CN114574959B - Nitride epitaxial layer preparation method and semiconductor epitaxial wafer thereof - Google Patents

Nitride epitaxial layer preparation method and semiconductor epitaxial wafer thereof Download PDF

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CN114574959B
CN114574959B CN202210088147.5A CN202210088147A CN114574959B CN 114574959 B CN114574959 B CN 114574959B CN 202210088147 A CN202210088147 A CN 202210088147A CN 114574959 B CN114574959 B CN 114574959B
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闫其昂
王国斌
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Jiangsu Third Generation Semiconductor Research Institute Co Ltd
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    • 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
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Abstract

The invention discloses a preparation method of a nitride epitaxial layer and a semiconductor epitaxial wafer thereof, which comprises the following steps: providing a substrate; growing a buffer layer on the substrate, wherein the buffer layer comprises a nitride buffer layer and an oxygen-containing buffer layer grown by periodically and cyclically alternately switching an MO source and an oxygen-containing MO source as precursor materials; a nitride epitaxial layer is grown on the buffer layer. According to the invention, the oxygen-containing buffer layer is grown through an oxygen-containing MO source process, on one hand, the in-situ growth of the oxygen-containing buffer layer has good lattice mismatch relaxation, the lattice adaptation is relieved, the stress of a substrate and an epitaxial layer is released, a high-quality gallium nitride epitaxial layer with low dislocation density can be obtained, and meanwhile, the distribution uniformity and nucleation density of oxygen-containing buffer crystal grains are improved due to the adoption of alternate growth, and a high-quality nitride epitaxial layer is obtained; on the other hand, the invention has simple technical process, reduces the pollution risk in the transfer process of the substrate and the epitaxial layer, has good repeatability and is beneficial to large-scale production.

Description

Nitride epitaxial layer preparation method and semiconductor epitaxial wafer thereof
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method of a nitride epitaxial layer and a semiconductor epitaxial wafer thereof.
Background
The wide-bandgap semiconductor material GaN has excellent physical and chemical properties of high breakdown field strength, high thermal conductivity, high electron saturation migration rate and the like, and has wide application prospect in blue-green light LEDs, photodetectors and high-temperature high-frequency high-power devices.
The existing mature MOCVD epitaxy technology for preparing GaN materials is an epitaxy technology for growing on a heterogeneous substrate, and the crystal materials grown by epitaxy have high dislocation density and high stress due to lattice and thermal expansion mismatch between the substrate and the epitaxy layer, so that the phenomena of warping and cracking and the like are easy to occur, the working efficiency and the service life of the device are influenced, and the application of the device in the field of semiconductor electronics is restricted.
In the MOCVD epitaxial technology, an MO source precursor material is a key material and a dopant of an epitaxially grown semiconductor compound, doping and defects are required to be strictly controlled to obtain a high-quality epitaxial layer, generally, the higher the purity of an MO source is, the less impurities are, the higher the product quality is, the introduction of impurities is avoided as much as possible in the epitaxial growth process, in the MOCVD epitaxial growth process, O is used as an unintended impurity source, deep level defects are introduced into a nitride epitaxial layer, yellow band luminescence existing in nitride is one of the judgment of poor growth quality of the nitride epitaxial layer, the deep level defects are generally considered to be related to O, the introduction of epitaxial growth O impurities is required to be strictly controlled, in the current process of synthesizing the MO source precursor material, in order to obtain a high-purity MO precursor, the MO source precursor material is required to be purified, the impurities such as O are removed, however, the purification process has high requirements on equipment tightness, poor safety, potential safety hazards exist and the like, the preparation cost of the MO source is increased, and therefore the quality of the MO source precursor material is most good, whether the product obtained by using the MO source is good or not, the requirements of the product obtained by using the MO source are basically met, and the requirements of the photoelectric device are low in cost.
Disclosure of Invention
The invention aims to provide a preparation method of a nitride epitaxial layer and a semiconductor epitaxial wafer thereof, which improve the performance of a nitride semiconductor device with a heteroepitaxial substrate.
In order to solve the technical problems, the invention provides a preparation method of a nitride epitaxial layer, which comprises the following steps:
s1: providing a substrate;
s2: growing a buffer layer on the substrate, wherein the buffer layer comprises a nitride buffer layer and an oxygen-containing buffer layer grown by periodically and cyclically alternately switching an MO source and an oxygen-containing MO source as precursor materials;
s3: a nitride epitaxial layer is grown on the buffer layer.
As a further improvement of the present invention, the oxygen-containing MO source includes one or more of oxygen-containing trimethylgallium, oxygen-containing triethylgallium, oxygen-containing trimethylaluminum, and oxygen-containing triethylaluminum.
As a further improvement of the present invention, the purity of the MO source is 99.9999% or more, and the oxygen content of the oxygen-containing MO source is 5-50000ppm.
As a further improvement of the present invention, the oxygen-containing buffer layer is an aluminum oxynitride layer or a gallium oxynitride layer, and the nitride buffer layer is an aluminum nitride layer or a gallium nitride layer.
As a further improvement of the present invention, the O and gallium bonds in the oxygen-containing trimethylgallium or triethylgallium are linked, or the O and C bonds are linked; the oxygen-containing trimethylgallium or triethylgallium is formed by OH groups to replace methyl and Ga bonds to link, or O bonds to link two Ga bonds, or O to replace methyl H;
o and aluminum bonds in the oxygen-containing trimethylaluminum or triethylaluminum are linked, or O and C bonds are linked; the oxygen-containing trimethylaluminum or triethylaluminum is formed by substituting OH groups for methyl and aluminum bond linkage, or by linking two Al bonds for O bonds, or by substituting O for methyl H.
As a further improvement of the invention, the growth condition of the step S2 is that the switching period of the MO source and oxygen-containing MO source precursor materials is 1-40 periods under the conditions of the temperature of 500-1000 ℃ and the growth pressure of 50-650torr, and the switching period of the MO source and oxygen-containing MO source precursor materials is inversely related to the thickness of the epitaxial layer of the nitride.
As a further improvement of the invention, the growth condition of the step S3 is that a nitride epitaxial layer with the thickness of 1 mu m to 10 mu m is grown at the temperature of 1000 ℃ to 1200 ℃ and the growth pressure of 50torr to 650 torr.
As a further improvement of the present invention, the growth thickness of the oxygen-containing buffer layer is 2-5nm, and the growth thickness of the nitride buffer layer is 3-10nm; wherein the thickness of the nitride buffer layer is greater than the thickness of the oxygen-containing buffer layer.
A nitride semiconductor epitaxial wafer comprises a nitride epitaxial layer and an epitaxial structure arranged on the nitride epitaxial layer, wherein the nitride epitaxial layer is prepared by the method.
As a further improvement of the present invention, the epitaxial structure is an LED epitaxial structure comprising an n-nitride layer, a nitride multiple quantum well light emitting layer, a p-type nitride electron blocking layer and a p-type nitride layer sequentially arranged in a direction away from the substrate surface, wherein the nitride multiple quantum well light emitting layer is a nitride quantum well layer and a nitride quantum barrier layer alternately arranged.
The preparation method of the LED epitaxial structure comprises the following steps:
growing an n-type nitride layer of 1-4 μm on the nitride epitaxial layer, wherein the growth temperature is 1000-1200deg.C, the growth pressure is 100-400torr, and the doping concentration of Si is 1×10 18 -1×10 19 cm -3 The growth atmosphere is H 2 An atmosphere;
growing a nitride multi-quantum well light-emitting layer on the n-type nitride layer, wherein the nitride multi-quantum well light-emitting layer is a nitride quantum well layer and a nitride quantum barrier layer which are periodically and repeatedly and alternately grown under the condition of the growth pressure of 100-400torr, the light-emitting layer is repeatedly and periodically 1-20, the thickness of the nitride quantum well layer is 1-6nm, the growth temperature is 700-900 ℃, the thickness of the nitride barrier is 6-20nm, and the growth temperature is 750-1000 ℃;
growing a p-nitride electron blocking layer of 10-50nm on the nitride multiple quantum well luminescent layer, wherein the growth atmosphere is N under the conditions of the growth temperature of 800-1100 ℃ and the growth pressure of 50-200torr 2 An atmosphere;
growing a p-nitride layer of 20-200nm on the p-nitride electron blocking layer, wherein the growth temperature is 900-1100 ℃, the growth pressure is 200-400torr, and the Mg doping concentration is 1×10 19 -5×10 20 cm -3 The growth atmosphere is switched to H 2 An atmosphere.
The invention has the beneficial effects that: according to the invention, the buffer layer is grown by periodically and circularly alternately switching the MO source precursor material and the oxygen-containing MO source precursor material, so that lattice mismatch relaxation of the oxygen-containing buffer layer on lattice mismatch of the substrate and the nitride epitaxial layer can be utilized, the lattice mismatch of the substrate and the nitride epitaxial layer is relieved, the stress of the substrate and the nitride epitaxial layer is released, meanwhile, due to the adoption of alternate growth, the distribution uniformity and nucleation density of oxygen-containing buffer crystal grains are improved by utilizing the difference between the surface energy of the substrate and the surface energy of the nitride buffer layer, and a high-quality nitride epitaxial layer is obtained, and on the other hand, by switching the oxygen-containing MO source precursor material, oxygen sources are not introduced through other equipment, the growth buffer layers such as CVD (chemical vapor deposition), MBE (molecular oxygen enhanced) and the like can be prevented from being transferred to MOCVD equipment, the pollution risk of the substrate and the epitaxial layer transfer process is reduced, the repeatability is good, and large-scale production is facilitated.
Drawings
FIG. 1 is a flow chart of the preparation of nitride epitaxial layers according to the present invention;
FIG. 2 is a graph showing the effect of the surface of the epitaxial layer OM according to the first embodiment of the present invention;
FIG. 3 is a graph showing the effect of the surface of the epitaxial layer OM prepared in comparative example one of the present invention;
FIG. 4 is a graph showing the effect of the surface of the epitaxial layer OM prepared in comparative example II of the present invention;
FIG. 5 is a graph showing the effect of the surface of the epitaxial layer OM prepared in the second embodiment of the present invention;
FIG. 6 is a graph showing the effect of the surface of the epitaxial layer OM prepared in comparative example III of the present invention;
FIG. 7 is a graph showing the effect of the surface of the epitaxial layer OM prepared in the third embodiment of the present invention;
FIG. 8 is a graph showing the effect of the surface of the epitaxial layer OM prepared in comparative example four of the present invention;
fig. 9 is a schematic structural diagram of a gallium nitride-based LED epitaxial wafer prepared in embodiment four of the present invention;
the reference numerals in the figures illustrate: 1. a sapphire substrate; 2. a buffer layer; 21. an oxygen-containing buffer layer; 22. a nitride buffer layer; 3. a gallium nitride epitaxial layer; 4. an nGaN layer; 5. a multi-quantum well light emitting layer; 51. an InGaN quantum well layer; 52. a GaN quantum barrier layer; 6. a pAlGaN electron blocking layer; 7. pGaN layer.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
As shown in fig. 1, the invention provides a method for preparing a nitride epitaxial layer, which comprises the following steps:
s1: providing a substrate;
s2: growing a buffer layer on the substrate, wherein the buffer layer comprises a nitride buffer layer and an oxygen-containing buffer layer grown by periodically and cyclically alternately switching an MO source and an oxygen-containing MO source as precursor materials;
s3: a nitride epitaxial layer is grown on the buffer layer.
Specifically, in the MOCVD reaction chamber, the preparation method comprises the following steps:
1) Providing a substrate, and H under the conditions of the temperature of 900-1200 ℃ and the growth pressure of 50-650torr 2 Performing atmosphere heat treatment for 1-10 min;
2) Growing a buffer layer of 10-100 nm on a substrate at the temperature of 500-1000 ℃ and the growth pressure of 50-650torr, wherein: the buffer layer growth comprises the steps of:
growing an oxygen-containing buffer layer with the thickness of 2-5nm, wherein a source required for growth is an oxygen-containing MO source;
growing a nitride buffer layer with the thickness of 3-10nm, wherein an MO source required by growth is a high-purity MO source;
the thickness of the nitride buffer layer is larger than that of the oxygen-containing buffer layer, so that the distribution uniformity and nucleation density of oxygen-containing buffer crystal grains are improved;
repeating the alternately growing oxygen-containing buffer layer and nitride buffer layer with a repetition period of 1-40 to form a buffer layer;
the main influence of the cycle period is the thickness of the buffer layer, in the range of 1-10 mu m of the thickness of the nitride epitaxial layer, the number of the cycle period is gradually reduced along with the increase of the thickness of the nitride epitaxial layer in a specific practical process, specifically, the thickness of the epitaxial layer is increased to 10 mu m from 1 mu m, the cycle period data is reduced to 1 mu m from 40, the cycle period is overlarge (> 40) at the end of the growth of the buffer layer, nucleation centers are formed on the surface of a substrate too densely, dislocation is not changed in the growth process of the nitride epitaxial layer so as to extend into the nitride epitaxial layer, and the crystal quality of the nitride epitaxial layer is reduced;
3) And growing a nitride epitaxial layer with the thickness of 1-10 mu m on the oxygen-containing buffer layer at the temperature of 1000-1200 ℃ and the growth pressure of 50-650 torr.
According to the invention, on the basis of a basic process, O is introduced into the buffer layer by adopting an oxygen-containing MO source precursor material, and because the radius of O atoms is smaller than that of N atoms, the overall lattice constant of the introduced buffer layer is reduced, so that the stress between the substrate and the buffer layer is increased, the stress is released between the substrate and the buffer layer in advance before the growth of the nitride epitaxial layer, so that the stress during the growth of the nitride epitaxial layer is reduced, meanwhile, the oxygen-containing MO source precursor material is utilized for growth, the precursor material is not required to be further purified and removed, the production cost is reduced on the premise of meeting the requirement of an epitaxial process, and furthermore, oxygen sources are not required to be introduced through other equipment, so that the growth buffer layer such as CVD (chemical vapor deposition), MBE (molecular oxygen beam) and the like can be prevented from being transferred to MOCVD equipment, the pollution risk in the transfer process of the substrate and the epitaxial layer is reduced, the repeatability is good, and mass production is facilitated.
The sapphire substrate is usually used for heteroepitaxial growth of GaN materials, subsurface damage exists on the surface of the sapphire substrate after chemical mechanical polishing, so that the same crystal face on the surface of the sapphire is anisotropic, and O atoms are unevenly distributed on the sapphire substrate.
Further, the oxygen-containing MO source comprises one or more than two of oxygen-containing Trimethylgallium (TMG), oxygen-containing Triethylgallium (TEG), oxygen-containing Trimethylaluminum (TMAL) and oxygen-containing Triethylaluminum (TEAL), and the oxygen-containing MO source is combined according to the principle: o in oxygen-containing Trimethylgallium (TMG) or Triethylgallium (TEG) can be linked with gallium bonds or C bonds, can be in a single-molecule structure, a linear structure or a ring or cluster structure, can be formed by linking OH groups with methyl and Ga bonds or linking O bonds with two Ga bonds or O replaces methyl H; o in the oxygen-containing Trimethylaluminum (TMAL) or Triethylaluminum (TEAL) can be linked with an aluminum bond, can be linked with a C bond, can be in a single molecular structure, a linear structure or a ring or cluster structure, can be formed by linking an OH group with an aluminum bond instead of methyl, and can be formed by linking two Al bonds with an O bond or O instead of methyl H.
Further, the MO source purity is 99.9999% or higher, and the oxygen content of the oxygen-containing MO source is 5 to 50000ppm, taking care that the oxygen content is not too high to affect the properties of the grown epitaxial layer.
Further, the oxygen-containing buffer layer may be an aluminum oxynitride layer (AlON) or a gallium oxynitride layer (GaON), and the nitride buffer layer is an aluminum nitride layer (AlN) or a gallium nitride layer (GaN).
Further, based on the above principle, the nitride epitaxial layer of the present invention at least comprises Al x In y Ga 1-x-y And an N nitride epitaxial layer, wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and x+y is more than or equal to 0 and less than or equal to 1.
The invention also provides a nitride semiconductor epitaxial wafer, which comprises a nitride epitaxial layer and an epitaxial structure arranged on the nitride epitaxial layer, wherein the nitride epitaxial layer is prepared by the method.
For example, the invention provides a nitride LED epitaxial wafer, which comprises a gallium nitride epitaxial layer and an epitaxial structure arranged on the gallium nitride epitaxial layer, wherein the gallium nitride epitaxial layer is prepared by the method, and the method comprises the following steps of:
the LED epitaxial structure comprises an nGaN layer, a nitride multi-quantum well light-emitting layer, a pAlGaN electron blocking layer and a pGaN layer which are sequentially arranged along the direction far away from the surface of the substrate, wherein the nitride multi-quantum well light-emitting layer is an InGaN quantum well layer and a GaN quantum barrier layer which are alternately arranged.
Specifically, the preparation method of the LED epitaxial structure comprises the following steps:
growing a 1-4 μm nGaN layer on the GaN epitaxial layer, wherein the growth temperature is 1000-1200deg.C, the growth pressure is 100-400torr, and the doping concentration of Si is 1×10 18 -1×10 19 cm -3 Ga source required by growth is TMG source, and growth atmosphere is H 2 An atmosphere;
an InGaN/GaN multi-quantum well luminescent layer is grown on the nGaN layer, wherein the InGaN/GaN multi-quantum well luminescent layer is an InGaN quantum well layer and a GaN quantum barrier layer which are periodically and repeatedly and alternately grown under the condition of the growth pressure of 100-400torr, the repetition period of the luminescent layer is 1-20, the thickness of the InGaN quantum well layer is 1-6nm, the growth temperature is 700-900 ℃, the thickness of the GaN barrier is 6-20nm, and the growth temperature is 750-1000 ℃;
growing a pAlGaN electron blocking layer of 10-50nm on the InGaN/GaN multiple quantum well luminous layer, wherein the Ga source required by growth is a TMG source, the Al source is TMAL, and the growth atmosphere is N at the growth temperature of 800-1100 ℃ and the growth pressure of 50-200torr 2 An atmosphere;
growing a pGaN layer of 20-200nm on the pAlGaN electron blocking layer, wherein the growth temperature is 900-1100 ℃, the growth pressure is 200-400torr, and the Mg doping concentration is 1 multiplied by 10 19 -5×10 20 cm -3 Ga source required by growth is TMG source, growth atmosphere is switched to H 2 An atmosphere.
Example 1
In this example, gaN buffer layers were alternately grown by an oxygen-containing TMG source and a TMG source, and gallium nitride epitaxial layers were prepared as comparative examples with comparative examples 1 and 2, respectively, in which all preparation environments were placed in a MOCVD reaction chamber, to illustrate the effects.
In this embodiment, the gallium nitride epitaxial layer is prepared by alternately growing a GaON and GaN buffer layer by an oxygen-containing TMG source and a TMG source, and includes the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, periodically and alternately growing a GaON buffer layer with the thickness of 3nm and a GaN buffer layer with the thickness of 5nm for 20 periods at the temperature of 540 ℃ and the growth pressure of 300torr, wherein a Ga source required for growing the GaON buffer layer is an oxygen-containing TMG source, the growing GaN buffer layer is switched into the TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, an unintentional doped GaN layer with a thickness of 3 mu m is grown, the required Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
Comparative example 1: preparing a gallium nitride epitaxial layer by growing a GaN buffer layer by a TMG source with an oxygen content of less than 1ppm, comprising the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, growing a 20nm GaN buffer layer at 540 ℃ under the condition of a growth pressure of 300torr, wherein a Ga source required by growth is a TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the GaN buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, an unintended doped GaN layer with 3 mu m is grown, the required Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
As shown in fig. 2 and 3, the OM surfaces of the unintentionally doped GaN epitaxial layers prepared in the first embodiment and the comparative embodiment 1 respectively, it can be seen that the OM surface is relatively smooth, and the OM surface roughness in the comparative embodiment 1 has more small particle distribution, because GaON has good lattice mismatch relaxation as a buffer layer, relieves lattice adaptation, releases stress of the sapphire substrate and the epitaxial layer, and simultaneously, by cyclically growing the buffer layer, the stress of each layer is different in surface energy, the nucleation point distribution is also different, the nucleation point of the oxygen-containing buffer layer is more uniform as a whole, the surface of the subsequent GaN epitaxial layer is more smooth, the crystal quality of the nitride layer is improved, and simultaneously, the epitaxial growth process window is enlarged, and the process stability is improved.
Comparative example 2: the gallium nitride epitaxial layer is prepared by growing a GaON buffer layer by only adopting an oxygen-containing TMG source, and comprises the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, under the conditions of the temperature of 540 ℃ and the growth pressure of 300torr, adopting an oxygen-containing TMG source to grow a GaON buffer layer with the thickness of 160nm, wherein the growth atmosphere is N 2 An atmosphere;
3) On the buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, an unintentional doped GaN layer with a thickness of 3 mu m is grown, the required Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
As shown in fig. 4, it is seen from the OM surface that only the grown GaON buffer layer exhibits large black dot agglomeration, and the GaON buffer layer cannot alleviate lattice adaptation, because it may be that GaOH nucleation density is low and nucleation center distribution uniformity is poor, a flat epitaxial surface cannot be formed during the two-dimensional growth of the GaN epitaxial layer, and dislocations extend to the GaN epitaxial layer surface.
Example two
The present embodiment is to alternately grow a GaON and GaN buffer layer and a pure TMG source growth buffer layer with an oxygen content of less than 1ppm by using an oxygen-containing TMG source and a TMG source to prepare gallium nitride epitaxial layers respectively as comparative description effects, and is different from the first embodiment in that the growth temperature of preparing gallium nitride epitaxial layers is different, wherein all preparation environments are placed in an MOCVD reaction chamber.
In this embodiment, the gallium nitride epitaxial layer is prepared by alternately growing a GaON and GaN buffer layer by an oxygen-containing TMG source and a TMG source, and includes the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, periodically and alternately growing a GaON buffer layer with the thickness of 3nm and a GaN buffer layer with the thickness of 5nm for 20 periods at the temperature of 540 ℃ and the growth pressure of 300torr, wherein a Ga source required by GaON growth is an oxygen-containing TMG source, the GaN buffer layer is switched into the TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the buffer layer, under the conditions of 1020 ℃ and 200torr of growth pressure, an unintentional doped GaN layer with a thickness of 3 mu m is grown, the Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
Comparative example 3: preparing a gallium nitride epitaxial layer by growing a GaN buffer layer by a TMG source with an oxygen content of less than 1ppm, comprising the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, growing a 20nm GaN buffer layer at 540 ℃ under the condition of a growth pressure of 300torr, wherein a Ga source required by growth is a TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the GaN buffer layer, under the conditions of 1020 ℃ and 200torr of growth pressure, an unintentional doped GaN layer with a thickness of 3 mu m is grown, the Ga source is a TMG source, and the growth atmosphere isH 2 An atmosphere.
As shown in fig. 5 and 6, which are respectively the surfaces of the unintentionally doped GaN epitaxial layers OM prepared in the second embodiment and the comparative example 3, the growth temperature of the GaN epitaxial layer is reduced to approximately 1000 ℃, and as can be seen from the OM surface, the surface of the second embodiment is still relatively flat and smooth, while a large number of black point defects appear on the surface of the comparative example 3.
Example III
The present embodiment is different from the first embodiment in that the growth temperature of the gallium nitride epitaxial layer is different, and all the preparation environments are placed in the MOCVD reaction chamber.
In this embodiment, the gallium nitride epitaxial layer is prepared by alternately growing a GaON and GaN buffer layer by an oxygen-containing TMG source and a TMG source, and includes the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, periodically and alternately growing a GaON buffer layer with the thickness of 3nm and a GaN buffer layer with the thickness of 5nm for 20 periods at the temperature of 540 ℃ and the growth pressure of 300torr, wherein a Ga source required by GaON growth is an oxygen-containing TMG source, the GaN buffer layer is switched into the TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the buffer layer, under the conditions of 1200 ℃ and 200torr of growth pressure, an unintentional doped GaN layer with a thickness of 3 mu m is grown, the Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
Comparative example 4: preparing a gallium nitride epitaxial layer by growing a GaN buffer layer by a TMG source with an oxygen content of less than 1ppm, comprising the following steps:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, growing a 20nm GaN buffer layer at 540 ℃ under the condition of a growth pressure of 300torr, wherein a Ga source required by growth is a TMG source, and the growth atmosphere is N 2 An atmosphere;
3) On the GaN buffer layer, the temperature is 1200 ℃ and the growth pressure is highUnder the condition of a force of 200torr, a 3 mu m unintentional doped GaN layer is grown, a required Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere.
As shown in fig. 7 and 8, which are respectively the OM surfaces of the unintentionally doped GaN layers prepared in the third embodiment and the comparative example 3, the growth temperature of the GaN epitaxial layer was raised to 1200 ℃, and the OM surface of the third embodiment was still relatively smooth, while the surface of the comparative example 3 showed a lot of high Wen Huahen defects.
As can be seen from examples one, two, three and 1, 2, 3 and 4, gaON has good lattice mismatch relaxation, relieves lattice adaptation, releases stress of sapphire substrate and epitaxial layer, and simultaneously, by cyclically growing the buffer layer, the stress of each layer is different in surface energy, nucleation point distribution is different, nucleation uniformity can be improved by introducing O, and the surface of the subsequent GaN epitaxial layer can be flatter, so that the quality of nitride layer crystal is improved, the epitaxial growth process window is enlarged, and the process stability is improved.
Example IV
In this embodiment, based on the AlON and AlN buffer layers alternately grown by the oxygen-containing TMAl source and the gallium nitride epitaxial layers prepared by the growth buffer layers of comparative example 5 and comparative example 6, the LED epitaxial wafers were prepared respectively, and finally the quality effects of the gallium nitride epitaxial layers prepared by the different buffer layers were illustrated by the effects of the LED epitaxial wafers, wherein all the preparation environments were placed in the MOCVD reaction chamber.
According to the embodiment, the LED epitaxial wafer is finally prepared by alternately growing AlON and AlN buffer layers of an oxygen-containing TMAL source and a TMAL source, and the method comprises the following steps of:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrate, periodically and alternately growing AlON buffer layers with the thickness of 3nm and AlN buffer layers with the thickness of 5nm for 20 periods at the temperature of 540 ℃ and the growth pressure of 300torr, wherein an Al source required for growing AlON is an oxygen-containing TMAL source, the Al source switched by the AlN buffer layers is the TMAL source, the purity is more than or equal to 99.9999%, the oxygen content is 5-50000ppm, and the growth atmosphere is N 2 An atmosphere;
3) On AlON buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, 3 mu m unintended doped GaN layer is grown, the required Ga source is TMG source, and the growth atmosphere is H 2 An atmosphere;
4) Growing 3 μm nGaN layer on undoped GaN layer at 1060 deg.C under 200torr of growth pressure, and doping concentration of Si is 8×10 18 cm -3 Ga source required by growth is TMG source, and growth atmosphere is H 2 An atmosphere;
5) Growing an InGaN/GaN multi-quantum well luminescent layer on the nGaN layer at 750 ℃ under the condition of the growth pressure of 250torr, wherein the InGaN/GaN multi-quantum well luminescent layer is an InGaN quantum well layer and a GaN quantum barrier layer which are periodically and repeatedly and alternately grown, the luminescent layer has a repetition period of 9, the thickness of the InGaN quantum well layer is 3nm, and the thickness of the GaN barrier is 12nm;
6) On the InGaN/GaN quantum well luminous layer, a pAlGaN electron blocking layer with the thickness of 25nm is grown under the conditions of the temperature of 850 ℃ and the growth pressure of 200torr, the Ga source required by growth is TMG source, the Al source is TMAL, and the growth atmosphere is N 2 An atmosphere;
7) Growing 150nm pGaN layer on pAlGaN electron blocking layer at 930 deg.C and 200torr growth pressure, with Mg doping concentration of 5×10 19 cm -3 Ga source required by growth is TMG source, growth atmosphere is switched to H 2 And (5) atmosphere, and finishing the preparation of the LED epitaxial wafer.
Based on the above steps, an LED epitaxial wafer as shown in fig. 8 was prepared, the LED epitaxial wafer comprising a sapphire substrate 1, a buffer layer 2, a GaN layer 3, and an n GaN layer 4, a multiple quantum well light-emitting layer 5, a pAlGaN electron blocking layer 6 and a pGaN layer 7 sequentially disposed in a direction away from the surface of the sapphire substrate 1, wherein the multiple quantum well light-emitting layer 5 is an InGaN quantum well layer 51 and a GaN quantum barrier layer 52 alternately disposed, and the buffer layer 2 is an oxygen-containing buffer layer 21 and a nitride buffer layer 22 alternately grown.
Comparative example 5: and finally preparing the LED epitaxial wafer by growing an AlN buffer layer through a TMAL source without oxygen, wherein the method comprises the following steps of:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) On a sapphire substrateGrowing an AlN buffer layer with the thickness of 20nm at the temperature of 540 ℃ and the growth pressure of 300torr, wherein an Al source required by growth is a TMAL source, and the growth atmosphere is N 2 An atmosphere;
3) On the AlN buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, an unintended doped GaN layer with a thickness of 3 mu m is grown, the required Ga source is a TMG source, and the growth atmosphere is H 2 An atmosphere;
4) Growing 3 μm nGaN layer on undoped GaN layer at 1060 deg.C under 200torr of growth pressure, and doping concentration of Si is 8×10 18 cm -3 Ga source required by growth is TMG source, and growth atmosphere is H 2 An atmosphere;
5) Growing an InGaN/GaN multi-quantum well luminescent layer on the nGaN layer at 750 ℃ under the condition of the growth pressure of 250torr, wherein the InGaN/GaN multi-quantum well luminescent layer is an InGaN quantum well layer and a GaN quantum barrier layer which are periodically and repeatedly and alternately grown, the luminescent layer has a repetition period of 9, the thickness of the InGaN quantum well layer is 3nm, and the thickness of the GaN barrier 71 is 12nm;
6) On the InGaN/GaN quantum well luminous layer, a pAlGaN electron blocking layer with the thickness of 25nm is grown under the conditions of the temperature of 850 ℃ and the growth pressure of 200torr, the Ga source required by growth is TMG source, the Al source is TMAL, and the growth atmosphere is N 2 An atmosphere;
7) Growing 150nm pGaN layer on pAlGaN electron blocking layer at 930 deg.C and 200torr growth pressure, with Mg doping concentration of 5×10 19 cm -3 Ga source required by growth is TMG source, growth atmosphere is switched to H 2 And (5) atmosphere, and finishing the preparation of the LED epitaxial wafer.
The following table is the LED epitaxial wafer property data prepared for example four and comparative example 5:
as can be seen from the table, the AlON is used as a buffer layer, has good lattice mismatch relaxation, relieves lattice adaptation and thermal adaptation, releases stress of a sapphire substrate and an epitaxial layer, simultaneously, by circularly growing the buffer layer, the stress of each layer is different in surface energy, nucleation points are distributed differently, the oxygen-containing buffer layer is more uniform in nucleation points on the whole, the surface of a subsequent GaN epitaxial layer is smoother, so that the crystal quality of a nitride layer is improved, the stress of a nitride quantum well is reduced, the uniformity of light emitting wavelength is improved, the excitation effect of the quantum well light emitting layer is reduced, the recombination probability of electron and hole radiation is increased, the brightness of an LED is improved, and meanwhile, the GaN epitaxial layer has better droop performance under a high-current test condition.
Comparative example 6: and finally preparing the LED epitaxial wafer by adopting a Physical Vapor Deposition (PVD) sputtering period to grow a buffer layer, wherein the method comprises the following steps of:
1) Providing a sapphire substrate, H 2 Performing atmosphere heat treatment for 5min;
2) Periodically and alternately growing an AlON buffer layer with the thickness of 3nm and an AlN buffer layer with the thickness of 5nm on a sapphire substrate by adopting Physical Vapor Deposition (PVD) sputtering under the conditions of the temperature of 540 ℃ and the growth pressure of 300 torr;
3) On AlON buffer layer, under the conditions of 1080 ℃ and 200torr of growth pressure, 3 mu m unintended doped GaN layer is grown, the required Ga source is TMG source, and the growth atmosphere is H 2 An atmosphere;
4) Growing 3 μm nGaN layer on undoped GaN layer at 1060 deg.C under 200torr of growth pressure, and doping concentration of Si is 8×10 18 cm -3 Ga source required by growth is TMG source, and growth atmosphere is H 2 An atmosphere;
5) Growing an InGaN/GaN multi-quantum well luminescent layer on the nGaN layer at 750 ℃ under the condition of the growth pressure of 250torr, wherein the InGaN/GaN multi-quantum well luminescent layer is an InGaN quantum well layer and a GaN quantum barrier layer which are periodically and repeatedly and alternately grown, the luminescent layer has a repetition period of 9, the thickness of the InGaN quantum well layer is 3nm, and the thickness of the GaN barrier is 12nm;
6) On the InGaN/GaN quantum well luminous layer, a pAlGaN electron blocking layer with the thickness of 25nm is grown under the conditions of the temperature of 850 ℃ and the growth pressure of 200torr, the Ga source required by growth is TMG source, the Al source is TMAL, and the growth atmosphere is N 2 An atmosphere;
7) Growing 150nm pGaN layer on pAlGaN electron blocking layer at 930 deg.C and 200torr growth pressure, with Mg doping concentration of 5×10 19 cm -3 Ga source required by growth is TMG source, growth atmosphere is switched to H 2 And (5) atmosphere, and finishing the preparation of the LED epitaxial wafer.
The tested epitaxy data are basically equivalent to those of the fourth embodiment, but comparative example 6 has larger fluctuation of the continuous growth (run-to-run) leakage performance, the average leakage of continuous 5 runs is increased by 0.1 mu A, the yield of the leakage performance is lower by 5%, and the anti-static discharge ESD performance is lower by 3%, because the epitaxial layer particle pollution forms a leakage channel in the process of transferring to the MOCVD reaction cavity after PVD sputtering.
Further, based on the above principle, the present invention can also grow other gallium nitride-based semiconductor epitaxial wafers, such as HEMT, FET, LD, HBT epitaxial structures and the like.
The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention. The protection scope of the invention is subject to the claims.

Claims (7)

1. A preparation method of a nitride epitaxial layer is characterized by comprising the following steps of: the method is realized in an MOCVD reaction cavity, and comprises the following steps:
s1: providing a substrate;
s2: growing a buffer layer on the substrate at the temperature of 500-1000 ℃ and under the growth pressure of 50-650torr, wherein the buffer layer comprises a nitride buffer layer and an oxygen-containing buffer layer which are grown by alternately switching an MO source and an oxygen-containing MO source as precursor materials in a periodic cycle, the oxygen-containing buffer layer is an aluminum oxynitride layer or a gallium oxynitride layer, the nitride buffer layer is an aluminum nitride layer or a gallium nitride layer, and the thickness of the nitride buffer layer is larger than that of the oxygen-containing buffer layer;
s3: growing a nitride epitaxial layer on the buffer layer at the temperature of 1000-1200 ℃ and under the growth pressure of 50-650 torr;
wherein the oxygen-containing MO source comprises one of oxygen-containing trimethylgallium, oxygen-containing triethylgallium, oxygen-containing trimethylaluminum and oxygen-containing triethylaluminum, the purity of the MO source is more than or equal to 99.9999 percent, and the oxygen content of the oxygen-containing MO source is 5-50000ppm; when the MO source and the oxygen-containing MO source are switched as precursor materials each time, the stress between the substrate and the nitride buffer layer is different, so that nucleation centers of the oxygen-containing buffer layer distributed at different positions are formed on each nitride buffer layer, and the nucleation points of the oxygen-containing buffer layer are uniform.
2. A method of fabricating a nitride epitaxial layer according to claim 1, wherein: o and gallium bonds in the oxygen-containing trimethylgallium or triethylgallium are linked, or O and C bonds are linked; the oxygen-containing trimethylgallium or triethylgallium is formed by OH groups to replace methyl and Ga bonds to link, or O bonds to link two Ga bonds, or O to replace methyl H;
o and aluminum bonds in the oxygen-containing trimethylaluminum or triethylaluminum are linked, or O and C bonds are linked; the oxygen-containing trimethylaluminum or triethylaluminum is formed by substituting OH groups for methyl and aluminum bond linkage, or by linking two Al bonds for O bonds, or by substituting O for methyl H.
3. A method of fabricating a nitride epitaxial layer according to claim 1, wherein: the MO source and oxygen-containing MO source precursor material switching period is inversely related to the epitaxial layer thickness of the nitride.
4. A method of fabricating a nitride epitaxial layer according to claim 1, wherein: the growth thickness of the nitride epitaxial layer is 1-10 mu m.
5. A method of producing a nitride epitaxial layer according to any one of claims 1 to 4, characterized in that: the growth thickness of the oxygen-containing buffer layer is 2-5nm, and the growth thickness of the nitride buffer layer is 3-10nm.
6. A nitride semiconductor epitaxial wafer is characterized in that: comprising a nitride epitaxial layer and an epitaxial structure provided on said nitride epitaxial layer, said nitride epitaxial layer being produced according to the method of any one of claims 1-5;
wherein the thickness of the nitride buffer layer is greater than the thickness of the oxygen-containing buffer layer; the buffer layer comprises a nitride buffer layer and an oxygen-containing buffer layer which are grown by alternately switching an MO source and an oxygen-containing MO source as precursor materials in a periodic cycle, and when the MO source and the oxygen-containing MO source are switched as precursor materials each time, the stress between the substrate and the nitride buffer layer is different, so that nucleation centers of the oxygen-containing buffer layer distributed at different positions are formed on each layer of nitride buffer layer, and the nucleation points of the oxygen-containing buffer layer are uniform.
7. A nitride semiconductor epitaxial wafer according to claim 6, characterized in that: the epitaxial structure is an LED epitaxial structure, and the LED epitaxial structure comprises an n-nitride layer, a nitride multi-quantum well light-emitting layer, a p-type nitride electron blocking layer and a p-type nitride layer which are sequentially arranged along the direction far away from the surface of the substrate, wherein the nitride multi-quantum well light-emitting layer is a nitride quantum well layer and a nitride quantum barrier layer which are alternately arranged.
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