CN111697427A - Laser diode based on gallium nitride substrate and preparation method thereof - Google Patents

Laser diode based on gallium nitride substrate and preparation method thereof Download PDF

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CN111697427A
CN111697427A CN202010535414.XA CN202010535414A CN111697427A CN 111697427 A CN111697427 A CN 111697427A CN 202010535414 A CN202010535414 A CN 202010535414A CN 111697427 A CN111697427 A CN 111697427A
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贾传宇
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Dongguan University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/30—Structure or shape of the active region; Materials used for the active region
    • H01S5/34—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers
    • H01S5/343—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/20—Structure or shape of the semiconductor body to guide the optical wave ; Confining structures perpendicular to the optical axis, e.g. index or gain guiding, stripe geometry, broad area lasers, gain tailoring, transverse or lateral reflectors, special cladding structures, MQW barrier reflection layers
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    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/30—Structure or shape of the active region; Materials used for the active region
    • H01S5/34—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers
    • H01S5/343—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser
    • H01S5/34333—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser with a well layer based on Ga(In)N or Ga(In)P, e.g. blue laser
    • H—ELECTRICITY
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    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/30—Structure or shape of the active region; Materials used for the active region
    • H01S5/34—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers
    • H01S5/343—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser
    • H01S5/34346—Structure or shape of the active region; Materials used for the active region comprising quantum well or superlattice structures, e.g. single quantum well [SQW] lasers, multiple quantum well [MQW] lasers or graded index separate confinement heterostructure [GRINSCH] lasers in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser characterised by the materials of the barrier layers

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Abstract

The invention discloses a laser diode based on a gallium nitride substrate and a preparation method thereof, wherein the laser diode comprises a GaN single crystal substrate, an n-GaN layer, an n-type limiting layer, a lower composite waveguide layer, a quantum well active region, an electronic barrier layer, an upper composite waveguide layer, a p-type limiting layer and a p-GaN contact layer which are sequentially stacked from bottom to top. The invention can effectively reduce the half-peak width of the laser and improve the beam quality of the laser by optimally designing the structures of the lower composite waveguide layer, the quantum well active region, the electronic barrier layer and the upper composite waveguide layer of the laser.

Description

Laser diode based on gallium nitride substrate and preparation method thereof
Technical Field
The invention relates to the technical field of laser diodes, in particular to a laser diode based on a gallium nitride substrate and a preparation method thereof.
Background
The III-V group nitride semiconductor material is a third generation semiconductor material following silicon and gallium arsenide, comprises gallium nitride (GaN), aluminum nitride (AlN), indium nitride (InN) and alloys thereof, is a direct band gap semiconductor, and has the advantages of large forbidden bandwidth (in the range of 0.7-6.2eV), high breakdown electric field, high thermal conductivity, high electron saturation rate, strong radiation resistance, chemical corrosion resistance and the like. These advantages in optoelectronic properties make III-V nitride materials have a very strong competitive advantage in optoelectronic fields (such as LEDs and LDs), are irreplaceable, and are ideal materials for fabricating semiconductor lasers in the ultraviolet to green wavelength bands.
With the rapid development of laser display technology, the demand for GaN-based lasers has become more urgent. However, the quantum efficiency of the semiconductor laser is low at present, and the half-peak width is between 3nm and 8 nm. Chinese patent application CN110729631A discloses a laser diode based on a gallium nitride single crystal substrate, which has high quantum efficiency, but the half-peak width of the laser is 7nm, which is difficult to meet the current demand. Therefore, it is necessary to develop a laser diode that has a narrower laser half-peak width.
Disclosure of Invention
In order to overcome the defect that the laser in the prior art is wider in half-peak width, the invention provides the laser diode based on the gallium nitride substrate, and the provided laser diode can effectively reduce the half-peak width of the laser and improve the beam quality of the laser.
Another objective of the present invention is to provide a method for preparing the above laser diode based on the gallium nitride substrate.
In order to solve the technical problems, the invention adopts the technical scheme that:
a laser diode based on a gallium nitride substrate comprises a GaN single crystal substrate, an n-GaN layer, an n-type limiting layer, a lower composite waveguide layer, a quantum well active region, an electron blocking layer, an upper composite waveguide layer, a p-type limiting layer and a p-GaN contact layer which are sequentially stacked from bottom to top;
the electron blocking layer is a p-AlGaN/InGaN superlattice with Al components distributed in a bidirectional stepped mode, the number of superlattice cycles is 10-15, and the electron blocking layer comprises a first gradient electron blocking layer, a second gradient electron blocking layer, a third gradient electron blocking layer, a fourth gradient electron blocking layer and a fifth gradient electron blocking layer which are sequentially stacked from bottom to top;
wherein the first gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0-0.05, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the second gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.10, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the third gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.10-0.15, the thickness of AlGaN is 0.5-1.5 nm,the thickness of the GaN is 0.5-1.5 nm; the fourth gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.10, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the fifth gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0-0.05, the thickness of AlGaN is 0.5-1.5 nm, the thickness of GaN is 0.5-1.5 nm, the doping concentration of Mg is 1017～1018cm-3(ii) a The magnesium metallocene is used as a p-type doping source.
Preferably, the lower composite waveguide layer is an InGaN composite waveguide layer with gradient In components, the total thickness is 120-160 nm, and the lower composite waveguide layer comprises a first InGaN layer, a second InGaN layer, a third InGaN layer and a fourth InGaN/GaN superlattice layer which are sequentially stacked from bottom to top;
wherein the thickness of the first InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.01-0.02; the thickness of the InGaN of the second layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.03-0.04; the thickness of the third InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.05-0.06; the fourth layer of InGaN/GaN superlattice has the periodicity of 10, the thickness of InGaN is 1.5-2 nm, the thickness of GaN is 1.5-2 nm, and the ratio of In component content to the total amount of In and Ga is 0.08-0.10; the doping concentration of Si in the GaN barrier layer in the InGaN/GaN superlattice is 1018～1019cm-3(ii) a Silane is used as an n-type doping source.
Preferably, the quantum well active region is an InGaN/GaN quantum well structure with asymmetrically distributed barrier thicknesses, and comprises a first barrier layer, a first well layer, a second barrier layer, a second well layer and a third barrier layer which are sequentially stacked from bottom to top;
wherein the first barrier layer is heavily doped n+-GaN，n+-GaN thickness of 10-15 nm, Si doping concentration of 1018～1019cm-3(ii) a The first well layer is an InGaN well layer, the thickness of the first well layer is 2-3 nm, and the ratio of In component content to the total amount of In and Ga is 0.1-0.3; the second barrier layer is u-InGaN, the thickness of the second barrier layer is 8-10 nm, and the ratio of the In component content to the total amount of In and Ga is 0.005-0.01; the second well layer is an InGaN well layer with the thickness of 3-4 nm, and the In component content accounts for In and GaThe ratio of the total amount is 0.10-0.30; the third barrier layer is non-doped u-InGaN, the thickness is 5-8 nm, and the ratio of the In component content to the total amount of In and Ga is 0.01-0.03; silane is used as an n-type doping source.
Preferably, the upper composite waveguide layer is an InGaN composite waveguide layer with gradient In components, the total thickness is 120-160 nm, and the upper composite waveguide layer comprises a first InGaN/GaN superlattice layer, a second InGaN layer, a third InGaN layer and a fourth InGaN layer which are sequentially stacked from bottom to top;
wherein the first layer of InGaN/GaN superlattice has the periodicity of 10, the thickness of InGaN is 1.5-2 nm, the thickness of GaN is 1.5-2 nm, and the ratio of In component content to the total amount of In and Ga is 0.08-0.10; the thickness of the InGaN of the second layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.04-0.05; the thickness of the third InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.03-0.04; the thickness of the InGaN layer of the fourth layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.02-0.03.
Preferably, the thickness of the n-GaN layer is 2-4 mu m, silane is used as an n-type doping source, and the doping concentration of Si is 1018～1019cm-3。
Preferably, the n-type limiting layer is an n-AlGaN/GaN superlattice, and the number of superlattice cycles is 100-150; the thickness of AlGaN is 2.5-3 nm, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.15, and the thickness of GaN is 2.5-3 nm; silane is used as an n-type doping source, and the doping concentration of Si is 1018～1019cm-3。
Preferably, the p-type limiting layer is a p-AlGaN/GaN superlattice, and the number of superlattice cycles is 100-150; the thickness of AlGaN is 2.5-3 nm, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.15, and the thickness of GaN is 2.5-3 nm; magnesium cyclopentadienyl is used as p-type doping source, and the Mg doping concentration is 1017～1018cm-3。
Preferably, the thickness of the p-GaN contact layer is 100-150 nm; magnesium cyclopentadienyl is used as p-type doping source, and the Mg doping concentration is 1017～1018cm-3。
The invention also provides a preparation method of the laser diode, which comprises the following steps:
s1, carrying out surface activation treatment on a GaN single crystal substrate in a mixed atmosphere of hydrogen and ammonia at the temperature of 900-1100 ℃;
s2, introducing trimethyl gallium as a group III source, ammonia as a group V source and SiH in a hydrogen atmosphere at the temperature of 950-1200 DEG C4As an n-type doping source, growing an n-GaN layer on a GaN single crystal substrate;
s3, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group source and SiH in a hydrogen atmosphere at 850-1050 DEG C4As an n-type doping source, growing an n-type limiting layer on the n-GaN layer;
s4, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources, silane as an n-type doping source, and growing a lower composite waveguide layer on an n-type limiting layer at the temperature of 820-850 ℃;
s5, in a nitrogen atmosphere, introducing trimethyl gallium as a group III source and ammonia as a group V source at the temperature of 750-850 ℃, and growing a quantum well active region on the lower composite waveguide layer;
wherein the growth temperature of the barrier layer is 850-900 ℃, and the growth temperature of the well layer is 750-800 ℃;
s6, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium as p-type doping sources in a nitrogen atmosphere at 850-1050 ℃, and growing an electron blocking layer on the quantum well active region;
s7, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources, and magnesium cyclopentadienyl as p-type doping sources at 820-850 ℃, and growing an upper composite waveguide layer on the electron blocking layer;
s8, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium chloride as p-type doping sources in a hydrogen atmosphere at 850-1050 ℃, and growing a p-type limiting layer on the upper composite waveguide layer;
s9, introducing trimethyl gallium as a group III source, ammonia as a group V source and magnesium chloride as a p-type doping source in a hydrogen atmosphere at the temperature of 950 ℃, and growing a p-GaN contact layer on the p-type limiting layer;
and after the epitaxial growth is finished, reducing the temperature of the reaction chamber to 700-750 ℃, annealing for 5-20 min in a pure nitrogen atmosphere, reducing the temperature to room temperature, and finishing the growth to obtain the laser diode.
Compared with the prior art, the invention has the beneficial effects that:
the laser diode comprises a lower composite waveguide layer, a quantum well active region with InGaN/GaN barrier thicknesses in asymmetric distribution, an electronic barrier layer and an upper composite waveguide layer, and by optimally designing the epitaxial structure of the laser, the half-peak width of the laser can be effectively reduced, and the beam quality of the laser is improved.
Drawings
Fig. 1 is a schematic structural diagram of a gallium nitride substrate-based laser diode according to the present invention.
Fig. 2 is a graph comparing the optical pumping of the laser diodes of example 1 of the present invention and comparative example 1.
Fig. 3 is a graph comparing the optical pumping of the laser diodes of example 2 of the present invention and comparative example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples are all commercially available;
the example preparation process of the present application uses the Aixtron corporation, a tightly coupled vertical reactor MOCVD growth system.
Trimethyl gallium (TMGa), trimethyl indium (TMIn) and trimethyl aluminum (TMAl) are used as a group III source in the growth process, and ammonia gas (NH)3) As group V source, Silane (SiH)4) As n-type doping source, magnesium dicocene (Cp)2Mg) as a p-type doping source.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
A gallium nitride substrate-based laser diode comprises a GaN single crystal substrate 101, an n-GaN layer 102, an n-type confinement layer 103, a lower composite waveguide layer 104, a quantum well active region 105, an electron blocking layer 106, an upper composite waveguide layer 107, a p-type confinement layer 108 and a p-GaN contact layer 109 which are sequentially stacked from bottom to top as shown in FIG. 1.
The laser diode is prepared by the following preparation steps:
s1, firstly, heating to 500 ℃ in a metal organic compound vapor phase epitaxy reaction chamber in a hydrogen atmosphere, then introducing ammonia gas to form a hydrogen and ammonia gas mixed atmosphere, heating to 900 ℃, and carrying out surface activation treatment on a GaN single crystal substrate for 3 min.
S2, in a hydrogen atmosphere, introducing trimethyl gallium as a III-group source, ammonia as a V-group source, silane as an n-type doping source, and growing an n-type GaN layer on a GaN single crystal substrate at the temperature of 950 ℃;
the thickness of the n-GaN layer was 2 μm, and the doping concentration of Si was 1 × 1018cm-3。
S3, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources, silane as n-type doping sources and growing an n-type limiting layer on the n-GaN layer in a hydrogen atmosphere at the temperature of 850 ℃;
the n-type confinement layer is n-AlGaN/GaN superlattice with a superlattice period of 100, AlGaN is 2.5nm, Al component accounts for 0.05 of the total amount of Al and Ga, GaN is 2.5nm, and Si doping concentration is 1 × 1018cm-3。
S4, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III-group sources, ammonia as V-group sources, silane as an n-type doping source, and growing a lower composite waveguide layer on an n-type limiting layer at 820 ℃;
the total thickness of the lower composite waveguide layer is 120nm, and the lower composite waveguide layer comprises a first InGaN layer, a second InGaN layer, a third InGaN layer and a fourth InGaN/GaN superlattice layer which are sequentially stacked from bottom to top;
wherein the thickness of the first InGaN layer is 30nm, and the ratio of the In component content to the total amount of In and Ga is 0.01; the thickness of the second InGaN layer is 30nm, and the ratio of the In component content to the total amount of In and Ga is 0.03; the thickness of the third InGaN layer is 30nm, the ratio of In component content to total amount of In and Ga is 0.05, the fourth layer of InGaN/GaN superlattice has the periodicity of 10, the thickness of InGaN is 1.5nm, the thickness of GaN is 1.5nm, the ratio of In component content to total amount of In and Ga is 0.08, and the doping concentration of Si In the GaN barrier layer In the InGaN/GaN superlattice is 1 × 1018cm-3(ii) a Silane is used as an n-type doping source.
S5, in a nitrogen atmosphere, introducing trimethyl gallium as a group III source, ammonia as a group V source, silane as an n-type doping source, and growing a quantum well active region on the lower composite waveguide layer at the temperature of 750 ℃;
the quantum well active region is an InGaN/GaN quantum well structure with asymmetrically distributed barrier thicknesses and comprises a first barrier layer, a first well layer, a second barrier layer, a second well layer and a third barrier layer which are sequentially stacked from bottom to top;
wherein the first barrier layer is heavily doped n+-GaN，n+GaN thickness of 10nm, growth temperature of 850 ℃ and Si doping concentration of 1 × 1018cm-3(ii) a The first well layer is an InGaN well layer, the thickness is 2nm, the growth temperature is 750 ℃, and the ratio of In component content to the total amount of In and Ga is 0.1; the second barrier layer is u-InGaN, the thickness is 8nm, the growth temperature is 850 ℃, and the ratio of In component content to the total amount of In and Ga is 0.005; the second well layer is an InGaN well layer, the thickness is 3nm, the growth temperature is 750 ℃, and the ratio of In component content to the total amount of In and Ga is 0.1; the third barrier layer is non-doped u-InGaN with the thickness of 5nm, the growth temperature of 850 ℃, and the ratio of In component content to total amount of In and Ga of 0.01.
S6, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium cyclopentadienyl as p-type doping sources in a nitrogen atmosphere at the temperature of 850 ℃, and growing an electron blocking layer on the quantum well active region;
the electron blocking layer is a p-AlGaN/InGaN superlattice distributed in a bidirectional stepped mode, the number of superlattice cycles is 10, and the electron blocking layer comprises a first gradient electron blocking layer, a second gradient electron blocking layer, a third gradient electron blocking layer, a fourth gradient electron blocking layer and a fifth gradient electron blocking layer which are sequentially stacked from bottom to top;
wherein the first gradient electron blocksThe AlGaN/InGaN superlattice with the layer number of cycles of 2, the ratio of Al component content to the total amount of Al and Ga of 0.05, the AlGaN thickness of 0.5nm and the GaN thickness of 0.5nm, the AlGaN/InGaN superlattice with the layer number of cycles of 2, the Al component content to the total amount of Al and Ga of 0.10, the AlGaN thickness of 0.5nm and the GaN thickness of 0.5nm, the AlGaN/InGaN superlattice with the layer number of cycles of 2, the Al component content to the total amount of Al and Ga of 0.15, the AlGaN thickness of 0.5nm and the GaN thickness of 0.5nm, the fourth gradient electron barrier layer to the AlGaN/InGaN superlattice with the layer number of cycles of 2, the ratio of Al component content to the total amount of Al and Ga of 0.10, the AlGaN thickness of 0.5nm, the GaN thickness of 0.5nm, the fifth gradient electron barrier layer to the AlGaN/InGaN superlattice with the layer number of cycles of 2, the Al component content to the total amount of Al and Ga of 0.05, the Mg concentration of 3510 nm and the thickness of 0.5nm17cm-3。
S7, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III-group sources, ammonia as V-group sources and magnesium chloride as a p-type doping source at 820 ℃, and growing an upper composite waveguide layer on the electron blocking layer;
the total thickness of the upper composite waveguide layer is 120nm, and the upper composite waveguide layer comprises a first InGaN/GaN superlattice layer, a second InGaN layer, a third InGaN layer and a fourth InGaN layer which are sequentially stacked from bottom to top;
wherein the first layer of InGaN/GaN superlattice has a cycle number of 10, the thickness of InGaN is 1.5nm, the thickness of GaN is 1.5nm, and the ratio of In component content to the total amount of In and Ga is 0.08; the thickness of the second InGaN layer is 30nm, and the ratio of the In component content to the total amount of In and Ga is 0.04; the thickness of the third layer of InGaN is 30nm, and the ratio of the In component content to the total amount of In and Ga is 0.03; the thickness of the fourth InGaN layer was 30nm, and the ratio of the In component content to the total amount of In and Ga was 0.02.
S8, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium chloride as p-type doping sources in a hydrogen atmosphere at the temperature of 850 ℃, and growing a p-type limiting layer on the upper composite waveguide layer;
the p-type limiting layer is a p-AlGaN/GaN superlattice, and the number of superlattice cycles is 100; AlGaN thickness of 2.5nm, AlThe ratio of the component content to the total amount of Al and Ga is 0.05, the thickness of GaN is 2.5nm, and the Mg doping concentration is 1 × 1017cm-3。
S9, introducing trimethyl gallium as a group III source, ammonia as a group V source and magnesium chloride as a p-type doping source in a hydrogen atmosphere at the temperature of 950 ℃, and growing a p-GaN contact layer on the p-type limiting layer;
the thickness of the p-GaN contact layer is 100nm, the Mg doping concentration is 1 × 1017cm-3；
And after the epitaxial growth is finished, reducing the temperature of the reaction chamber to 700 ℃, annealing for 5min in a pure nitrogen atmosphere, reducing the temperature to room temperature, finishing the growth, and finally preparing the laser diode.
Example 2
A gallium nitride substrate-based laser diode comprises a GaN single crystal substrate 101, an n-GaN layer 102, an n-type confinement layer 103, a lower composite waveguide layer 104, a quantum well active region 105, an electron blocking layer 106, an upper composite waveguide layer 107, a p-type confinement layer 108 and a p-GaN contact layer 109 which are sequentially stacked from bottom to top as shown in FIG. 1.
The laser diode is prepared by the following preparation steps:
s1, firstly, heating to 700 ℃ in a metal organic compound vapor phase epitaxy reaction chamber in a hydrogen atmosphere, then introducing ammonia gas to form a mixed atmosphere of hydrogen gas and ammonia gas, heating to 1100 ℃, and carrying out surface activation treatment on a GaN single crystal substrate for 15 min.
S2, in a hydrogen atmosphere, introducing trimethyl gallium as a III-group source, ammonia as a V-group source, silane as an n-type doping source, and growing an n-type GaN layer on a GaN single crystal substrate at the temperature of 1200 ℃;
the thickness of the n-GaN layer was 4 μm, and the doping concentration of Si was 1 × 1019cm-3。
S3, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources, silane as n-type doping sources and growing an n-type limiting layer on the n-GaN layer in a hydrogen atmosphere at 1050 ℃;
the n-type confinement layer is n-AlGaN/GaN superlattice with the number of superlattice cycles being150, AlGaN thickness of 3nm, Al component content in the total amount of Al and Ga of 0.15, GaN thickness of 3nm, and Si doping concentration of 1 × 1019cm-3。
S4, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources, silane as an n-type doping source, and growing a lower composite waveguide layer on an n-type limiting layer at the temperature of 850 ℃;
the total thickness of the lower composite waveguide layer is 160nm, and the lower composite waveguide layer comprises a first InGaN layer, a second InGaN layer, a third InGaN layer and a fourth InGaN/GaN superlattice layer which are sequentially stacked from bottom to top;
the thickness of the first InGaN layer is 40nm, the ratio of In component content to total amount of In and Ga is 0.02, the thickness of the second InGaN layer is 40nm, the ratio of In component content to total amount of In and Ga is 0.04, the thickness of the third InGaN layer is 40nm, the ratio of In component content to total amount of In and Ga is 0.06, the fourth InGaN/GaN superlattice layer is provided, the periodicity is 10, the thickness of the InGaN layer is 2nm, the thickness of the GaN layer is 2nm, the ratio of In component content to total amount of In and Ga is 0.1, and the doping concentration of Si In the GaN barrier layer In the InGaN/GaN superlattice layer is 1 × 1019cm-3(ii) a Silane is used as an n-type doping source.
S5, in a nitrogen atmosphere, introducing trimethyl gallium as a group III source, ammonia as a group V source, silane as an n-type doping source, and growing a quantum well active region on the lower composite waveguide layer at the temperature of 850 ℃;
the quantum well active region is an InGaN/GaN quantum well structure with asymmetrically distributed barrier thicknesses and comprises a first barrier layer, a first well layer, a second barrier layer, a second well layer and a third barrier layer which are sequentially stacked from bottom to top;
wherein the first barrier layer is heavily doped n+-GaN，n+GaN thickness of 15nm, growth temperature of 900 ℃ and Si doping concentration of 1 × 1019cm-3(ii) a The first well layer is an InGaN well layer, the thickness is 3nm, the growth temperature is 800 ℃, and the ratio of In component content to the total amount of In and Ga is 0.3; the second barrier layer is u-InGaN, the thickness is 10nm, the growth temperature is 900 ℃, and the ratio of In component content to the total amount of In and Ga is 0.01; the second well layer is InGaN well layer with thickness of 4nm, growth temperature of 800 deg.C, and In componentThe ratio of the amount of the indium to the total amount of the gallium is 0.3; the third barrier layer is non-doped u-InGaN, the thickness is 8nm, the growth temperature is 900 ℃, and the ratio of In component content to the total amount of In and Ga is 0.03.
S6, in a nitrogen atmosphere, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as a V group source and magnesium chloride as a p-type doping source at 1050 ℃, and growing an electron blocking layer on the quantum well active region;
the electron blocking layer is a p-AlGaN/InGaN superlattice distributed in a bidirectional stepped mode, the number of superlattice cycles is 15, and the electron blocking layer comprises a first gradient electron blocking layer, a second gradient electron blocking layer, a third gradient electron blocking layer, a fourth gradient electron blocking layer and a fifth gradient electron blocking layer which are sequentially stacked from bottom to top;
the first gradient electron blocking layer is an AlGaN/InGaN superlattice with the periodicity of 3, the ratio of the Al component content to the total amount of Al and Ga is 0.05, the AlGaN thickness is 1.5nm, the GaN thickness is 1.5nm, the second gradient electron blocking layer is an AlGaN/InGaN superlattice with the periodicity of 3, the ratio of the Al component content to the total amount of Al and Ga is 0.05, the AlGaN thickness is 1.5nm, the GaN thickness is 1.5nm, the third gradient electron blocking layer is an AlGaN/InGaN superlattice with the periodicity of 3, the ratio of the Al component content to the total amount of Al and Ga is 0.1, the AlGaN thickness is 1.5nm, the GaN thickness is 1.5nm, the fourth gradient electron blocking layer is an AlGaN/InGaN superlattice with the periodicity of 3, the ratio of the Al component content to the total amount of Al and Ga is 0.05, the AlGaN thickness is 1.5nm, the GaN thickness is 1.5nm, the fifth gradient electron blocking layer is an AlGaN/InGaN superlattice with the periodicity of 3, the Al component content to the total amount of Al and Ga is 0.05, the concentration is 1.5nm, and the thickness of the doped AlGaN is 3518cm-3。
S7, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources and magnesium chloride as a p-type doping source at the temperature of 850 ℃, and growing an upper composite waveguide layer on the electron blocking layer;
the total thickness of the upper composite waveguide layer is 160nm, and the upper composite waveguide layer comprises a first InGaN/GaN superlattice layer, a second InGaN layer, a third InGaN layer and a fourth InGaN layer which are sequentially stacked from bottom to top;
wherein the first layer of InGaN/GaN superlattice has a cycle number of 10, the thickness of InGaN is 2nm, the thickness of GaN is 2nm, and the ratio of In component content to the total amount of In and Ga is 0.1; the thickness of the second InGaN layer is 40nm, and the ratio of the In component content to the total amount of In and Ga is 0.05; the thickness of the third InGaN layer is 40nm, and the ratio of the In component content to the total amount of In and Ga is 0.04; the thickness of the fourth InGaN layer was 40nm, and the ratio of the In component content to the total amount of In and Ga was 0.03.
S8, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium chloride as p-type doping sources in a hydrogen atmosphere at 1050 ℃, and growing a p-type limiting layer on the upper composite waveguide layer;
the p-type confinement layer is p-AlGaN/GaN superlattice with a superlattice period of 150, AlGaN thickness of 3nm, Al component content of 0.15 in total amount of Al and Ga, GaN thickness of 3nm, and Mg doping concentration of 1 × 1018cm-3。
S9, introducing trimethyl gallium as a group III source, ammonia as a group V source and magnesium chloride as a p-type doping source in a hydrogen atmosphere at the temperature of 950 ℃, and growing a p-GaN contact layer on the p-type limiting layer;
the thickness of the p-GaN contact layer is 150nm, the Mg doping concentration is 1 × 1018cm-3；
And after the epitaxial growth is finished, reducing the temperature of the reaction chamber to 750 ℃, annealing for 20min in a pure nitrogen atmosphere, reducing the temperature to room temperature, finishing the growth, and finally preparing the laser diode.
Comparative example 1
Comparative example 1 provides a gallium nitride substrate-based laser diode comprising, stacked in order from bottom to top, a GaN single crystal substrate, an n-GaN layer, an n-type confinement layer, a lower waveguide layer, a quantum well active region, an upper waveguide layer, a p-type confinement layer, and a p-GaN contact layer.
Comparative example 1 differs from example 1 in that:
comparative example 1 no electron blocking layer was present in the structure;
the lower waveguide layer in comparative example 1 is an undoped GaN waveguide layer;
in the comparative example 1, the active region of the quantum well adopts an InGaN/GaN double quantum well structure, wherein the InGaN well layer of the active region grows at a constant temperature, the growth temperature is 750-800 ℃, the growth thickness is 3nm, the ratio of In component content to the total amount of In and Ga is 0.15, the total thickness of GaN In the middle barrier layer is 10nm, the GaN barrier layer grows at a constant temperature, and the growth temperature is 850-900 ℃;
the upper waveguide layer in comparative example 1 was a u-GaN waveguide layer with a thickness of 100 nm.
Performance testing
The gallium nitride-based laser diodes prepared in examples 1 and 2 and comparative example 1 were optically pumped,
optical pumping and lasing: low temperature PL luminescence spectrum, pump laser wavelength 355nm, test conditions: the humidity is 45%; and testing the temperature, wherein the temperature can be regulated and controlled at 5K-300K according to the testing requirement. Specifically, a short-wavelength 355nm violet laser is adopted to irradiate the surface of a long-wavelength laser epitaxial material, atoms are pumped from a low energy state to a high energy state by regulating irradiation energy, and the population inversion is realized so as to maintain energy required by laser operation.
The test results are shown in fig. 2 and 3.
The laser diodes of example 1 and example 2 both had an optical pumping half-width of 3nm, and the laser diode of comparative example 1 had an optical pumping half-width of 8 nm.
The technical scheme of the invention is adopted to prepare the laser diode, so that the half-peak width of the laser can be effectively reduced, the limiting factor of a light field in a laser emission area is improved, the gain of a quantum well active area is improved, and the beam quality of the laser is improved.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. A laser diode based on a gallium nitride substrate is characterized by comprising a GaN single crystal substrate, an n-GaN layer, an n-type limiting layer, a lower composite waveguide layer, a quantum well active region, an electron blocking layer, an upper composite waveguide layer, a p-type limiting layer and a p-GaN contact layer which are sequentially stacked from bottom to top;
the electron blocking layer is a p-AlGaN/InGaN superlattice with Al components distributed in a bidirectional stepped mode, the number of superlattice cycles is 10-15, and the electron blocking layer comprises a first gradient electron blocking layer, a second gradient electron blocking layer, a third gradient electron blocking layer, a fourth gradient electron blocking layer and a fifth gradient electron blocking layer which are sequentially stacked from bottom to top;
wherein the first gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0-0.05, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the second gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.10, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the third gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.10-0.15, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the fourth gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.10, the thickness of AlGaN is 0.5-1.5 nm, and the thickness of GaN is 0.5-1.5 nm; the fifth gradient electron blocking layer is AlGaN/InGaN superlattice with the periodicity of 2-3, the ratio of Al component content to the total amount of Al and Ga is 0-0.05, the thickness of AlGaN is 0.5-1.5 nm, the thickness of GaN is 0.5-1.5 nm, the doping concentration of Mg is 1017～1018cm-3。
2. The laser diode of claim 1, wherein the lower composite waveguide layer is an InGaN composite waveguide layer with gradient In composition, has a total thickness of 120-160 nm, and comprises a first InGaN layer, a second InGaN layer, a third InGaN layer, and a fourth InGaN/GaN superlattice layer which are sequentially stacked from bottom to top;
wherein the thickness of the first InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.01-0.02; the thickness of the InGaN of the second layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.03-0.04; the thickness of the third InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.05-0.06; the fourth layer of InGaN/GaN superlattice has the periodicity of 10, the thickness of InGaN is 1.5-2 nm, the thickness of GaN is 1.5-2 nm, and the ratio of In component content to the total amount of In and Ga is 0.08-0.10; the doping concentration of Si in the GaN barrier layer in the InGaN/GaN superlattice is 1018～1019cm-3。
3. The laser diode of claim 2, wherein the quantum well active region is an InGaN/GaN quantum well structure with asymmetrically distributed barrier thicknesses, and comprises a first barrier layer, a first well layer, a second barrier layer, a second well layer, and a third barrier layer, which are sequentially stacked from bottom to top;
wherein the first barrier layer is heavily doped n+-GaN，n+-GaN thickness of 10-15 nm, Si doping concentration of 1018～1019cm-3(ii) a The first well layer is an InGaN well layer, the thickness of the first well layer is 2-3 nm, and the ratio of In component content to the total amount of In and Ga is 0.1-0.3; the second barrier layer is u-InGaN, the thickness of the second barrier layer is 8-10 nm, and the ratio of the In component content to the total amount of In and Ga is 0.005-0.01; the second well layer is an InGaN well layer, the thickness of the second well layer is 3-4 nm, and the ratio of In component content to the total amount of In and Ga is 0.10-0.30; the third barrier layer is non-doped u-InGaN, the thickness is 5-8 nm, and the ratio of In component content to the total amount of In and Ga is 0.01-0.03.
4. The laser diode of claim 3, wherein the upper composite waveguide layer is an InGaN composite waveguide layer with gradient In composition, has a total thickness of 120-160 nm, and comprises a first InGaN/GaN superlattice layer, a second InGaN layer, a third InGaN layer and a fourth InGaN layer which are sequentially stacked from bottom to top;
wherein the first layer of InGaN/GaN superlattice has the periodicity of 10, the thickness of InGaN is 1.5-2 nm, the thickness of GaN is 1.5-2 nm, and the ratio of In component content to the total amount of In and Ga is 0.08-0.10; the thickness of the InGaN of the second layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.04-0.05; the thickness of the third InGaN layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.03-0.04; the thickness of the InGaN layer of the fourth layer is 30-40 nm, and the ratio of the In component content to the total amount of In and Ga is 0.02-0.03.
5. The laser diode of claim 4, wherein the n-GaN layer has a thickness of 2-4 μm and a Si doping concentration of 1018～1019cm-3。
6. The laser diode of claim 5, wherein the n-type confinement layer is an n-AlGaN/GaN superlattice, and the number of superlattice periods is 100-150; the thickness of AlGaN is 2.5-3 nm, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.15, the thickness of GaN is 2.5-3 nm, and the doping concentration of Si is 1018～1019cm-3。
7. The laser diode of claim 6, wherein the p-type confinement layer is a p-AlGaN/GaN superlattice, and the number of superlattice periods is 100-150; the thickness of AlGaN is 2.5-3 nm, the ratio of Al component content to the total amount of Al and Ga is 0.05-0.15, the thickness of GaN is 2.5-3 nm, and the doping concentration of Mg is 1017～1018cm-3。
8. The laser diode of claim 7, wherein the p-GaN contact layer has a thickness of 100-150 nm and a Mg doping concentration of 1017～1018cm-3。
9. A method of manufacturing a laser diode as claimed in claim 8, comprising the steps of:
s1, carrying out surface activation treatment on a GaN single crystal substrate in a mixed atmosphere of hydrogen and ammonia at the temperature of 900-1100 ℃;
s2, introducing the mixture into a hydrogen atmosphere at the temperature of 950-1200 DEG CTrimethyl gallium as group III source, ammonia as group V source, SiH4As an n-type doping source, growing an n-GaN layer on a GaN single crystal substrate;
s3, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group source and SiH in a hydrogen atmosphere at 850-1050 DEG C4As an n-type doping source, growing an n-type limiting layer on the n-GaN layer;
s4, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources, silane as an n-type doping source, and growing a lower composite waveguide layer on an n-type limiting layer at the temperature of 820-850 ℃;
s5, in a nitrogen atmosphere, introducing trimethyl gallium as a group III source and ammonia as a group V source at the temperature of 750-850 ℃, and growing a quantum well active region on the lower composite waveguide layer;
wherein the growth temperature of the barrier layer is 850-900 ℃, and the growth temperature of the well layer is 750-800 ℃;
s6, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium as p-type doping sources in a nitrogen atmosphere at 850-1050 ℃, and growing an electron blocking layer on the quantum well active region;
s7, in a nitrogen atmosphere, introducing trimethyl gallium and trimethyl indium as III group sources, ammonia as V group sources, and magnesium cyclopentadienyl as p-type doping sources at 820-850 ℃, and growing an upper composite waveguide layer on the electron blocking layer;
s8, introducing trimethyl gallium, trimethyl aluminum and trimethyl indium as III group sources, ammonia as V group sources and magnesium chloride as p-type doping sources in a hydrogen atmosphere at 850-1050 ℃, and growing a p-type limiting layer on the upper composite waveguide layer;
and S9, introducing trimethyl gallium as a group III source, ammonia as a group V source and magnesium as a p-type doping source in a hydrogen atmosphere at the temperature of 950 ℃, and growing a p-GaN contact layer on the p-type limiting layer to obtain the laser diode.
10. The method of claim 9, wherein the steps S1 to S9 are performed in a metal-organic compound vapor phase epitaxy reaction chamber.
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