause electric leakage, reduced withstand voltage, reverse breakdown and even failure of electronic devices. Among the defects, the micropipes, the screw dislocations and the basal plane dislocations mainly originate from the substrate material, most of the defects of the substrate extend to the epitaxial layer in the growth process except the defects brought by the epitaxial growth process, some defects are larger and larger, and some defects are fewer and smaller or even disappear due to the optimization of the epitaxial growth process, so that the silicon carbide epitaxy can improve or eliminate the defects to the maximum extent by improving the epitaxial growth process besides using the substrate with low defect density.
For micropipes, the reduction or elimination is mainly achieved by reducing the carbon-silicon ratio (C/Si ratio), growing in a Si-rich environment or reducing the growth temperature or increasing the growth rate, and when the methods are used alone, the micropipes can be reduced or eliminated, but new defects or epitaxial quality problems are accompanied. Such as: problems associated with the degradation of crystal quality and doping uniformity when grown in a Si-rich environment by reducing the C/Si ratio; the quality of epitaxial crystal may be affected when the growth temperature is lowered; increasing the growth rate is accompanied by increasing triangular and carrot dislocations, which also affect the uniformity of doping.
For this reason, there is a need to improve existing methods of epitaxial growth of silicon carbide.
Disclosure of Invention
To overcome the above disadvantages, the present application aims to: provided is a silicon carbide epitaxial growth method by which micropipe defects in a silicon carbide epitaxial wafer are reduced or even eliminated, while the defect density of the silicon carbide epitaxial wafer as a whole is reduced.
In order to achieve the purpose, the following technical scheme is adopted in the application:
a silicon carbide epitaxial growth method comprises the following steps;
substrate in-situ etching stage:
introducing hydrogen into the reaction cavity based on the spray assembly to adjust the pressure of the reaction cavity to a first preset pressure, heating the reaction cavity based on the heater,
when the temperature of the substrate reaches a first preset temperature, introducing hydrogen chloride gas into the reaction cavity, starting in-situ etching,
utilizing a heater to raise the temperature of the reaction cavity to a second preset temperature within the first preset temperature rise time, and maintaining the second preset temperature for the first preset time to finish in-situ etching;
and (3) a buffer layer growth stage: introducing doping gas, hydrogen chloride gas and C source gas and Si source gas with the initial carbon-silicon ratio less than 1 into the reaction cavity based on the spraying assembly, increasing the flow rates of the doping gas, the hydrogen chloride gas, the C source gas and the Si source gas to corresponding preset values, and simultaneously raising the temperature of the reaction cavity to a third preset temperature based on the heater and maintaining the third preset temperature for a second preset time to grow a buffer layer with a certain thickness;
in the transition layer growth stage, the flow rates of introduced C source gas, si source gas, doping gas and hydrogen chloride gas are respectively adjusted to corresponding growth preset values on the basis of the spraying assembly, the pressure of the reaction cavity is adjusted to a second preset pressure and lasts for a third preset time, and a transition layer with a certain thickness grows on the buffer layer;
and in the main body layer growth stage, the flow of the C source gas, the Si source gas, the doping gas and the hydrogen chloride gas introduced at the end of the transition layer growth stage is respectively maintained on the basis of the spraying assembly, the temperature of the reaction cavity is maintained at a third preset temperature for a fourth preset time, and the growth of the main body layer is completed. The growth method reduces the possibility of other problems caused by a unionization micropipe elimination method to the minimum, so as to achieve the purposes of reducing or even eliminating the micropipes of the epitaxial wafer with the highest efficiency, reducing the whole defect density of the epitaxial wafer and improving the uniformity of the thickness and the doping concentration.
In one embodiment, the C source gas and the Si source gas with the initial carbon-silicon ratio of 0.6-0.9 are introduced into the reaction chamber based on the spray assembly in the buffer layer growth stage.
In one embodiment, the second predetermined pressure is 50 to 150mbar higher than the first predetermined pressure.
In one embodiment, the third predetermined temperature is 10-20 ℃ higher than the second predetermined temperature. Therefore, the growth rate of the buffer layer is gradually increased in the process of uniformly increasing the temperature of the reaction cavity to close the micropipes on the substrate, so as to achieve the purpose of reducing or eliminating the micropipes.
In one embodiment, the buffer layer has a thickness of 0.5 to 1.5 μm.
In one embodiment, the bulk layer growth phase is performed by introducing a C source gas and a Si source gas into the reaction chamber based on the shower assembly, wherein the initial carbon-to-silicon ratio of the C source gas and the Si source gas is between 1.1 and 1.5.
In one embodiment, the substrate in-situ etch stage comprises:
introducing hydrogen with the flow rate of 50-110slm into the reaction cavity based on the spraying assembly, adjusting the pressure of the reaction cavity to 100-200mbar, and heating the reaction cavity at the heating rate of 0.5-2 ℃/S based on the heater;
when the temperature of the substrate reaches 1400-1500 ℃, introducing hydrogen chloride gas with the flow rate of 100-500sccm into the reaction cavity, starting in-situ etching,
and (3) increasing the temperature of the reaction cavity to 1550-1650 ℃ within 2-5 minutes by using a heater and maintaining for 1-3 minutes to finish in-situ etching.
In one embodiment, the buffer layer growth phase comprises:
c source gas with initial flow of 10-30sccm, si source gas with initial flow of 30-90sccm, doping gas with initial flow of 5-15sccm and hydrogen chloride with initial flow of 100-500sccm are introduced into the reaction cavity based on the spray assembly to start the growth of the buffer layer,
and uniformly raising the temperature of the reaction cavity to a third preset temperature by using a heater within 30-120S, simultaneously uniformly and rapidly adjusting the flow rate of the introduced C source gas to 40-120sccm, the flow rate of the introduced Si source gas to 100-300sccm, the flow rate of the doping gas to 15-40sccm, the flow rate of the hydrogen chloride to 400-1000sccm by using the spraying assembly, maintaining the third preset temperature for a second preset time, and growing a buffer layer with the thickness of 0.5-1.5 microns.
In one embodiment, the buffer layer comprises 2 layers or more than 2 layers, and the growth temperature for growing each buffer layer is sequentially increased layer by layer. This increases the growth temperature during buffer layer growth to reduce or eliminate micropipes.
In one embodiment, the body layer growth stage further comprises:
stopping introducing all process gases into the reaction cavity based on the spraying assembly, switching to introducing hydrogen, and cooling at the speed of 1-3 ℃/S;
and when the temperature of the reaction cavity is reduced to the wafer taking temperature, taking out the substrate or the substrate together with the tray by using the manipulator, and finishing the epitaxial growth.
Advantageous effects
The growth method of the embodiment of the application achieves the aim of reducing or eliminating micropipes, and simultaneously reduces the whole defect density of the obtained silicon carbide epitaxial wafer. In addition, the growth method has the aim of improving the uniformity of the thickness and the doping concentration of the epitaxial layer. In one embodiment, the micropipe density of the obtained silicon carbide epitaxial wafer is reduced by more than 99%, and other defects are maintained at a low level, so that the yield of electronic devices manufactured by the micropipe density is improved, and the cost of the electronic devices is reduced.
Drawings
The accompanying drawings are included to provide an understanding of the disclosed embodiments and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the example serve to explain the principles of the disclosure and not to limit the disclosure. The shapes and sizes of the various elements in the drawings are not to be considered as true proportions, but rather are merely intended to illustrate the context of the application.
Fig. 1 is a schematic cross-sectional view of a silicon carbide epitaxial growth apparatus according to an embodiment of the present application;
fig. 2 is a schematic flow chart illustrating a method for epitaxial growth of silicon carbide according to an embodiment of the present disclosure;
FIG. 3 is a schematic flow chart of an in-situ etching stage of the substrate in FIG. 2;
FIG. 4a is a graph illustrating a variation in process gas flow rate according to an embodiment of the present application;
FIG. 4b is a graph illustrating the variation of the process gas flow rate according to another embodiment of the present application;
FIG. 5a is a C/Si ratio plot of the introduced C source gas and the introduced Si source gas for the example of FIG. 4 a;
FIG. 5b is a C/Si ratio plot of the introduced C source gas and the introduced Si source gas for the 4b embodiment;
FIG. 6a is a graph showing the temperature of the substrate and the pressure in the reaction chamber for the example of FIG. 4 a;
FIG. 6b is a graph showing the temperature of the substrate and the pressure in the reaction chamber for the example of FIG. 4 b.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present application. The conditions employed in the examples may be further adjusted as determined by the particular manufacturer, and the conditions not specified are generally those used in routine experimentation.
The application provides a silicon carbide epitaxial growth method. The growth method comprises the following steps: the method comprises a substrate in-situ etching stage, a buffer layer growth stage, a transition layer growth stage and a main body layer growth stage. The growth method removes impurities adsorbed on the surface of the substrate through in-situ etching of the substrate, and obtains a pure and smooth surface beneficial to epitaxial growth. And in the buffer layer growth stage, introducing a C source gas, a Si source gas, a doping gas and a hydrogen chloride gas with the initial C/Si (carbon-silicon ratio) ratio of less than 1 into the reaction cavity based on the spraying assembly, then gradually increasing the flow of the introduced doping gas, hydrogen chloride gas, C source gas and Si source gas, simultaneously heating by using a heater to uniformly raise the temperature of the reaction cavity so as to adjust the growth rate of the lateral growth of the buffer layer to improve the microtube, and growing the buffer layer with the thickness of 0.5-1.5 mu m on the surface of the substrate. And in the transition layer stage, the flow rates of the introduced C source gas, si source gas, doping gas and hydrogen chloride gas are increased so as to rapidly and smoothly transition the C/Si ratio in the buffer layer stage to the C/Si ratio in the high-speed growth mode in the main body layer growth stage. And in the growth stage of the main body layer, the flow rates of the doping gas, the hydrogen chloride gas, the C source gas and the Si source gas which are introduced when the transition layer is finished are kept, and the preset time is maintained to finish the growth of the main body layer. The growth method can effectively reduce or eliminate micropipes, and simultaneously reduce the whole defect density of the obtained silicon carbide epitaxial wafer. The growth method is suitable for a horizontal gas flow type silicon carbide epitaxial growth apparatus or a vertical gas flow type silicon carbide epitaxial growth apparatus (the flow direction of the process gas is substantially perpendicular to the substrate).
The silicon carbide epitaxial growth method will be described below by taking a vertical gas flow type silicon carbide epitaxial growth apparatus as an example.
Fig. 1 is a schematic cross-sectional view of a silicon carbide epitaxial growth apparatus (hereinafter referred to as a growth apparatus) according to an embodiment of the present application.
The growing apparatus includes: the reaction module (10) is provided with a plurality of reaction modules,
a reaction chamber 10a is formed in the reaction module 10, a spray assembly 20 is disposed at the top of the reaction module 10, and the spray assembly 20 is used for introducing a gas (e.g., a C source gas, a Si source gas, a doping gas, a carrier gas, a shielding gas, etc.) into the reaction chamber 10 a.
The graphite tray 30 is disposed at the bottom of the reaction chamber 10a through a support 31, and the graphite tray 30 faces the shower assembly 20, and the graphite tray 30 is used for placing the substrate 40. The support portion 31 is connected to a driving portion (not shown), and rotates according to the driving of the driving portion, and the support portion rotates to drive the graphite tray to rotate. The bottom of the reaction chamber 10a is provided with an air outlet 11, which is connected to a vacuum pumping device 70 through a pipe 60. A heater 50 is disposed in the support 31, and the reaction chamber, the graphite tray, and the substrate are heated by the heater 50. The growth apparatus is operated to adjust the gas inflow of the shower unit 20 and the gas exhaust amount of the vacuum apparatus 70 to adjust the pressure of the reaction chamber 10 a. A temperature sensor is arranged in the reaction module and used for detecting the temperature of the substrate and the temperature of the reaction cavity.
During epitaxial growth, the substrate 40 is placed on the graphite tray 30, the graphite tray is driven to rotate based on the driving of the driving part, the substrate is further driven to rotate, and ethylene (C) is introduced into the reaction cavity by the spraying component 2 H 4 ) And trichlorosilane (SiHCL) 3 ) Or propane (C) 3 H 8 ) And Silane (SiH) 4 ) And introducing doping gas nitrogen to grow an epitaxial layer on the substrate.
Next, a silicon carbide epitaxial growth method (hereinafter referred to as a growth method) using the above-described growth apparatus will be described with reference to fig. 2 and 3. FIG. 2 is a schematic flow chart of an epitaxial growth method; fig. 3 is a schematic flow chart of the in-situ etching stage of the substrate in fig. 2.
The growth method comprises the following steps: the method comprises a substrate in-situ etching stage, a buffer layer growth stage, a transition layer growth stage and a main body layer growth stage.
In the in-situ etching stage of the substrate:
introducing hydrogen gas with flow rate of 50-110slm into the reaction chamber based on the spray assembly to adjust the pressure of the reaction chamber to a first preset pressure (such as 100-200 mbar), simultaneously heating the reaction chamber at a heating rate of 0.5-2 deg.C/S based on the heater,
when the temperature of the substrate rises to a first preset temperature (such as 1400-1500 ℃), introducing hydrogen chloride gas with the flow of 100-500sccm into the reaction cavity based on the spraying component, starting in-situ etching,
and (3) within the first preset temperature rise time (such as 2-5 minutes), raising the temperature of the reaction chamber to a second preset temperature (1550-1650 ℃) by using the heater, and maintaining the second preset temperature for the first preset time (such as 1-3 minutes) to finish the in-situ etching. A clean and smooth surface favorable for epitaxial growth is obtained on the substrate. And then entering a buffer layer growth stage.
And (3) a buffer layer growth stage:
c source gas with the initial flow of 10-30sccm, si source gas with the initial flow of 30-90sccm, doping gas with the initial flow of 5-15sccm and hydrogen chloride gas with the initial flow of 100-500sccm are introduced into the reaction cavity based on the spraying assembly,
in a second preset temperature rise time (such as 30-120S), the temperature of the reaction cavity is raised to a third preset temperature (the third preset temperature is higher than the second preset temperature by 10-20 ℃) by using the heater, meanwhile, the flow rate of the C source gas introduced into the reaction cavity is raised to 40-120sccm, the flow rate of the Si source gas is raised to 100-300sccm, the flow rate of the doping gas is raised to 15-40sccm, the flow rate of the hydrogen chloride is raised to 400-1000sccm by using the spray assembly, and the second preset time at the third preset temperature is maintained, so that a buffer layer with the thickness of 0.5-1.5 microns is grown on the surface of the substrate. And finishing the growth of the buffer layer. In this step, according to different requirements, the buffer layer can be split into 2 steps: respectively growing a first buffer layer and a second buffer layer; can also be split into more than 2 steps. In the step, the temperature of the heating reaction cavity based on the heater is gradually increased (the temperature of the substrate is synchronously and gradually increased), so that the growth rate of the buffer layer is gradually increased from slow to fast (the growth of the buffer layer adopts lateral growth) to close the micro-tubes on the substrate, and the aim of reducing or eliminating the micro-tubes is fulfilled. Microtube closure is described by way of example with a 4 ° off-axis silicon carbide substrate: during epitaxial growth, the microtubule can be decomposed into a plurality of unit closed-nucleus screw dislocations, the screw dislocations gradually incline and penetrate through a growth base crystal face to achieve the purpose of microtubule closure, and the screw dislocations hardly affect subsequently prepared devices. The growth mode of the Si-rich condition is advantageous for enhancing the closure of the micropipes during the CVD growth of the silicon carbide single crystal, so that the initial C/Si ratio is set to less than 1 (the initial C/Si ratio in the present application is between 0.6 and 0.9) at the growth stage of the buffer layer, and the micropipes can be substantially eliminated during the growth of the buffer layer having a thickness of between 0.5 and 1.5 μm on the surface of the substrate. However, the Si-rich growth brings other epitaxial defects, such as large steps or Si drops, and therefore the temperature is uniformly increased in the growth stage of the buffer layer to adjust the growth rate of lateral growth, improve the micropipe and simultaneously improve other epitaxial defects.
In the growth stage of the transition layer,
and within 10-30S, increasing the flow rate of the C source gas introduced into the reaction cavity to 80-240sccm, the flow rate of the Si source gas to 130-390sccm, the flow rate of the doping gas to 30-90sccm and the flow rate of the hydrogen chloride gas to 500-1500sccm based on the spraying assembly, uniformly increasing the pressure of the reaction cavity to 250-350mbar, maintaining the third preset temperature for 10-30S (the third preset time), and growing a transition layer with a certain thickness on the buffer layer. The transition layer stage is used for rapidly and smoothly transitioning the C/Si ratio of the buffer layer stage to the C/Si ratio of the high-speed growth mode of the main body layer growth stage.
The growth stage of the main body layer is carried out,
and respectively maintaining the flow of the introduced process gas when the growth stage of the transition layer is finished based on the spraying assembly, maintaining the temperature of the reaction cavity at a third preset temperature for a fourth preset time (such as 200-3600S), and finishing the growth of the main body layer.
Then stopping introducing all process gases into the reaction cavity based on the spraying assembly, switching to introducing hydrogen, and cooling at the speed of 1-3 ℃/S;
when the temperature of the reaction chamber is reduced to the temperature of taking the wafer (such as 900 ℃), the substrate or the substrate together with the tray is taken out by the mechanical arm, and the growth is finished. In the present embodiment, the epitaxial layer of 80% or more of the thickness of the epitaxial wafer is completed in the growth stage of the bulk layer. The initial C/Si ratio of the C source gas and the Si source gas introduced into the reaction chamber during the growth phase of the body layer must be greater than 1. Preferably, the initial C/Si ratio is between 1.1 and 1.5. In the method, the temperature of the substrate is slightly equal to the temperature of the reaction cavity. The flow of the process gas introduced in the substrate in-situ etching stage, the buffer layer growth stage, the transition layer growth stage and the main body layer growth stage needs to be in smooth transition (cannot be suddenly changed) according to a certain slope.
The silicon carbide epitaxial growth method proposed in the present application is verified below with reference to specific embodiments:
example 1:
the growth method for growing the silicon carbide epitaxial wafer of the 6-inch 4H crystal form with the buffer layer by adopting the growth device comprises the following reaction gases: ethylene (C) 2 H 4 ) Trichlorosilane (SiHCL) 3 ) And hydrogen chloride gas, and the doping gas is nitrogen. The carrier gas is hydrogen in the growth process. The reactant gas and the dopant gas are collectively referred to as a process gas.
The growth method comprises the following steps:
the substrate in-situ etching stage comprises:
introducing hydrogen with the flow rate of 110slm into the reaction cavity based on a spray pipe device, adjusting the pressure of the reaction cavity to 200mbar, and simultaneously heating the reaction cavity by using a heater at the heating rate of 1.2 ℃/S;
when the temperature of the substrate rises to 1500 ℃, introducing hydrogen chloride gas with the flow rate of 320sccm into the reaction cavity based on the spray pipe device, and starting in-situ etching;
the temperature of the reaction chamber is raised to 1590 ℃ by a heater within 2 minutes of raising time, and maintained at 1590 ℃ for 2 minutes, thereby completing the in-situ etching. Then entering the growth stage of the buffer layer,
the buffer layer growth stage comprises:
introducing ethylene with the initial flow of 20sccm, trichlorosilane with the initial flow of 60sccm, nitrogen with the initial flow of 8sccm and hydrogen chloride gas with the initial flow of 320sccm into the reaction cavity based on the spraying assembly, and starting to grow the buffer layer;
and (3) increasing the temperature of the reaction cavity to 1602 ℃ at a constant speed by using a heater within 100S (12 ℃), and simultaneously increasing the flow of ethylene gas introduced into the reaction cavity to 120sccm at a constant speed, the flow of trichlorosilane to 240sccm at a constant speed, the flow of nitrogen to 48sccm at a constant speed, the flow of hydrogen chloride to 960sccm at a constant speed by using a spray assembly, maintaining 100S, and finishing the growth of the buffer layer. And then entering a growth stage of the transition layer.
The growth stage of the transition layer comprises:
in the time of 30S, utilizing a spraying assembly to respectively increase the flow rate of ethylene introduced into the reaction cavity to 150sccm at a constant speed, increase the flow rate of trichlorosilane to 260sccm at a constant speed, increase the flow rate of nitrogen to 56sccm at a constant speed, increase the flow rate of hydrogen chloride to 1050sccm at a constant speed, increase the pressure of the reaction cavity to 300mbar at a constant speed, maintain the temperature of the reaction cavity to 1602 ℃ for 20S continuously, complete the growth of the transition layer, and then enter a main body layer growth stage;
the growth stage of the body layer comprises:
and (3) keeping the flow rate of the introduced process gas (ethylene 150sccm, trichlorosilane 260sccm, nitrogen 56sccm and hydrogen chloride 1050 sccm) at the end of the growth stage of the transition layer on the basis of the spray assembly, maintaining the temperature of the reaction chamber of 1602 ℃ for 600 seconds, and finishing the growth of the main body layer.
Then stopping introducing all process gases into the reaction cavity based on the spraying assembly, switching to introducing hydrogen into the reaction cavity, and cooling at the speed of 2 ℃/S;
when the temperature of the reaction chamber is reduced to the temperature of taking the wafer (such as 900 ℃), the substrate or the substrate together with the tray is taken out by the manipulator, and the growth is finished.
In the present embodiment, a process gas flow rate change curve in the epitaxial growth process is shown in fig. 4a, where in fig. 4a, the horizontal axis represents the growth time and the vertical axis represents the process gas flow rate. The growth time 0-t10 represents the substrate in-situ etching stage S1, t10-t20 represents the buffer layer growth stage S2, t20-t30 represents the transition layer growth stage S3, and t30-t40 represents the bulk layer growth stage S4.
The C/Si ratio curve of the C source gas and the Si source gas introduced into the reaction chamber during the epitaxial growth is shown in FIG. 5a, the horizontal axis represents the growth time (the time node on the horizontal axis represents the meaning of FIG. 4 a), and the vertical axis represents the C/Si ratio.
The graph of the substrate temperature and the reaction chamber pressure during the epitaxial growth process is shown in fig. 6a, in which the horizontal axis of fig. 6a represents the growth time (the time node on the horizontal axis represents the meaning of fig. 4 a), and the vertical axis represents the substrate temperature and the reaction chamber pressure.
Example 2:
the difference from example 1 is that the growth method was used to grow a 6 inch 4H crystal form silicon carbide epitaxial wafer with two/two buffer layers.
The growth method comprises the following steps:
the substrate in-situ etching stage comprises:
introducing hydrogen with the flow rate of 110slm into the reaction cavity based on a spray pipe device, adjusting the pressure of the reaction cavity to 200mbar, and simultaneously heating the reaction cavity by using a heater at the heating rate of 1.2 ℃/S;
when the temperature of the substrate rises to 1500 ℃, introducing hydrogen chloride gas with the flow rate of 320sccm into the reaction cavity based on the spray pipe device, and starting in-situ etching;
the temperature of the reaction chamber is raised to 1590 ℃ by a heater within 2 minutes of raising time, and maintained at 1590 ℃ for 2 minutes, thereby completing the in-situ etching. And then entering a buffer layer growth stage.
The growth stage of the buffer layer comprises:
introducing ethylene with the initial flow of 20sccm, trichlorosilane with the initial flow of 60sccm, nitrogen with the initial flow of 8sccm and hydrogen chloride gas with the initial flow of 320sccm into the reaction cavity based on the spraying assembly, and starting to grow a first buffer layer;
the temperature of the reaction cavity is uniformly increased to 1595 ℃ by using a heater within 50S, meanwhile, the flow rate of ethylene gas introduced into the reaction cavity is uniformly increased to 80sccm, the flow rate of trichlorosilane is uniformly increased to 200sccm, the flow rate of nitrogen is uniformly increased to 32sccm, the flow rate of hydrogen chloride is uniformly increased to 800sccm, the process is continued for 50S, the growth of the first buffer layer is completed, and then the growth of the second buffer layer is started;
and (3) increasing the temperature of the reaction cavity to 1602 ℃ at a constant speed by using a heater within 70S, simultaneously increasing the flow of ethylene introduced into the reaction cavity to 120sccm at a constant speed, increasing the flow of trichlorosilane to 240sccm at a constant speed, increasing the flow of nitrogen to 48sccm at a constant speed, increasing the flow of hydrogen chloride gas to 960sccm at a constant speed by using a spraying assembly, continuing for 70S, and finishing the growth of the second buffer layer. Then entering a growth stage of a transition layer;
the growth stage of the transition layer comprises:
in the time of 20S, the flow rate of ethylene introduced into the reaction cavity is increased to 150sccm at a constant speed, the flow rate of trichlorosilane is increased to 260sccm, the flow rate of nitrogen is increased to 56sccm, the flow rate of hydrogen chloride gas is increased to 1050sccm, the pressure of the reaction cavity is increased to 300mbar at a constant speed, the temperature of the reaction cavity is maintained at 1602 ℃ for 20S, and the growth of the transition layer is completed. Then the stage of the body layer is entered,
the growth stage of the body layer comprises:
and keeping the flow rate of the introduced process gas (ethylene 150sccm, trichlorosilane 260sccm, nitrogen 56sccm and hydrogen chloride 1050 sccm) at the end of the growth stage of the transition layer based on the spraying assembly, and maintaining the temperature of the reaction chamber at 1602 ℃ for 600 seconds to finish the growth of the main body layer.
Then stopping introducing all process gases into the reaction cavity based on the spraying assembly, switching to introducing hydrogen, and cooling at the speed of 2 ℃/S;
when the temperature of the reaction chamber is reduced to the temperature of taking the wafer (such as 900 ℃), the substrate or the substrate together with the tray is taken out by the mechanical arm, and the growth is finished.
In the present embodiment, a process gas flow rate change curve in the epitaxial growth process is shown in fig. 4b, in which the horizontal axis of fig. 4b represents the growth time and the vertical axis represents the process gas flow rate. The growth time of 0-t10 represents the substrate in-situ etching stage S1, the growth of a first buffer layer S21 in the buffer layer growth stage is represented by t10-t11, the growth of a second buffer layer S22 in the buffer layer growth stage is represented by t11-t20, the growth of a transition layer S3 is represented by t20-t30, and the growth of a main body layer S4 is represented by t30-t 40.
The C/Si ratio curve of the C source gas and the Si source gas introduced into the reaction chamber during the epitaxial growth is shown in fig. 5b, in which the horizontal axis of fig. 5b represents the growth time (the time node on the horizontal axis represents the meaning of fig. 4 b), and the vertical axis represents the C/Si ratio.
The graph of the substrate temperature and the chamber pressure during the epitaxial growth is shown in fig. 6b, in which the horizontal axis of fig. 6b represents the growth time (the time node on the horizontal axis represents the meaning of fig. 4 b), and the vertical axis represents the substrate temperature and the chamber pressure. The epitaxial wafer grown according to the method of this example had a measured thickness of about 12.6 μm and a doping concentration of 9.3E15/CM 3 The number of micropipes of the test epitaxial substrate before growth is 225, and the number of micropipes after growth is reduced to 1. The growth method proposed in the present application thus achieves the object of reducing or eliminating micropipes.
The above embodiments are merely illustrative of the technical concepts and features of the present application, and the purpose of the embodiments is to enable those skilled in the art to understand the content of the present application and implement the present application, and not to limit the protection scope of the present application. All equivalent changes and modifications made according to the spirit of the present application are intended to be covered by the scope of the present application.
Claims (8)
1. A silicon carbide epitaxial growth method is characterized by comprising the following steps:
substrate in-situ etching stage: introducing hydrogen into the reaction cavity based on the spraying assembly to adjust the pressure of the reaction cavity to a first preset pressure, heating the reaction cavity based on the heater, introducing hydrogen chloride gas into the reaction cavity when the temperature of the substrate reaches the first preset temperature, starting in-situ etching, raising the temperature of the reaction cavity to a second preset temperature by using the heater within a first preset temperature rise time, and maintaining the second preset temperature for a first preset time to finish in-situ etching;
and (3) a buffer layer growth stage: introducing doping gas, hydrogen chloride gas and C source gas and Si source gas with the initial carbon-silicon ratio of 0.6-0.9 into the reaction cavity based on the spraying assembly, increasing the flow rates of the doping gas, the hydrogen chloride gas, the C source gas and the Si source gas to corresponding preset values, and simultaneously raising the temperature of the reaction cavity to a third preset temperature based on the heater and maintaining the third preset temperature for a second preset time to grow a buffer layer with a certain thickness;
in the transition layer growth stage, the flow rates of introduced C source gas, si source gas, doping gas and hydrogen chloride gas are respectively adjusted to corresponding growth preset values on the basis of the spraying assembly, the pressure of the reaction cavity is adjusted to a second preset pressure and lasts for a third preset time, and a transition layer with a certain thickness grows on the buffer layer;
and in the main body layer growth stage, the flow rates of the C source gas, the Si source gas, the doping gas and the hydrogen chloride gas are respectively maintained when the growth stage of the transition layer is finished based on the spraying assembly, the initial carbon-silicon ratio of the introduced C source gas and the introduced Si source gas is between 1.1 and 1.5, the temperature of the reaction cavity is maintained at a third preset temperature and lasts for a fourth preset time, and the growth of the main body layer is finished.
2. The method of epitaxial growth of silicon carbide according to claim 1,
the thickness of the buffer layer is between 0.5 and 1.5 mu m.
3. The method of epitaxial growth of silicon carbide according to claim 1,
the second predetermined pressure is 50-150mbar higher than the first predetermined pressure.
4. The silicon carbide epitaxial growth method of claim 1,
the third preset temperature is 10-20 ℃ higher than the second preset temperature.
5. The method of epitaxial growth of silicon carbide according to claim 1,
the substrate in-situ etching stage comprises:
introducing hydrogen with the flow rate of 50-110slm into the reaction cavity based on the spraying assembly, adjusting the pressure of the reaction cavity to 100-200mbar, and simultaneously heating the reaction cavity at the heating rate of 0.5-2 ℃/S based on the heater;
when the temperature of the substrate reaches 1400-1500 ℃, introducing hydrogen chloride gas with the flow rate of 100-500sccm into the reaction cavity, starting in-situ etching,
and (3) increasing the temperature of the reaction cavity to 1550-1650 ℃ within 2-5 minutes by using a heater and maintaining for 1-3 minutes to finish in-situ etching.
6. The silicon carbide epitaxial growth method of claim 1,
the buffer layer growth stage comprises:
c source gas with initial flow of 10-30sccm, si source gas with initial flow of 30-90sccm, doping gas with initial flow of 5-15sccm and hydrogen chloride gas with flow of 100-500sccm are introduced into the reaction cavity based on the spraying assembly to start the growth of the buffer layer,
and uniformly raising the temperature of the reaction cavity to a third preset temperature by using a heater within 30-120S, simultaneously uniformly and rapidly adjusting the flow of the introduced C source gas to 40-120sccm, the flow of the Si source gas to 100-300sccm, the flow of the doping gas to 15-40sccm, the flow of the hydrogen chloride gas to 400-1000sccm by using a spraying assembly, maintaining the third preset temperature for a second preset time, and growing a buffer layer with the thickness of 0.5-1.5 microns.
7. The silicon carbide epitaxial growth method according to claim 6,
the buffer layer comprises 2 layers or more than 2 layers, and the growth temperature corresponding to each layer of buffer layer is increased layer by layer.
8. The method of epitaxial growth of silicon carbide according to claim 1,
the main body layer growth stage is followed by:
stopping introducing all process gases into the reaction cavity based on the spraying assembly, switching to introducing hydrogen, and cooling at the speed of 1-3 ℃/S;
and when the temperature of the reaction cavity is reduced to the wafer taking temperature, taking out the substrate or the substrate together with the tray by using the manipulator, and finishing the epitaxial growth.
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