CN114203865B - Preparation method of aluminum nitride epitaxial wafer based on sapphire substrate - Google Patents

Preparation method of aluminum nitride epitaxial wafer based on sapphire substrate Download PDF

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CN114203865B
CN114203865B CN202111483678.6A CN202111483678A CN114203865B CN 114203865 B CN114203865 B CN 114203865B CN 202111483678 A CN202111483678 A CN 202111483678A CN 114203865 B CN114203865 B CN 114203865B
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齐胜利
温荣吉
周飚
刘亚柱
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Ningbo Anxinmei Semiconductor Co ltd
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Abstract

The invention belongs to the technical field of semiconductor electronic devices, and particularly relates to a preparation method of an aluminum nitride epitaxial wafer based on a sapphire substrate. The method mainly carries out process optimization in a buffer stage, and carries out temperature gradient cyclic variation growth in a buffer stage, and the method comprises the steps of trimethylaluminum source long-pass and NH 3 The periodic variation is introduced. After the optimized buffer layer is grown, island-shaped (3D) and two-dimensional (2D) growth are carried out to prepare an aluminum nitride transition layer; and sequentially growing an undoped gallium nitride layer, an N-type gallium nitride layer, a multiple quantum well layer, a P-type electron blocking layer, a P-type gallium nitride layer and a P-type contact layer on the aluminum nitride transition layer to prepare the aluminum nitride epitaxial wafer based on the sapphire substrate. The AlN thin film material grown by the process can change the inclination behavior of dislocation, reduce dislocation density, reduce cracks of an AlN epitaxial wafer, improve crystal quality and obtain a better AlN thin film material, thereby directly improving the photoelectric performance of a device of a product.

Description

Preparation method of aluminum nitride epitaxial wafer based on sapphire substrate
Technical Field
The invention belongs to the technical field of semiconductor electronic devices, and particularly relates to a preparation method of an aluminum nitride epitaxial wafer based on a sapphire substrate.
Background
As a III-V compound semiconductor material, alN not only has ultra-wide direct band gap (6.2 eV), high thermal conductivity, high resistivity, high breakdown field strength, excellent piezoelectric performance and good optical performance, but also has wide application prospect in the fields of ultraviolet light sources, radiation detectors, microwave millimeter wave devices, photoelectric devices, power electronic devices, surface acoustic wave devices and the like. Especially in deep ultraviolet LED light emitting devices, it remains a challenge to obtain high quality AlN with low dislocation density.
In the field of optoelectronic devices, the quality of AlN thin films relates to the performance of UVC deep ultraviolet products. Most UVC LED heterostructures for growing AlN grow on a C-plane sapphire substrate, and the typical growth temperature is 1200-1500 ℃ by adopting MOCVD growth technology, and due to large lattice mismatch between an AlN material and the sapphire substrate, more defects of a deposition layer are caused, and the dislocation density is also high>5×10 8 cm -2 ) The photoelectric performance of the device is seriously affected.
Disclosure of Invention
Aiming at the defect problem of the AlN material used for the deep ultraviolet LED device, the invention provides an effective epitaxial growth method, so that lower defect density and better photoelectric device performance improvement can be obtained.
In order to solve the technical problem of the invention, the adopted technical scheme is that the preparation method of the aluminum nitride epitaxial wafer based on the sapphire substrate comprises the following steps:
step one, baking on a sapphire flat substrate for 1-15min at 1000-1200 ℃. NH (NH) 3 The flow is 1000-10000sccm; the rotating speed of the epitaxial growth basal disc is 100-1200r/min, and the pressure is 5-800mbar;
step two, growing an optimized buffer layer, wherein the temperature in the reaction cavity is subjected to gradient heating, the temperature of the whole stage is controlled to be 800-1200 ℃, the gradient heating process comprises n temperature constant stages and n temperature lifting stages, and the temperature constant stages and the temperature lifting stages alternately appear along with the time; when n is more than or equal to 2, the starting temperature of the temperature increasing stage is equal to the temperature of the previous temperature constant stage, wherein n is a positive integer which is more than or equal to 3 and less than or equal to 6;
NH 3 the amount of the inlet is divided into n flow changesA chemical phase and n flow constant phases, wherein the n flow change phases and the n flow constant phases alternately appear along with the time increment, the n flow change phases correspond to the time of the n temperature lifting phases, and the n flow constant phases correspond to the time of the n temperature constant phases;
setting m as a positive integer of which the value is equal to or more than 1 and is equal to or less than n, and NH in the mth flow change stage 3 According to small flow A m And a large flow A m+1 Alternately and periodically introducing NH at the mth flow constant stage 3 According to the large flow A m+1 Continuously introducing; small flow a in the first flow change stage 1 500-1000sccm, low flow A in the latter flow change stage m+1 High flow a from the previous flow change stage m The same, small flow A in each flow change stage m And a large flow A m+1 The difference of (2) is 500-5000sccm;
continuously introducing trimethylaluminum at a constant speed, wherein the flow is 100-500sccm;
the rotating speed of the epitaxial growth base plate is 200-1200r/min, and the pressure is 10-800mbar, so that an aluminum nitride buffer layer is prepared;
thirdly, firstly growing a 3D aluminum nitride transition layer on the aluminum nitride buffer layer, and then growing a 2D aluminum nitride transition layer to prepare the aluminum nitride transition layer;
and step four, sequentially growing an undoped gallium nitride layer, an N-type gallium nitride layer, a multiple quantum well layer, a P-type electron blocking layer, a P-type gallium nitride layer and a P-type contact layer on the aluminum nitride transition layer to prepare the aluminum nitride epitaxial wafer based on the sapphire substrate.
The preparation method of the aluminum nitride epitaxial wafer based on the sapphire substrate is further improved:
preferably, the duration of each of said temperature ramp-up phases is between 50 and 500s, the rate of temperature ramp-up being greater than 0 and less than 1.5 ℃/s.
Preferably, each of said temperature-constant phases has a duration of 50-500s
Preferably, in each of said flow rate variation phases, a small flow rate A m And a large flow A m+1 The single-pass time is 2-10s, and the small flow A m And a large flow A m+1 The number of cycles of alternate passage is 10-30.
Preferably, in the third step, the growth parameters of the 3D aluminum nitride transition layer are as follows: at 900-1300 ℃ and NH 3 The flow rate of the film is 100-5000sccm, and the growth thickness is 500-1000nm; the rotation speed of the epitaxial growth basal disc is 200-1200r/min, and the pressure is 10-800mbar.
Preferably, in the third step, the growth parameters of the 2D aluminum nitride transition layer are as follows: at 1000-1500 deg.C, NH 3 The flow is 100-5000sccm, and the thickness is 500-1500nm; the rotation speed of the epitaxial growth basal disc is 200-1200r/min, and the pressure is 10-800mbar.
Preferably, the temperature in the reaction chamber is 800-1000 ℃.
Preferably, n is 3.
Preferably, the high-purity hydrogen is used as carrier gas, the trimethylaluminum is used as Al source, and the ammonia gas is used as N source.
Compared with the prior art, the invention has the beneficial effects that:
an epitaxial growth method of aluminium nitride based on sapphire substrate is mainly process optimization in buffer stage, and comprises the steps of cyclic variation growth of temperature gradient, long-pass of trimethylaluminium source and NH in buffer stage 3 And (5) introducing a periodic gradient change. After the optimized buffer layer is grown, the island-shaped (3D) and two-dimensional (2D) growth can be carried out, and a better AlN film material can be obtained. The AlN thin film material grown by the process can change the inclination behavior of dislocation, reduce dislocation density, reduce AlN epitaxial wafer cracks and improve crystal quality, thereby directly improving the photoelectric performance of a device of a product.
The invention aims to reduce dislocation density, reduce AlN epitaxial wafer cracks and improve crystal quality by growing an AlN material on a sapphire substrate and optimizing a growth process of a buffer layer, thereby directly improving the photoelectric performance of a device of a product.
Drawings
FIG. 1 is a temperature, trimethylaluminum (TMAL) feed-through during growth of an optimized buffer layer in the process of the present inventionQuantity and NH 3 Graph of change over time.
FIG. 2 is a chart showing the XRD 002 and XRD 102 bicrystal diffraction analysis of the samples of the conventional aluminum nitride epitaxial wafer prepared in the comparative example.
FIG. 3 is a chart showing the XRD/002 and XRD/102 bicrystal diffraction analysis of the aluminum nitride epitaxial wafer sample obtained in example 1.
FIG. 4 is a chart showing the XRD/002 and XRD/102 bicrystal diffraction analysis of the aluminum nitride epitaxial wafer sample obtained in example 2.
Detailed Description
The present invention will be further described in detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more apparent, and all other examples obtained by those skilled in the art without making any inventive effort are within the scope of the present invention based on the examples in the present invention.
The following examples use high purity hydrogen or nitrogen as carrier gas, trimethylaluminum (TMAL) as Al source, ammonia (NH) 3 ) Is an N source.
Comparative example
An aluminum nitride epitaxial growth method based on a sapphire substrate comprises the following steps:
and firstly, baking on a sapphire flat substrate for 10min at 1050 ℃. NH (NH) 3 The flow rate is 10000sccm; the rotation speed of the epitaxial growth basal disc is 500r/min, and the pressure is 60mbar;
step two, growing a buffer layer at 950 ℃; the ammonia gas amount is 20000sccm, the trimethylaluminum flow is 300sccm, the epitaxial growth substrate rotation speed is 600r/min, and the pressure is 60mbar;
step three, after the buffer layer is grown, 3D AlN is grown at 1100 ℃ and NH 3 The flow rate is 2000sccm, and the thickness is 750nm; the rotation speed is 600r/min, and the pressure is 70mbar;
step four, after the 3D AlN growth is finished, growing 2D AlN at 1200 ℃ and NH 3 The flow rate is between 3000sccm, and the thickness is 1000nm; the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 70mbar; preparing a common aluminum nitride epitaxial wafer sampleThe product is obtained.
Carrying out XRD 002 and XRD 102 bicrystal diffraction analysis graph test on the prepared common aluminum nitride epitaxial wafer sample, wherein the result is shown in figure 2; as can be seen from fig. 2, the half-width of the XRD:002 of the aluminum nitride epitaxial wafer prepared by the method is 255, and the half-width of the XRD:102 is 540.4, which is relatively large; the crystal quality deviation is proved to have more defects. Especially in a thermal state, the brightness influence is large, and the light attenuation is obvious. The yield is affected, especially VF4 and leakage yield are low. The device has larger influence on brightness attenuation and large current performance of the device, and the service life of the device is reduced.
Example 1
An aluminum nitride epitaxial growth method based on a sapphire substrate comprises the following steps:
and firstly, baking on a sapphire flat substrate for 10min at 1050 ℃. NH (NH) 3 Flow 10000sccm; the rotation speed of the epitaxial growth basal disc is 500r/min, and the pressure is 60mbar;
step two, growing an optimized buffer layer, wherein the temperature Ramp is changed, the initial temperature is 800 ℃, and the temperature in the whole stage is controlled at 950 ℃; the gradient heating process comprises 3 temperature constant stages and 3 temperature lifting stages, wherein the 3 temperature constant stages and the 3 temperature lifting stages alternately appear along with the time increment, the starting temperature of each temperature lifting stage is equal to the temperature of the previous temperature constant stage, and the ending temperature of each temperature lifting stage is equal to the temperature of the next temperature constant stage; the duration of the constant temperature phase is 200s, and the duration of the temperature rise phase is 60s;
NH 3 the introduced quantity is divided into 3 flow change phases and 3 flow constant phases, wherein the 3 flow change phases and the 3 flow constant phases alternately appear along with the time increment, the 3 flow change phases correspond to the time of the 3 temperature lifting phases, and the 3 flow constant phases correspond to the time of the 3 temperature constant phases; NH in the mth flow rate variation stage 3 According to small flow A m And a large flow A m+1 Alternately and periodically introducing NH at the mth flow constant stage 3 According to the large flow A m+1 Continuously introducing; first flow rate variation stageSmall flow A 1 At 500sccm, the small flow A at the latter flow change stage m+1 High flow a from the previous flow change stage m The same; small flow a in each flow change phase m And a large flow B m The difference between the two flows is 1000sccm, and the small flow A m And a large flow A m+1 The cycle number of the alternate inlet is 20, and in each flow change phase, the small flow A m And a large flow A m+1 The single-pass time is 3s, and m is a positive integer which is more than or equal to 1 and less than or equal to 3;
the trimethylaluminum is in a direct-through state, and the flow is 300sccm;
the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 60mbar;
step three, after the growth of the optimized buffer layer is finished, 3D AlN is grown at 1100 ℃ and NH 3 Flow rate 2000sccm, thickness 750nm; the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 70mbar;
step four, after the 3D AlN growth is finished, growing 2D AlN at 1200 ℃ and NH 3 Flow rate is 3000sccm, thickness is 1000nm; the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 70mbar; an aluminum nitride epitaxial wafer sample 1 was produced.
Carrying out XRD 002 and XRD 102 bicrystal diffraction analysis chart test on the obtained aluminum nitride epitaxial wafer sample 1, wherein the result is shown in figure 3; as can be seen from fig. 3, the half-width of the XRD:002 of the aluminum nitride epitaxial wafer prepared by the method is 94.62, and the half-width of the XRD:102 is 367.9, which are relatively small; the crystal lattice quality is better, the defects are fewer, and the dislocation density is low.
Example 2
And firstly, baking on a sapphire flat substrate for 10min at 1050 ℃. NH (NH) 3 Flow 10000sccm; the rotation speed of the epitaxial growth basal disc is 500r/min, and the pressure is 60mbar;
step two, growing an optimized buffer layer, wherein the temperature Ramp is changed, the initial temperature is 800 ℃, and the temperature in the whole stage is controlled at 950 ℃; the gradient heating process comprises 4 temperature constant stages and 4 temperature lifting stages, wherein the 4 temperature constant stages and the 4 temperature lifting stages alternately appear along with the time increase, the starting temperature of each temperature lifting stage is equal to the temperature of the previous temperature constant stage, and the ending temperature of each temperature lifting stage is equal to the temperature of the next temperature constant stage; the duration of the constant temperature phase was 300s and the duration of the elevated temperature phase was 60s.
NH 3 The input quantity is divided into 4 flow change phases and 4 flow constant phases, the 4 flow change phases and the 4 flow constant phases alternately appear along with the time increment, the 4 flow change phases correspond to the time of the 4 temperature lifting phases, and the 4 flow constant phases correspond to the time of the 4 temperature constant phases; NH in the mth flow rate variation stage 3 According to small flow A m And a large flow A m+1 Alternately and periodically introducing NH at the mth flow constant stage 3 According to the large flow A m+1 Continuously introducing; the first flow change stage is small flow A 1 1000sccm, a small flow A in the latter flow change stage m+1 High flow a from the previous flow change stage m The same; small flow a in each flow change phase m And a large flow B m The difference of (C) is 700sccm, and the small flow A m And a large flow A m+1 The number of periods of alternate feeding is 15, and in each flow change phase, the small flow A m And a large flow A m+1 The single-pass time is 4s, and m is 3;
the trimethylaluminum is in a direct-through state, and the flow is 300sccm;
the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 60mbar;
step three, after the growth of the optimized buffer layer is finished, 3D AlN is grown at the temperature of 1000 ℃ and NH 3 Flow rate is 3000sccm, thickness is 750nm; the rotating speed of the epitaxial growth basal disc is 600r/min, and the pressure is 70mbar;
step four, after the 3D AlN growth is finished, growing 2D AlN at 1200 ℃ and NH 3 The flow is 3500sccm, and the thickness is 1000nm; the rotation speed of the epitaxial growth substrate is 600r/min, and the pressure is as follows: 70mbar; sample 2 of an aluminum nitride epitaxial wafer was obtained.
Carrying out XRD 002 and XRD 102 bicrystal diffraction analysis chart test on the obtained aluminum nitride epitaxial wafer sample 2, wherein the result is shown in figure 4; as can be seen from FIG. 4, the half-width of the XRD:002 of the aluminum nitride epitaxial wafer prepared by the method is 122.5, and the half-width of the XRD:102 is 374.2, which is relatively small; the crystal lattice quality is better, the defects are fewer, and the dislocation density is low.
As shown by the test results of the comparative example and the example, the AlN thin film material grown by the process can reduce dislocation density, reduce cracks of an AlN epitaxial wafer and improve crystal quality, thereby directly improving the photoelectric performance of a device of a product.
Those skilled in the art will appreciate that the foregoing is merely a few, but not all, embodiments of the invention. It should be noted that many variations and modifications can be made by those skilled in the art, and all variations and modifications which do not depart from the scope of the invention as defined in the appended claims are intended to be protected.

Claims (9)

1. The preparation method of the aluminum nitride epitaxial wafer based on the sapphire substrate is characterized by comprising the following steps of:
step one, baking on a sapphire flat substrate for 1-15min at 1000-1200 ℃ and NH 3 The flow is 1000-10000sccm; the rotating speed of the epitaxial growth basal disc is 100-1200r/min, and the pressure is 5-800mbar;
step two, growing an optimized buffer layer, wherein the temperature in the reaction cavity is subjected to gradient heating, the temperature of the whole stage is controlled to be 800-1200 ℃, the gradient heating process comprises n temperature constant stages and n temperature lifting stages, and the temperature constant stages and the temperature lifting stages alternately appear along with the time; when n is more than or equal to 2, the starting temperature of the temperature increasing stage is equal to the temperature of the previous temperature constant stage, wherein n is a positive integer which is more than or equal to 3 and less than or equal to 6;
NH 3 the introduced quantity is divided into n flow change phases and n flow constant phases, the n flow change phases and the n flow constant phases alternately appear along with the time increment, the n flow change phases correspond to the time of the n temperature rise phases, and the n flow constant phases are constant with the n temperaturesThe time of the stage appearance corresponds to that of the stage;
setting m as a positive integer of which the value is equal to or more than 1 and is equal to or less than n, and NH in the mth flow change stage 3 According to small flow A m And a large flow A m+1 Alternately and periodically introducing NH at the mth flow constant stage 3 According to the large flow A m+1 Continuously introducing; small flow a in the first flow change stage 1 500-1000sccm, low flow A in the latter flow change stage m+1 High flow a from the previous flow change stage m The same, small flow A in each flow change stage m And a large flow A m+1 The difference of (2) is 500-5000sccm;
continuously introducing trimethylaluminum at a constant speed, wherein the flow is 100-500sccm;
the rotating speed of the epitaxial growth base plate is 200-1200r/min, and the pressure is 10-800mbar, so that an aluminum nitride buffer layer is prepared;
thirdly, firstly growing a 3D aluminum nitride transition layer on the aluminum nitride buffer layer, and then growing a 2D aluminum nitride transition layer to prepare the aluminum nitride transition layer;
and step four, sequentially growing an undoped gallium nitride layer, an N-type gallium nitride layer, a multiple quantum well layer, a P-type electron blocking layer, a P-type gallium nitride layer and a P-type contact layer on the aluminum nitride transition layer to prepare the aluminum nitride epitaxial wafer based on the sapphire substrate.
2. The method of manufacturing an aluminum nitride epitaxial wafer on a sapphire substrate according to claim 1, wherein the duration of each of the temperature-elevating stages is 50-500s, and the rate of temperature elevation is greater than 0 and less than 1.5 ℃/s.
3. The method for producing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein the duration of each of the constant temperature stages is 50 to 500s.
4. The method for producing an aluminum nitride epitaxial wafer on the basis of a sapphire substrate according to claim 1, wherein in each of the flow rate variation stagesSmall flow A m And a large flow A m+1 The single-pass time is 2-10s, and the small flow A m And a large flow A m+1 The number of cycles of alternate passage is 10-30.
5. The method for preparing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein the growth parameters of the 3D aluminum nitride transition layer in the third step are as follows: at 900-1300 ℃ and NH 3 The flow rate of the film is 100-5000sccm, and the growth thickness is 500-1000nm; the rotation speed of the epitaxial growth basal disc is 200-1200r/min, and the pressure is 10-800mbar.
6. The method for preparing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein the growth parameters of the 2D aluminum nitride transition layer in the third step are as follows: at 1000-1500 deg.C, NH 3 The flow is 100-5000sccm, and the thickness is 500-1500nm; the rotation speed of the epitaxial growth basal disc is 200-1200r/min, and the pressure is 10-800mbar.
7. The method for preparing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein the temperature in the reaction chamber is 800-1000 ℃.
8. The method for manufacturing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein n is 3.
9. The method for producing an aluminum nitride epitaxial wafer based on a sapphire substrate according to claim 1, wherein high purity hydrogen is used as a carrier gas, trimethylaluminum is used as an Al source, and ammonia is used as an N source.
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