CN110429019B - Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN layer - Google Patents
Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN layer Download PDFInfo
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Abstract
An epitaxial growth method for inserting an InGaN layer to improve the quality of a nonpolar GaN material belongs to the technical field of GaN material epitaxy, and utilizes the Metal Organic Chemical Vapor Deposition (MOCVD) technology to grow the nonpolar GaN material with low dislocation density, wherein the epitaxial structure comprises an r-plane sapphire substrate and a low-temperature GaN nucleating layer from bottom to top in sequence; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio (molar flow ratio of V-group source to III-group source); a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time; an InGaN insertion layer; and growing a high-temperature two-dimensional GaN layer under the conditions of low pressure and low V/III ratio for the second time. The invention is characterized in that the InGaN insertion layer is inserted into the two-dimensional GaN layer, which can relieve stress and prevent transmission of threading dislocation generated by mismatch of part of the sapphire substrate and the GaN. The invention improves the defects of the prior art, can reduce the dislocation density of the nonpolar GaN material, improves the surface appearance of the material and improves the quality of an epitaxial wafer.
Description
The technical field is as follows:
the invention belongs to the technical field of GaN material epitaxy, and relates to a technology for improving the quality of a nonpolar GaN material and reducing dislocation.
Background art:
gallium nitride (GaN) has the characteristics of direct wide bandgap, stable chemical property and high temperature resistance, and is widely applied to luminescent devices, photoelectric detectors, solar cells and the like. The traditional GaN film prepared on a sapphire substrate grows along the c axis of a polar axis, and a strong polarization electric field can appear in an active region of a device, so that electron hole pairs are separated, a quantum confinement Stark effect appears, and the luminous efficiency of the device is reduced. To avoid polarization effects, a-plane or m-plane nonpolar GaN material may be grown on the substrate. Due to the fact thatThe bulk GaN substrate is small in size and high in price, and currently, the main nonpolar GaN material is grown on an external substrate, such as a r-plane sapphire substrate, and a-plane nonpolar GaN is heteroepitaxially grown. Hetero-epitaxial a-plane nonpolar GaN with c-axis and m-axis at the growth plane (11)20) And the crystal lattice mismatch with the r-plane sapphire substrate is large, the crystal lattice mismatch is 1.2% along the c axis, and the crystal lattice mismatch is 16% along the m axis, so that the quality of the heteroepitaxial GaN material is poor, and the epitaxial material shows anisotropy. The quality of non-polar GaN material is a greater distance from commercial production requirements than polar GaN material grown along the c-axis. Although many in-situ defect and dislocation removal techniques are widely used for the growth of non-polar GaN materials, such as two-step growth method of converting three-dimensional growth into two-dimensional growth, SiN insertion layer technique, pattern substrate technique, etc. The two-step growth method is simple and effective, but a thicker three-dimensional GaN layer needs to be grown to reduce dislocation, and the thicker three-dimensional GaN layer can degrade the surface appearance of the material. In any method, the problem of material quality is not completely solved, and at present, two main problems exist in the growth of the non-polar GaN material, one is poor surface appearance, and a large number of stripes and triangular pits which fluctuate along the c axis exist; another is the presence of a large number of defects including threading dislocations and basal plane stacking faults.
Therefore, there is a need to provide a method for growing a non-polar GaN material based on a sapphire substrate, which has a low dislocation density and a good surface morphology and can improve the quality of a non-polar GaN film, so as to solve the above problems. The InGaN insertion layer method provided by the inventor is combined with a two-step growth method, so that dislocation can be continuously reduced, and the surface appearance of the material is improved.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and the quality of a nonpolar a-plane GaN thin film material growing on a sapphire substrate is improved, the dislocation density is reduced, and the surface appearance is improved by a Metal Organic Chemical Vapor Deposition (MOCVD) method.
A structure for improving the epitaxial quality of a nonpolar GaN material by inserting an InGaN layer is characterized in that an r-plane sapphire substrate is sequentially arranged from bottom to top; a low temperature GaN nucleation layer; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time; an InGaN insertion layer; and growing a high-temperature two-dimensional GaN layer under the conditions of low pressure and low V/III ratio for the second time.
Or in the second scheme, the r-plane sapphire substrate is sequentially arranged from bottom to top; a low temperature GaN nucleation layer; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio; an InGaN insertion layer; and growing the high-temperature two-dimensional GaN layer under the growth conditions of low pressure and low V/III ratio.
Wherein the growth temperature of the InGaN insertion layer is 700-800 ℃, the thickness of the InGaN insertion layer is 5-40nm, and the mole percentage of the In component In the InGaN insertion layer is 5-20%.
Wherein, the high-temperature three-dimensional GaN layer grows under the growth conditions of high pressure and high V/III ratio. The temperature is 1000-1100 ℃, the pressure is 300-600mbar, the V/III ratio is 1000-3000, and the thickness is 1-2 μm.
Wherein, the high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time has the temperature of 1000-1100 ℃, the pressure of 50-200mbar, the V/III ratio of 50-300 and the thickness of less than 2 μm.
Wherein, the high-temperature two-dimensional GaN layer grows under the growth conditions of low pressure and low V/III ratio for the second time, the temperature is 1000-1100 ℃, the pressure is 50-200mbar, the V/III ratio is 50-300, and the thickness is 2-5 μm.
And in the second scheme, a high-temperature two-dimensional GaN layer grows under the growth conditions of medium and low pressure and low V/III ratio, the temperature is 1000-1100 ℃, the pressure is 50-200mbar, the V/III ratio is 50-300, and the thickness is 2-5 μm.
The growth steps are as follows:
a substrate is selected, and impurities in the substrate are removed at a high temperature.
Nitriding in a mixed atmosphere of hydrogen and nitrogen.
And cooling to grow a nucleation layer.
And (4) heating, and growing the nonpolar GaN film under the conditions of high pressure and high V/III ratio.
Growing the nonpolar GaN film under the conditions of low pressure and low V/III ratio.
Cooling and growing InGaN insertion layer
And (4) heating, and growing the nonpolar GaN film under the conditions of low pressure and low V/III ratio.
An epitaxial growth method for improving the quality of a nonpolar GaN material by inserting an InGaN layer is characterized by comprising the following steps:
the method comprises the following steps: the selected substrate is a r-surface sapphire substrate, the r-surface sapphire substrate is placed on a substrate holder in an MOCVD reaction chamber, and the substrate is baked for 3-10 minutes at the temperature of 1000-1100 ℃.
Step two: nitriding for 2-10 min at 1000-1100 deg.c in mixed atmosphere of nitrogen and ammonia in the volume ratio of 2 to 1.
Step three: reducing the temperature to 500-600 ℃, and growing a low-temperature nucleation GaN layer with the thickness of 20-40nm under the pressure of 500-600 mbar.
Step four: heating to 1000-1100 deg.C, pressure 300-.
Step five: growing a two-dimensional GaN layer with low pressure and low V/III ratio at the temperature of 1000-1100 ℃ and the pressure of 50-200mbar and the V/III ratio of 50-300, wherein the thickness of the two-dimensional GaN layer is less than 2 mu m.
Step six: lowering the temperature to 700-800 ℃ to grow an InGaN layer, wherein the In component is 5-20%. The thickness is 5-40 nm.
Step seven: heating to 1000-1100 deg.C, pressure 50-200mbar, V/III ratio 50-300, growing two-dimensional GaN layer with low pressure and low V/III ratio, and thickness 2-5 μm.
Trimethyl gallium is a gallium source, trimethyl indium is an indium source, ammonia is a nitrogen source, and carrier gas is hydrogen and nitrogen.
The position (figure 1) of the insertion layer between the high-temperature three-dimensional GaN layer grown under the high-pressure and high-V/III-ratio growth condition and the high-temperature two-dimensional GaN layer grown under the low-pressure and low-V/III-ratio growth condition is 0 μm of the thickness of the InGaN insertion layer; the insert layer is in the middle of the high temperature two-dimensional GaN layer grown under low pressure, low V/III ratio growth conditions (FIG. 2), and the thickness of the InGaN insert layer is less than 2 μm.
The mechanism of the invention is characterized in that: by utilizing the MOCVD growth technology, a two-step growth method (firstly growing a three-dimensional GaN layer and then growing a two-dimensional GaN layer on the basis) is adopted on an r-plane sapphire substrate, an InGaN insertion layer is introduced, and the InGaN layer is inserted into the middle of the two-dimensional gallium nitride layer. The conventional method is a two-step growth method, a three-dimensional nonpolar GaN film grows under the conditions of high pressure and high V/III ratio, dislocation can be reduced, but the excessively thick three-dimensional GaN grows to bring rough surface appearance and influence the quality of materials grown subsequently. On the basis, the two-dimensional nonpolar GaN film grows under the conditions of low pressure and low V/III ratio, and the surface appearance can be improved. However, the nonpolar GaN thin film grown by the two-step growth method still has high dislocation density and a rough surface, which is not beneficial to the growth of subsequent semiconductor devices. According to the invention, the InGaN insertion layer is introduced, and has the capabilities of relieving stress generated due to different lattice constants, changing the dislocation transmission direction and cutting off partial dislocation, and blocking transmission of threading dislocation generated by mismatch of most sapphire substrates and GaN epitaxial layers. Therefore, the grown nonpolar GaN film has lower dislocation density and better surface appearance. Can improve the defects of the original two-step growth method.
Description of the drawings:
FIG. 1 is a schematic view of a growth structure in which an InGaN insertion layer is inserted between a three-dimensional GaN layer and a two-dimensional GaN layer
FIG. 2 is a schematic view of the growth structure of the present invention with an InGaN insertion layer inserted between two-dimensional GaN layers
FIG. 3 shows a sample (11) without an InGaN layer interposed20) X-ray diffraction ω scan of the surface along the c-axis;
FIG. 4 is (11) of the sample (embodiment 1) with an InGaN layer interposed between a three-dimensional GaN layer and a two-dimensional GaN layer20) X-ray diffraction ω scan of the surface along the c-axis;
FIG. 5 shows (11) of a sample (embodiment 2) in which an InGaN layer is interposed between two-dimensional GaN layers20) X-ray diffraction ω scan of the surface along the c-axis;
FIG. 6 is an atomic force microscope surface topography of a sample without an inserted InGaN layer;
FIG. 7 is an atomic force microscope surface topography of a sample (embodiment 1) inserted with an InGaN layer between a three-dimensional GaN layer and a two-dimensional GaN layer;
fig. 8 is an atomic force microscope surface topography of a sample (embodiment 2) inserted between InGaN layers in a two-dimensional GaN layer.
Detailed Description
Specific embodiment example 1:
FIG. 1 schematic view of InGaN insertion layer interposed between a three-dimensional GaN layer and a two-dimensional GaN layer
The invention is further illustrated below with reference to embodiment 1:
the method is characterized in that an InGaN layer is inserted into a r-plane sapphire substrate by a Metal Organic Chemical Vapor Deposition (MOCVD) method to improve the quality of a nonpolar a-plane GaN film, reduce dislocation density and improve surface appearance. As shown in fig. 1, the InGaN insertion layer is inserted between the three-dimensional GaN layer and the two-dimensional GaN layer, and the specific experimental steps are as follows:
the method comprises the following steps: the r-surface sapphire substrate is placed on a substrate holder in an MOCVD reaction chamber and baked for 3 minutes at 1050 ℃.
Step two: nitriding is carried out for 10 minutes at 1050 ℃ in a mixed atmosphere of nitrogen and ammonia in a volume ratio of 2 to 1.
Step three: the temperature is reduced to 550 ℃, the pressure is 500mbar, and a low-temperature nucleation GaN layer with the thickness of 40nm is grown.
Step four: heating to 1050 deg.C, pressure 500mbar, V/III ratio 3000, growing high-pressure high V/III ratio three-dimensional GaN layer with thickness 2 μm.
Step five: the temperature was lowered to 750 ℃ to grow an InGaN insertion layer In which the In component was 10% and the thickness was 20 nm.
Step six: heating to 1050 ℃, the pressure is 50mbar, the V/III ratio is 100, and a low-pressure and low-V/III ratio two-dimensional GaN layer with the thickness of 4 mu m is grown.
Trimethyl gallium is a gallium source, trimethyl indium is an indium source, ammonia is a nitrogen source, and carrier gas is hydrogen and nitrogen.
Specific embodiment example 2:
fig. 2 is a schematic view of the growth structure of the present invention in which an InGaN buffer layer is inserted between two-dimensional GaN layers, and the specific steps are as follows:
the method comprises the following steps: the r-surface sapphire substrate is placed on a substrate holder in an MOCVD reaction chamber and baked for 3 minutes at 1050 ℃.
Step two: nitriding is carried out for 10 minutes at 1050 ℃ in a mixed atmosphere of nitrogen and ammonia in a proportional volume of 2 to 1.
Step three: the temperature is reduced to 550 ℃, the pressure is 500mbar, and a low-temperature nucleation GaN layer with the thickness of 40nm is grown.
Step four: heating to 1050 deg.C, pressure 500mbar, V/III ratio 3000, growing high-pressure high V/III ratio three-dimensional GaN layer with thickness 2 μm.
Step five: and growing a two-dimensional GaN layer with low pressure and low V/III ratio at 1050 ℃, 50mbar and 100V/III ratio, wherein the thickness of the two-dimensional GaN layer is 2 mu m.
Step six: the temperature was lowered to 750 ℃ to grow an InGaN layer In which the In component was 10% and the thickness was 20 nm.
Step seven: heating to 1050 ℃, the pressure is 50mbar, the V/III ratio is 100, and a low-pressure and low-V/III ratio two-dimensional GaN layer with the thickness of 4 mu m is grown.
Trimethyl gallium is a gallium source, trimethyl indium is an indium source, ammonia is a nitrogen source, and carrier gas is hydrogen and nitrogen.
Test results, FIG. 3 shows the sample without InGaN layer insertion (11)20) X-ray diffraction ω scan of the surface along the c-axis with a half-width of 1148 arcsec; FIG. 4 is (11) of the sample (embodiment 1) with an InGaN layer interposed between a three-dimensional GaN layer and a two-dimensional GaN layer20) An x-ray diffraction omega scanning graph along a c axis is formed, the half width is 1060arcsec, and the half width is reduced by 88arcsec compared with that of a sample without an inserted InGaN layer; FIG. 5 shows (11) of a sample (embodiment 2) in which an InGaN layer is interposed between two-dimensional GaN layers20) The surface was x-ray diffraction ω scanned along the c-axis with a half-width of 1018arcsec, which was 130arcsec less than the sample without the intervening InGaN layer. It can be seen that after insertion into the InGaN layer, the half-width is reduced, indicating a reduction in the dislocation density of the material. FIG. 6 is an atomic force microscope surface topography of a sample without an inserted InGaN layer, with a root mean square roughness of 1.01 nm; fig. 7 is an atomic force microscope surface topography of a sample (embodiment 1) inserted with an InGaN layer between a three-dimensional GaN layer and a two-dimensional GaN layer, with a root mean square roughness of the surface of 0.76 nm; FIG. 8 is an atomic force microscope surface topography of a sample (embodiment 2) with an InGaN layer interposed between two-dimensional GaN layers, with a root mean square roughness of the surface of 0.70nm, with an insertionThe samples of embodiment 1 and embodiment 2 after the InGaN layer have reduced roughness and flatter surface.
From the test results, the nonpolar GaN thin films prepared in the embodiment 1 and the embodiment 2 have lower dislocation density and better surface morphology. The quality of the nonpolar GaN material is improved, and the defects of the prior art are improved.
Finally, it should be noted that: the above facts are the general embodiments of the present invention, not the limitations thereof; any simple changes or modifications in the technical solutions of the above embodiments, or any equivalent replacement of part or all of the technical solutions, should be included in the protection scope of the present invention.
Claims (2)
1. A method for improving the epitaxial quality of a nonpolar GaN material by inserting an InGaN layer is characterized in that an r-plane sapphire substrate is sequentially arranged from bottom to top; a low temperature GaN nucleation layer; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time; an InGaN insertion layer; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the second time;
or in the second scheme, the r-plane sapphire substrate is sequentially arranged from bottom to top; a low temperature GaN nucleation layer; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio; an InGaN insertion layer; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio;
a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio; the temperature is 1000-1100 ℃, the pressure is 300-600mbar, the V/III ratio is 1000-3000, and the thickness is 1-2 μm;
growing a high-temperature two-dimensional GaN layer under the growth conditions of low pressure and low V/III ratio for the first time at the temperature of 1000-1100 ℃, under the pressure of 50-200mbar and with the V/III ratio of 50-300 and with the thickness of less than 2 mu m;
the InGaN insertion layer grows at the temperature of 700-800 ℃ and the thickness of 5-40nm, and the mole percentage of an In component In the InGaN layer is 5% -20%;
and a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the second time, wherein the temperature is 1000-1100 ℃, the pressure is 50-200mbar, the V/III ratio is 50-300, and the thickness is 2-5 mu m.
2. The method of claim 1, wherein: and in the second scheme, a high-temperature two-dimensional GaN layer grows under the growth conditions of medium and low pressure and low V/III ratio, the temperature is 1000-1100 ℃, the pressure is 50-200mbar, the V/III ratio is 50-300, and the thickness is 2-5 μm.
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