CN110429019A - A kind of insertion InGaN layer improves the epitaxial growth method of non-polar GaN quality of materials - Google Patents
A kind of insertion InGaN layer improves the epitaxial growth method of non-polar GaN quality of materials Download PDFInfo
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Abstract
It is a kind of insertion InGaN layer improve non-polar GaN quality of materials epitaxial growth method belong to GaN material epitaxy technology field, utilize metal-organic chemical vapor deposition equipment (MOCVD) technology, the low-dislocation-density non-polar GaN material of growth, epitaxial structure is from bottom to top successively are as follows: r surface sapphire substrate, low temperature GaN nucleating layer；High pressure, the high-temperature three-dimensional GaN layer of high V/III ratio (V race and group III source molar flow ratio) growth conditions growth；First time low pressure, low V/III are than high temperature two-dimensional GaN layer that growth conditions is grown；InGaN insert layer；Second of low pressure, low V/III are than high temperature two-dimensional GaN layer that growth conditions is grown.It is characteristic of the invention that being inserted into InGaN insert layer in two-dimentional GaN layer, stress can be alleviated, and block the transmitting for the threading dislocation that part Sapphire Substrate and GaN mismatch generate.Present invention improves the deficiencies in the prior art, can reduce non-polar GaN material dislocation density, improve material surface pattern, improve the quality of epitaxial wafer.
Description
Technical field:
The invention belongs to GaN material epitaxy technology fields, are related to a kind of raising non-polar GaN quality of materials, reduce dislocation
Technology.
Background technique:
Gallium nitride (GaN) has direct broad stopband, and chemical property is stablized, and feature resistant to high temperature is widely used in photophore
Part, photodetector, solar battery etc..Traditional GaN film prepared on a sapphire substrate is raw along polar axis c-axis
Long, it will appear very strong polarized electric field in device active region, electron hole pair caused to separate, quantum confined Stark occur
Effect leads to the reduction of device light emitting efficiency.In order to avoid polarity effect occurs, the non-of the face a or the face m can be grown on substrate
Polar GaN material.Since body GaN substrate size is small and price is high, current main non-polar GaN material is still grown in outer
On portion's substrate, such as the face heteroepitaxial growth a non-polar GaN in r surface sapphire substrate.The face hetero-epitaxy a non-polar GaN, c-axis
With m axle position in aufwuchsplate (1120) in, there is big lattice mismatch with r surface sapphire substrate, along c-axis lattice mismatch 1.2%, along m
Axis mismatch 16% leads to hetero-epitaxy GaN material poor quality, and epitaxial material shows anisotropy.It is grown with along c-axis
Polar GaN material compare, non-polar GaN quality of materials and commercially produce requirement and have relatively large distance.Although many go in place
Except defect and dislocation technology are widely used in the growth of non-polar GaN material, as three dimensional growth is converted to two steps of bidimensional growth
Growth method, SiN insert layer technology, graph substrate technology etc..Two-step growth method therein is simple and effective, but there is positions to be reduced
Mistake is it is necessary to grow thicker three-dimensional GaN layer, but the problem of thicker three-dimensional GaN layer can make material surface pattern degenerate.No matter
Which kind of method is not all fully solved quality of materials problem, currently, there are two main problems in non-polar GaN Material growth,
One is poor surface topography, there is the striped largely to rise and fall along c-axis and triangle hole；The other is there is a large amount of lack
It falls into, including threading dislocation and basal plane stacking fault.
Therefore, it is necessary to provide a kind of based on Sapphire Substrate, the non-polar GaN material of growth, dislocation density is small, surface
Pattern is good, can improve the method for nonpolar GaN film quality, to solve the above problems.It is proposed that InGaN insert layer
Method can continue to reduce dislocation, and improve material surface pattern in conjunction with two-step growth method.
Summary of the invention:
It is an object of the invention to improve the deficiencies in the prior art, pass through metal-organic chemical vapor deposition equipment (MOCVD)
Method improves the nonpolar a face GaN thin-film material quality grown on a sapphire substrate, reduces dislocation density, improves surface shape
Looks.
It is a kind of insertion InGaN layer improve non-polar GaN material epitaxy quality structure, which is characterized in that from bottom to top according to
It is secondary are as follows: r surface sapphire substrate；Low temperature GaN nucleating layer；High pressure, high V/III are than high-temperature three-dimensional GaN layer that growth conditions is grown；The
Low pressure, low V/III are than high temperature two-dimensional GaN layer that growth conditions is grown；InGaN insert layer；Second of low pressure, low V/III
Than the high temperature two-dimensional GaN layer of growth conditions growth.
Either scheme two, from bottom to top successively are as follows: r surface sapphire substrate；Low temperature GaN nucleating layer；High pressure, high V/III
Than the high-temperature three-dimensional GaN layer of growth conditions growth；InGaN insert layer；Low pressure, low V/III are than high temperature two that growth conditions is grown
Tie up GaN layer.
Wherein, InGaN insert layer, 700 DEG C -800 DEG C of growth temperature, thickness 5-40nm, In component in InGaN layer
Molar percentage is in 5%-20%.
Wherein, high pressure, high V/III are than high-temperature three-dimensional GaN layer that growth conditions is grown.1000 DEG C -1100 DEG C of temperature, pressure
Power 300-600mbar, V/III ratio 1000-3000,1 μm -2 μm of thickness.
Wherein, first time low pressure, low V/III are than the high temperature two-dimensional GaN layer that growth conditions is grown, 1000 DEG C of temperature-
1100 DEG C, pressure 50-200mbar, V/III ratio 50-300, thickness is less than 2 μm.
Wherein, second of low pressure, low V/III are than the high temperature two-dimensional GaN layer that growth conditions is grown, 1000 DEG C of temperature-
1100 DEG C, pressure 50-200mbar, V/III ratio 50-300,2 μm -5 μm of thickness.
Two mesolow of scheme, low V/III are than the high temperature two-dimensional GaN layer that growth conditions is grown, and 1000 DEG C -1100 DEG C of temperature,
Pressure 50-200mbar, V/III ratio 50-300,2 μm -5 μm of thickness.
Its growth step is as follows:
A kind of substrate is selected, the impurity in substrate is removed in high temperature.
It is nitrogenized in hydrogen and nitrogen mixture atmosphere.
Cooling growth nucleating layer.
Heating, the growing nonpolar GaN film under the conditions of high pressure, high V/III ratio.
The growing nonpolar GaN film under the conditions of low pressure, low V/III ratio.
Cooling grows InGaN insert layer
Heating, under the conditions of low pressure, low V/III ratio, growing nonpolar GaN film.
A kind of insertion InGaN layer improves the epitaxial growth method of non-polar GaN quality of materials, it is characterised in that following step
It is rapid:
Step 1: the substrate of selection is r surface sapphire substrate, and r surface sapphire substrate is put into MOCVD reaction chamber
On substrate bracket, at 1000 DEG C -1100 DEG C of temperature, toast 3-10 minutes.
Step 2: at 1000 DEG C -1100 DEG C of temperature, mixed atmosphere that nitrogen and ammonia (volume ratio) ratio are 2 to 1
In, it nitrogenizes 2-10 minutes.
Step 3: reducing the temperature to 500 DEG C -600 DEG C, pressure 500-600mbar, growth a layer thickness 20-40nm's
Low temperature is nucleated GaN layer.
Step 4: 1000 DEG C -1100 DEG C, pressure 300-600mbar, V/III ratio 1000-3000 are warming up to, growth is high
Pressure, high V/III are than three-dimensional GaN layer, and 1 μm -2 μm of thickness.
Step 5: at 1000 DEG C -1100 DEG C of temperature, pressure 50-200mbar, V/III ratio 50-300, growth low pressure, low
V/III is than two-dimentional GaN layer, and thickness is less than 2 μm.
Step 6: reducing the temperature to 700 DEG C -800 DEG C, grows InGaN layer, wherein In component 5%-20%.Thickness 5-
40nm。
Step 7: being warming up to 1000 DEG C -1100 DEG C, pressure 50-200mbar, V/III ratio 50-300, growth low pressure, low
V/III is than two-dimentional GaN layer, and 2 μm -5 μm of thickness.
Trimethyl gallium is gallium source, and trimethyl indium is indium source, and ammonia is nitrogen source, and carrier gas is hydrogen and nitrogen.
Insert layer, than the high-temperature three-dimensional GaN layer that growth conditions is grown, is given birth in high pressure, high V/III with low pressure, low V/III ratio
Position (Fig. 1) between the high temperature two-dimensional GaN layer of elongate member growth, is 0 μm of the InGaN insert layer thickness；Insert layer exists
Low pressure, low V/III are the InGaN insert layers than GaN layers of intermediate position (Fig. 2) of high temperature two-dimensional that growth conditions is grown
Thickness is less than 2 μm.
Characteristics of the invention are: passing through two-step growth in r surface sapphire substrate using MOCVD growing technology
Method (first growing three-dimensional GaN layer, then grow two-dimentional GaN layer on this basis) simultaneously introduces InGaN insert layer, and InGaN layer is inserted into
To among two-dimentional gallium nitride layer.Currently used method is two-step growth method, the growing three-dimensional under the conditions of high pressure, high V/III ratio
Nonpolar GaN film, although dislocation can be reduced, blocked up three-dimensional GaN growth can bring surface topography coarse, influence
The quality of materials of subsequent growth.Low pressure on this basis grows two-dimentional nonpolar GaN film, Ke Yigai under the conditions of low V/III ratio
Kind surface topography.But, rough surface still higher by the nonpolar GaN film dislocation density that two-step growth method is grown, no
Conducive to the growth of subsequent semiconductor devices.Present invention introduces InGaN insert layer, InGaN insert layer, which has, to be alleviated because lattice is normal
The stress that number is different and generates changes dislocation direction of transfer to the ability of truncation part dislocation, blocks most of sapphire
The transmitting for the threading dislocation that substrate and GaN epitaxial layer mismatch generate.Therefore the nonpolar GaN film dislocation density of growth is lower,
Surface topography is preferable.The deficiency of original two-step growth method can be improved.
Detailed description of the invention:
Fig. 1 is the growth structure schematic diagram being inserted into InGaN insert layer between three-dimensional GaN layer and two-dimentional GaN layer
Fig. 2 is the growth structure schematic diagram that InGaN insert layer is inserted between two-dimentional GaN layer by the present invention
Fig. 3 is to be not inserted into InGaN layer sample (1120) face is along c-axis x-ray diffraction ω scanning figure；
Fig. 4 be inserted into InGaN layer between three-dimensional GaN layer and two-dimentional GaN layer sample (specific implementation case 1) (1120)
Face is along c-axis x-ray diffraction ω scanning figure；
Fig. 5 is be inserted into sample (specific implementation case 2) of the InGaN layer between two-dimentional GaN layer (1120) face is along c-axis x
X ray diffraction ω scanning figure；
Fig. 6 is the atomic force microscopy surface shape appearance figure for being not inserted into InGaN layer sample；
Fig. 7 is the atomic force for being inserted into InGaN layer sample (specific implementation case 1) between three-dimensional GaN layer and two-dimentional GaN layer
Microscopy surface shape appearance figure；
Fig. 8 is the atomic force microscope table for being inserted into sample (specific implementation case 2) of the InGaN layer between two-dimentional GaN layer
Face shape appearance figure.
Specific embodiment
Case 1 is embodied:
InGaN insert layer is inserted into the schematic diagram between three-dimensional GaN layer and two-dimentional GaN layer by Fig. 1
Below with reference to specific implementation case 1, the present invention is further described:
Present case is inserted into r surface sapphire substrate by metal-organic chemical vapor deposition equipment (MOCVD) method
InGaN layer improves the quality of nonpolarity a face GaN film, reduces dislocation density, improves surface topography.As shown in Figure 1, by InGaN
Insert layer is inserted between three-dimensional GaN layer and two-dimentional GaN layer, and steps are as follows for specific experiment:
Step 1: using r surface sapphire substrate, r surface sapphire substrate be put on the substrate bracket in MOCVD reaction chamber,
At 1050 DEG C of temperature, toast 3 minutes.
Step 2: it in 1050 DEG C of temperature, the mixed atmosphere that nitrogen and ammonia volume ratio are 2 to 1, nitrogenizes 10 minutes.
Step 3: 550 DEG C, pressure 500mbar are reduced the temperature to, the low temperature of growth a layer thickness 40nm is nucleated GaN layer.
Step 4: being warming up to 1050 DEG C, and pressure 500mbar, V/III are than 3000, and growth high pressure, high V/III are than three-dimensional
GaN layer, 2 μm of thickness.
Step 5: reducing the temperature to 750 DEG C, grows InGaN insert layer, wherein In component 10%, thickness 20nm.
Step 6: being warming up to 1050 DEG C, and pressure 50mbar, V/III are than 100, and growth low pressure, low V/III are than two-dimentional GaN
Layer, 4 μm of thickness.
Trimethyl gallium is gallium source, and trimethyl indium is indium source, and ammonia is nitrogen source, and carrier gas is hydrogen and nitrogen.
Case 2 is embodied:
Fig. 2 is the growth structure schematic diagram that InGaN buffer layer is inserted between two-dimentional GaN layer by the present invention, specific to walk
It is rapid as follows:
Step 1: using r surface sapphire substrate, r surface sapphire substrate be put on the substrate bracket in MOCVD reaction chamber,
At 1050 DEG C of temperature, toast 3 minutes.
Step 2: it at 1050 DEG C of temperature, in the mixed atmosphere that nitrogen and ammonia proportional volume are 2 to 1, nitrogenizes 10 minutes.
Step 3: 550 DEG C, pressure 500mbar are reduced the temperature to, the low temperature of growth a layer thickness 40nm is nucleated GaN layer.
Step 4: being warming up to 1050 DEG C, and pressure 500mbar, V/III are than 3000, and growth high pressure, high V/III are than three-dimensional
GaN layer, 2 μm of thickness.
Step 5: at 1050 DEG C of temperature, pressure 50mbar, V/III are than 100, and growth low pressure, low V/III are than two-dimentional GaN
Layer, 2 μm of thickness.
Step 6: reducing the temperature to 750 DEG C, grows InGaN layer, wherein In component 10%, thickness 20nm.
Step 7: being warming up to 1050 DEG C, and pressure 50mbar, V/III are than 100, and growth low pressure, low V/III are than two-dimentional GaN
Layer, 4 μm of thickness.
Trimethyl gallium is gallium source, and trimethyl indium is indium source, and ammonia is nitrogen source, and carrier gas is hydrogen and nitrogen.
Test result, Fig. 3 are to be not inserted into InGaN layer sample (1120) face is along c-axis x-ray diffraction ω scanning figure, half-breadth
For 1148arcsec；Fig. 4 is to be inserted into InGaN layer sample (specific implementation case 1) between GaN layers of three-dimensional GaN layer and two dimension
(1120) face reduces along c-axis x-ray diffraction ω scanning figure, half-breadth 1060arcsec than being not inserted into InGaN layer sample half-breadth
88arcsec；Fig. 5 is be inserted into sample (specific implementation case 2) of the InGaN layer between two-dimentional GaN layer (1120) face is along c-axis
X-ray diffraction ω scanning figure, half-breadth 1018arcsec reduce 130arcsec than being not inserted into InGaN layer sample half-breadth.It can
After seeing insertion InGaN layer, half-breadth reduces, and illustrates the dislocation density for reducing material.Fig. 6 is not inserted into InGaN layer sample
Atomic force microscopy surface shape appearance figure, surface Root Mean Square roughness are 1.01nm；Fig. 7 be insertion InGaN layer in three-dimensional GaN layer and
The atomic force microscopy surface shape appearance figure of sample (specific implementation case 1), surface Root Mean Square roughness are between two-dimentional GaN layer
0.76nm；Fig. 8 is the atomic force microscopy surface for being inserted into sample (specific implementation case 2) of the InGaN layer between two-dimentional GaN layer
Shape appearance figure, surface Root Mean Square roughness are 0.70nm, specific implementation case 1 and specific implementation 2 sample of case after being inserted into InGaN layer
Product, reduce roughness, and surface is more flat.
From test result as can be seen that the nonpolar GaN film dislocation density that makes of case study on implementation 1 and case study on implementation 2 compared with
Low, surface topography is preferable.Non-polar GaN quality of materials is improved, the deficiencies in the prior art are improved.
Finally, it should be noted that the above fact case is usual embodiment of the invention, rather than its limitations；It is any right
The simple change or modification that the technical solution of aforementioned each case study on implementation carries out, or some or all of technologies are equal
Replacement, is intended to be included in protection scope of the present invention.
Claims (6)
1. a kind of method that insertion InGaN layer improves non-polar GaN material epitaxy quality, which is characterized in that from bottom to top successively
Are as follows: r surface sapphire substrate；Low temperature GaN nucleating layer；High pressure, high V/III are than high-temperature three-dimensional GaN layer that growth conditions is grown；First
Secondary low pressure, low V/III are than high temperature two-dimensional GaN layer that growth conditions is grown；InGaN insert layer；Second of low pressure, low V/III ratio
The high temperature two-dimensional GaN layer of growth conditions growth；
Either scheme two, from bottom to top successively are as follows: r surface sapphire substrate；Low temperature GaN nucleating layer；High pressure, the life of high V/III ratio
The high-temperature three-dimensional GaN layer of elongate member growth；InGaN insert layer；Low pressure, low V/III are than high temperature two-dimensional GaN that growth conditions is grown
Layer.
2. according to the method described in claim 1, it is characterized by: high pressure, high V/III are than the high-temperature three-dimensional that growth conditions is grown
GaN layer；1000 DEG C -1100 DEG C of temperature, pressure 300-600mbar, V/III ratio 1000-3000,1 μm -2 μm of thickness.
3. according to the method described in claim 1, it is characterized by: first time low pressure, low V/III are higher than what growth conditions was grown
Warm two dimension GaN layer, 1000 DEG C -1100 DEG C of temperature, pressure 50-200mbar, V/III ratio 50-300, thickness is less than 2 μm.
4. according to the method described in claim 1, it is characterized by: InGaN insert layer, 700 DEG C -800 DEG C of growth temperature, thick
5-40nm is spent, the molar percentage of the In component in InGaN layer is in 5%-20%.
5. according to the method described in claim 1, it is characterized by: second of low pressure, low V/III are higher than what growth conditions was grown
Warm two dimension GaN layer, 1000 DEG C -1100 DEG C of temperature, pressure 50-200mbar, V/III ratio 50-300,2 μm -5 μm of thickness.
6. according to the method described in claim 1, it is characterized by: two mesolow of scheme, low V/III are grown than growth conditions
High temperature two-dimensional GaN layer, 1000 DEG C -1100 DEG C of temperature, pressure 50-200mbar, V/III ratio 50-300,2 μm -5 μm of thickness.
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