CN111081834A - Novel method for growing GaN epitaxial layer on sapphire and GaN epitaxial layer - Google Patents

Novel method for growing GaN epitaxial layer on sapphire and GaN epitaxial layer Download PDF

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CN111081834A
CN111081834A CN201911402230.XA CN201911402230A CN111081834A CN 111081834 A CN111081834 A CN 111081834A CN 201911402230 A CN201911402230 A CN 201911402230A CN 111081834 A CN111081834 A CN 111081834A
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temperature
gan
epitaxial layer
nucleation
sapphire
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CN111081834B (en
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刘双韬
赵德刚
朱建军
杨静
江德生
刘宗顺
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0095—Post-treatment of devices, e.g. annealing, recrystallisation or short-circuit elimination
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/26—Materials of the light emitting region
    • H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
    • H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen

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Abstract

A method for growing a GaN epitaxial layer on sapphire and the GaN epitaxial layer are provided, wherein the method comprises the following steps: performing high-temperature nucleation treatment on the sapphire substrate to form a GaN nucleation center on the sapphire substrate; growing a buffer layer on the sapphire substrate containing the GaN nucleation centers; heating and annealing the buffer layer to form the buffer layer with nucleation islands; and growing a GaN epitaxial layer on the buffer layer with the nucleation islands to obtain the GaN epitaxial layer on the sapphire. According to the invention, a high-temperature nucleation source is introduced in the high-temperature surface treatment process, so that a high-temperature nucleation point is formed on the surface of a sample, then a low-temperature buffer layer is grown again, a high-quality GaN epitaxial layer can be obtained, the dislocation density of the GaN epitaxial layer can be far lower than that of the GaN epitaxial layer grown by a conventional two-step method, and the influence of reaction chamber residue on growth can be reduced by using the method for growth.

Description

Novel method for growing GaN epitaxial layer on sapphire and GaN epitaxial layer
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for growing a GaN epitaxial layer on sapphire and the GaN epitaxial layer.
Background
In recent years, the preparation technology of GaN-based semiconductor materials has made great progress, which has vigorously promoted the development of visible light band Light Emitting Diodes (LEDs), Laser Diodes (LDs), and other optoelectronic devices. For optoelectronic devices, dislocations and defects in the material will largely determine the performance of the whole device, so how to obtain high-quality GaN epitaxial layers is always a major research issue in the development of GaN-based devices. Currently, GaN-based LEDs are epitaxially grown on a sapphire substrate, and since the two-step epitaxial growth method is proposed by Akasaki, Amano, Nakamura, and others, the crystal quality of GaN materials epitaxially grown on a sapphire substrate is greatly improved, but the dislocation density is much higher than that of GaAs and InP materials that are both III/V groups. Although GaN-based LEDs have been commercialized to reduce the effect of dislocations on the active region by growing a series of dislocation filter layers, it is still far from sufficient for LDs. Although most of current GaN-based LDs adopt GaN substrates for homoepitaxy, the GaN homoepitaxy substrate is expensive, the price of 2 inches is up to 20000 RMB, the GaN substrate cannot be directly used in optimization experiments at ordinary times, the growth conditions of the LD can be optimized only by relying on growth on sapphire, and when higher dislocation density exists in GaN materials, the judgment of experimental results by people can be influenced to a great extent by the existence of dislocation, so that the reduction of the dislocation density of GaN epitaxially grown on sapphire is also crucial for the optimization of the growth of a laser.
On the other hand, when the epitaxial growth of GaN is carried out on sapphire by adopting the two-step method, the quality of the grown GaN material is closely related to the state of equipment, particularly after the spray header or the reaction base of the equipment is replaced, the crystal quality of the material is far lower than that before the replacement by directly adopting the two-step method for growth, and the crystal quality of the material slowly returns to the state before the replacement after the material is grown for a period of time by using the same program.
In conclusion, how to further improve the crystal quality of the epitaxial GaN material on the sapphire on the basis of the two-step method and ensure the stability of epitaxial growth are very important, and the two problems are solved, so that the application of the GaN-based laser is further improved, and the experiment cost is reduced.
Disclosure of Invention
In view of the above, the present invention provides a method for growing a GaN epitaxial layer on sapphire and a GaN epitaxial layer, so as to at least partially solve at least one of the above-mentioned technical problems.
As an aspect of the present invention, there is provided a method of growing a GaN epitaxial layer on sapphire, the method comprising the steps of:
performing high-temperature nucleation treatment on the sapphire substrate to form a GaN nucleation center on the sapphire substrate;
growing a buffer layer on the sapphire substrate containing the GaN nucleation centers;
heating and annealing the buffer layer to form the buffer layer with nucleation islands;
and growing a GaN epitaxial layer on the buffer layer with the nucleation islands to obtain the GaN epitaxial layer on the sapphire.
As another aspect of the present invention, there is also provided a GaN epitaxial layer on sapphire prepared by the method as described above.
Based on the technical scheme, the present disclosure provides a method for growing a high-quality GaN epitaxial layer on sapphire, which has at least one or one part of the following beneficial effects:
performing high-temperature nucleation treatment on the sapphire substrate to form high-temperature nucleation points (namely GaN nucleation centers) on the surface of the sapphire substrate, wherein the quality of the generated high-temperature nucleation points is higher than that of the nucleation points generated when the sapphire substrate is grown on a low-temperature buffer layer in the prior art; then, carrying out low-temperature buffer and annealing treatment, and then growing a high-temperature GaN epitaxial layer; the dislocation density of the GaN epitaxial layer obtained by the method can be far lower than that of the conventional two-step growth, and the influence of reaction chamber residue on the growth of the GaN epitaxial layer can be reduced by the growth of the method; the application of the GaN-based laser can be further improved to a great extent, and the experiment cost is reduced.
Drawings
FIG. 1 is a flowchart of a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention;
FIG. 2 is a graph showing the temperature dependence of growth time in a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention;
FIG. 3 is a graph showing the relationship between TMGa and NH3 as a function of growth time in a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention;
fig. 4 is a XRD ω -scan graph of epitaxially growing high-quality GaN epitaxial layers (002) and (102) on the surface of sapphire in example 1 of the present invention.
Detailed Description
The invention provides a method for obtaining a high-quality GaN epitaxial layer on a sapphire surface, which is characterized in that a certain amount of TMGa and NH are introduced in the high-temperature treatment process of the sapphire surface3The method forms high-temperature nucleation points on the surface of the sapphire and then grows the buffer layer and the epitaxial layer, and the obtained GaN epitaxial layer has high crystal quality and low dislocation. Meanwhile, the method can greatly reduce the influence of MOCVD equipment growth residues on the growth of the GaN epitaxial layer, so that the epitaxy is more stable. The method is beneficial to further improving the application of the GaN-based laser and reducing the experiment cost.
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings.
As an aspect of the present invention, there is provided a method of growing a GaN epitaxial layer on sapphire, the method comprising the steps of:
performing high-temperature nucleation treatment on the sapphire substrate to form a GaN nucleation center on the sapphire substrate;
growing a buffer layer on the sapphire substrate containing the GaN nucleation center;
heating and annealing the buffer layer to form the buffer layer with the nucleation islands;
and growing a GaN epitaxial layer on the buffer layer with the nucleation islands to obtain the GaN epitaxial layer on the sapphire.
More specifically, in the embodiment of the present invention, in the step of performing the high temperature nucleation process on the sapphire substrate, the operation of the high temperature nucleation process includes: and heating the sapphire substrate at a high temperature, and introducing a high-temperature nucleation source of GaN to perform high-temperature nucleation treatment.
In the embodiment of the invention, in the step of carrying out high-temperature nucleation treatment on the sapphire substrate, the high-temperature nucleation source of GaN comprises TMGa and NH3Wherein, in the step (A),
the flow rate of TMGa is more than 3 mu mol/min and less than 20 mu mol/min;
NH3the flow rate of (A) is more than 100. mu. mol/min and less than 1000. mu. mol/min.
In the embodiment of the invention, in the step of carrying out high-temperature nucleation treatment on the sapphire substrate, the temperature of the high-temperature nucleation treatment is 1050-1100 ℃.
In the embodiment of the invention, in the step of carrying out high-temperature nucleation treatment on the sapphire substrate, the time of the high-temperature nucleation treatment is 3-10 min.
In the embodiment of the invention, in the step of growing the buffer layer, the temperature of the buffer layer is 500-600 ℃; the buffer layer comprises a GaN buffer layer or an A1N buffer layer; the thickness of the buffer layer is 20 nm-30 nm.
In the embodiment of the invention, in the step of heating and annealing the buffer layer, the heating rate of the heating and annealing treatment is 60-120 ℃/min; the size of the nucleation island is 400 nm-700 nm.
In the embodiment of the invention, in the step of growing the GaN epitaxial layer, the temperature for growing the GaN epitaxial layer is 1000-1100 ℃, and NH3And TMGa flow rates of 3mol/min to 20mol/min and 100mo, respectivelyl/min～1000mol/min。
As another aspect of the invention, the invention also provides a GaN epitaxial layer on sapphire, which is prepared by adopting the method.
In an embodiment of the invention, the threading dislocation density of the GaN epitaxial layer on sapphire is 3.71 x 107cm-3Edge dislocation density of 1.94 x 108cm-3。
The following will further describe a method for growing a GaN epitaxial layer on sapphire according to the present invention with reference to specific embodiments.
Example 1
FIG. 1 is a flow chart of a method for epitaxially growing a high quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention; FIG. 2 is a graph showing the temperature change with growth time in a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention; FIG. 3 is a schematic diagram showing MO sources (i.e., TMGa and NH) in a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to example 1 of the present invention3) A graph of variation with growth time; fig. 4 is a XRD ω -scan graph showing the epitaxial growth of the (002) plane and the (102) plane of the high-quality GaN epitaxial layer on the sapphire surface in example 1 of the present invention.
Referring to fig. 1, 2 and 3, a method for epitaxially growing a high-quality GaN epitaxial layer on a sapphire surface according to the present invention includes:
step S11: carrying out surface high-temperature treatment on the sapphire substrate, and introducing a certain amount of NH in the high-temperature treatment process3And TMGa is used as a high-temperature nucleation source to form nucleation centers on the surface of the sapphire.
Referring to fig. 2 and 3, the sapphire substrate was heated to increase the temperature to 1100 ℃, and then a TMGa source and NH were introduced3The time of the high temperature surface treatment process was 5 min. Introduced TMGa source and NH3Much less than the normal GaN long term flow. Wherein the flow rate of the introduced TMGa is required to be less than 20 mu mol/min and more than 3 mu mol/min. Into which NH is introduced3The flow rate of (A) is required to be less than 1000. mu. mol/min and more than 100. mu. mol/min. .
T introduced in the processMGa and NH3Can be decomposed at high temperature and react to generate GaN, and because the input amount is very small, the GaN can not be directly generated into an epitaxial layer, but small nucleation points can be formed on the surface of the sapphire substrate, and TMGa and NH are input3The method is equivalent to a high-temperature nucleation process, and the quality of the generated high-temperature nucleation points is far higher than that of the traditional nucleation points generated in the process of growing the low-temperature buffer layer due to high temperature.
Too high a flux will result in too many surface nucleation sites and thus a higher dislocation density in the final epitaxial layer, while low a flux will result in insufficient nucleation sites and thus a portion of the nucleation sites at low temperature will be needed to supplement the nucleation sites and thus increase the dislocation density in the final epitaxial layer. Comprehensively, the flow rate of the introduced TMGa needs to be less than 20 mu mol/min and more than 3 mu mol/min. Into which NH is introduced3The flow rate of (A) is required to be less than 1000. mu. mol/min and more than 100. mu. mol/min.
Step S12: growing a GaN buffer layer on the sapphire substrate at a low temperature;
referring to fig. 2 and 3, after high temperature treatment, the temperature is reduced to 550 ℃, and then a GaN buffer layer is grown on sapphire at a low temperature, wherein the reference value of the thickness of the grown GaN buffer layer is 20 nm-30 nm, and the growth temperature is 550 ℃. At this time, TMGa and NH were introduced3The flow rate is much larger than the amount introduced in step S11. Wherein NH3And the flow rates of TMGa were 0.267mol/min and 90. mu. mol/min, respectively.
In this embodiment, the thickness of the GaN buffer layer is 20 nm.
Step S13: heating and annealing to recrystallize the low-temperature buffer layer;
and (3) raising the temperature of the sample to 1050 ℃, wherein the temperature raising process is a recrystallization process, namely, the low-temperature buffer layer is recrystallized in the temperature raising process, when the temperature is raised to 1050 ℃, a series of nucleation islands are formed on the surface of the sapphire, the size and the density of the nucleation islands are closely connected with the step S11, and the step S11 can increase the size and reduce the density of the nucleation islands.
Step S14: and growing a GaN epitaxial layer.
Referring to FIGS. 2 and 3, when the temperature is raised to 1050 deg.CThen NH is introduced3And TMGa starts the growth of GaN epitaxial layer, NH introduced during the process3And the TMGa flow rate is also much larger than the amount passed in step S11. Wherein NH3And TMGa at a flow rate of 0.3mol/min and 90. mu. mol/min, respectively.
The crystal quality of the grown GaN epitaxial layer can be measured by XRD, and FIG. 4 is a XRD ω scan graph of a (002) plane and a (102) plane of a high-quality GaN epitaxial layer epitaxially grown on the surface of sapphire according to example 1 of the present invention, wherein the full width at half maximum of the (002) plane is 136 "and the full width at half maximum of the (102) plane is 191". The screw dislocation density is 3.71 x 10 according to the relation between the half width and the dislocation density7cm-3Edge dislocation density of 1.94 x 108cm-3. This value is much lower than for conventional two-step growth.
Comparative example 1
Comparative example 1 of the present invention is a conventional method for growing a GaN epitaxial layer by two-step method, and the temperature variation trend of the method is not changed from that of example 1, as shown in fig. 1, the main difference is that in step S11, NH3 and TMGa are not introduced into the method of comparative example 1, and only the temperature is raised to perform a high temperature treatment on the sapphire surface to remove some adsorbed atoms on the sapphire surface.
The growth method of comparative example 1 has exactly the same steps S12, S13, and S14 as example 1. The threading dislocation density of the GaN layer obtained by the conventional two-step GaN epitaxial layer growth method of comparative example 1 was approximately 5 x 108cm-3Left and right, edge dislocation density 7 x 108cm-3～8*108cm-3。
It should be noted that the preparation processes, reaction conditions, and the like in steps S12, S13, and S14 are well-established techniques in the art, and those skilled in the art can make adaptive settings according to actual needs.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for growing a GaN epitaxial layer on sapphire is characterized by comprising the following steps:
performing high-temperature nucleation treatment on the sapphire substrate to form a GaN nucleation center on the sapphire substrate;
growing a buffer layer on the sapphire substrate containing the GaN nucleation centers;
heating and annealing the buffer layer to form the buffer layer with nucleation islands;
and growing a GaN epitaxial layer on the buffer layer with the nucleation islands to obtain the GaN epitaxial layer on the sapphire.
2. The method according to claim 1, wherein in the step of subjecting the sapphire substrate to the high-temperature nucleation treatment, the operation of the high-temperature nucleation treatment comprises: and heating the sapphire substrate at a high temperature, and introducing a high-temperature nucleation source of GaN to perform high-temperature nucleation treatment.
3. The method of claim 2, wherein in the step of high temperature nucleation of the sapphire substrate, the high temperature nucleation source of GaN comprises TMGa and NH3Wherein, in the step (A),
the flow rate of TMGa is more than 3 mu mol/min and less than 20 mu mol/min;
NH3the flow rate of (A) is more than 100. mu. mol/min and less than 1000. mu. mol/min.
4. The method according to claim 2, wherein in the step of performing the high-temperature nucleation treatment on the sapphire substrate, the temperature of the high-temperature nucleation treatment is 1050 ℃ to 1100 ℃.
5. The method according to claim 2, wherein in the step of performing the high-temperature nucleation treatment on the sapphire substrate, the time of the high-temperature nucleation treatment is 3min to 10 min.
6. The method according to claim 1, wherein in the step of growing the buffer layer, the temperature of the buffer layer is 500-600 ℃; the buffer layer comprises a GaN buffer layer or an AlN buffer layer; the thickness of the buffer layer is 20 nm-30 nm.
7. The method according to claim 1, wherein in the step of annealing the buffer layer at an elevated temperature, the temperature-raising rate of the annealing treatment at an elevated temperature is 60 ℃/min to 120 ℃/min; the size of the nucleation island is 400 nm-700 nm.
8. The method of claim 1, wherein the step of growing the GaN epitaxial layer comprises growing the GaN epitaxial layer at 1000-1100 ℃ and NH3And the flow rates of TMGa are respectively 3-20 mol/min and 100-1000 mol/min.
9. A GaN epitaxial layer on sapphire prepared by the method of any one of claims 1 to 8.
10. The GaN-on-sapphire epitaxial layer of claim 9, wherein the GaN-on-sapphire epitaxial layer has a threading dislocation density of 3.71 x 107cm-3Edge dislocation density of 1.94 x 108cm-3。
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