CN113764549A - Preparation method of light-emitting diode - Google Patents
Preparation method of light-emitting diode Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 230000004888 barrier function Effects 0.000 claims abstract description 121
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 230000000903 blocking effect Effects 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010030 laminating Methods 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 330
- 229910002601 GaN Inorganic materials 0.000 description 104
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 30
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 23
- 238000000151 deposition Methods 0.000 description 23
- 230000008021 deposition Effects 0.000 description 21
- 238000012360 testing method Methods 0.000 description 19
- 229910021529 ammonia Inorganic materials 0.000 description 14
- 239000007771 core particle Substances 0.000 description 14
- 238000004020 luminiscence type Methods 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 229910052594 sapphire Inorganic materials 0.000 description 8
- 239000010980 sapphire Substances 0.000 description 8
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 230000007547 defect Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
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- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
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Abstract
The invention belongs to the technical field of semiconductor lighting, and particularly relates to a preparation method of a light-emitting diode. The preparation method of the light emitting diode provided by the invention comprises the steps of sequentially preparing an undoped GaN layer, an N-type GaN layer, a quantum well barrier light emitting layer, an electronic barrier layer and a P-type GaN layer on the surface of a substrate, wherein the quantum well barrier light emitting layer is prepared by alternately laminating a quantum well layer and a quantum barrier layer, the quantum well layer and the quantum barrier layer have the same layer number, the quantum well layer in the outer layer is in contact with the N-type GaN layer, the preparation method of the quantum well layer is a metal organic chemical vapor deposition method, and the preparation method of the quantum barrier layer is a molecular beam epitaxy method. The LED obtained by the preparation method provided by the invention has the advantages that the blue shift and the half-peak width are not obviously increased along with the increase of the working current, the light-emitting concentration of the LED is improved, and the light-emitting brightness is improved.
Description
Technical Field
The invention belongs to the technical field of semiconductor lighting, and particularly relates to a preparation method of a light-emitting diode.
Background
The semiconductor Light Emitting Diode (LED) has the advantages of small volume, firmness, durability, strong controllability of light emitting wave band, high lighting effect, low heat loss, small light attenuation, energy conservation, environmental protection and the like, has wide application in the fields of full-color display, backlight source, signal lamp, photoelectric computer interconnection, short-distance communication and the like, and gradually becomes a hotspot of research in the field of the current electronic electromechanics. The gallium nitride material has a series of advantages of wide band gap, high electron mobility, high thermal conductivity, high stability and the like, so that the gallium nitride material has wide application and huge market prospect in the aspects of short-wavelength light-emitting devices, light detection devices and high-power devices.
In general, an LED includes an N-type substrate, an undoped GaN layer (U-GaN) formed on the substrate, an N-type GaN layer (N-GaN layer), a quantum well barrier layer light emitting layer, an electron blocking layer, and a P-type GaN layer (P-GaN layer).
At present, in the prior art, a Metal Organic Chemical Vapor Deposition (MOCVD) is adopted to prepare an LED, and as the working current of the prepared LED chip increases, the blue shift during light emission becomes large, so that the light emission concentration of the LED chip is poor, and the brightness is low.
Disclosure of Invention
In view of this, the invention provides a method for manufacturing a light emitting diode, and the blue shift of the LED manufactured by the method provided by the invention does not increase significantly with the increase of the working current.
The invention provides a preparation method of a light-emitting diode, which comprises the steps of sequentially preparing an undoped GaN layer, an N-type GaN layer, a quantum well barrier light-emitting layer, an electronic barrier layer and a P-type GaN layer on the surface of a substrate, wherein the quantum well barrier light-emitting layer is prepared by alternately laminating a quantum well layer and a quantum barrier layer, the quantum well layer and the quantum barrier layer have the same layer number, the quantum well layer in contact with the N-type GaN layer is a quantum well layer positioned at the outer layer, the preparation method of the quantum well layer is a metal organic chemical vapor deposition method, and the preparation method of the quantum barrier layer is a molecular beam epitaxy method.
Preferably, the temperature for preparing the quantum well layer is 750-770 ℃ independently, and the temperature for preparing the quantum barrier layer is 260-750 ℃ independently.
Preferably, the temperature for preparing the quantum barrier layer is 250-420 ℃.
Preferably, the number of the quantum barrier layers is 3-20.
Preferably, the quantum barrier layer comprises a first GaN layer, an AlN layer, and Al stacked in this orderXGa1-XN layer and second GaN layer, the AlxGa1-xIn the N layer, x is more than or equal to 0 and less than 1.
Preferably, the thickness of the first GaN layer is 0.5-1.5 nm, the thickness of the AlN layer is 0.5-1 nm, and the Al layer isXGa1-XThe thickness of the N layer is 0.5-5 nm, and the thickness of the second GaN layer is 6-8 nm.
Preferably, the Al isXGa1-XIn the N layer, x is more than or equal to 0.1 and less than 0.15.
Preferably, the thickness of each quantum barrier layer is independently 2-16 nm.
Preferably, the thickness of each quantum well layer is 4-7 nm independently.
Preferably, the thickness of the substrate is 650-660 mu m, the thickness of the non-doped GaN layer is 1000-2500 nm, the thickness of the N-type GaN layer is 800-1500 nm, the thickness of the electron blocking layer is preferably 100-130 nm, and the thickness of the P-GaN layer is preferably 150-350 nm.
The invention provides a preparation method of a light-emitting diode, which comprises the steps of sequentially preparing an undoped GaN layer, an N-type GaN layer, a quantum well barrier light-emitting layer, an electronic barrier layer and a P-type GaN layer on the surface of a substrate, wherein the quantum well barrier light-emitting layer is prepared by alternately laminating a quantum well layer and a quantum barrier layer, the quantum well layer and the quantum barrier layer have the same layer number, the quantum well layer in contact with the N-type GaN layer is a quantum well layer positioned at the outer layer, the preparation method of the quantum well layer is a metal organic chemical vapor deposition method, and the preparation method of the quantum barrier layer is a molecular beam epitaxy method. According to the preparation method provided by the invention, the quantum well layer with few defects is prepared by adopting MOCVD, and then the quantum barrier layer is prepared by adopting a Molecular Beam Epitaxy (MBE) method with the preparation temperature lower than that of MOCVD, so that the defect that the quantum well layer forms a V-shaped pit when the quantum barrier layer is prepared in a high-temperature environment can be effectively avoided, the adverse effect of the quantum well defect on the growth structure of the quantum barrier is reduced, and the crystal quality of the quantum barrier is improved; meanwhile, the quantum barrier layer prepared by the MBE method can effectively cover the V-shaped pit defect of the quantum well layer, the overall performance of the LED crystal structure is improved, the blue shift and the half-peak width of the obtained LED are not obviously increased along with the increase of the working current, and the light-emitting concentration of the light-emitting diode is improved, so that the light-emitting brightness is improved.
The preparation method provided by the invention is convenient to operate, simple in process flow and strong in controllability.
Drawings
FIG. 1 is a schematic structural diagram of a light emitting diode prepared according to the present invention;
FIG. 2 is a schematic diagram showing the temperature variation curve with thickness of a quantum well barrier light-emitting layer prepared by the preparation method of comparative example 1;
fig. 3 is a schematic diagram of a temperature variation curve with thickness of a quantum well barrier light emitting layer prepared by the preparation method provided in embodiment 1 of the present invention.
Detailed Description
The invention provides a preparation method of a light-emitting diode, which comprises the steps of sequentially preparing an undoped GaN layer, an N-type GaN layer, a quantum well barrier light-emitting layer, an electronic barrier layer and a P-type GaN layer on the surface of a substrate, wherein the quantum well barrier light-emitting layer is prepared by alternately laminating a quantum well layer and a quantum barrier layer, the quantum well layer and the quantum barrier layer have the same layer number, the quantum well layer in contact with the N-type GaN layer is a quantum well layer positioned at the outer layer, the preparation method of the quantum well layer is a metal organic chemical vapor deposition method, and the preparation method of the quantum barrier layer is a molecular beam epitaxy method.
The invention has no special requirement on the material of the substrate, in the specific embodiment of the invention, the substrate is sapphire, and the thickness of the substrate is preferably 650-660 mu m.
The substrate is preferably purified, in a specific embodiment of the invention, the purification is preferably performed in an MOCVD reaction chamber, the purified atmosphere is preferably a hydrogen atmosphere, and the flow rate of hydrogen is preferably 100-150L/min, and more preferably 120L/min; the pressure of the purification is preferably 150-250 Torr, and more preferably 200 Torr; the purification temperature is preferably 1000-1200 ℃, and more preferably 1080 ℃; the heat preservation time of the purification is preferably 200-350 s, and more preferably 300 s; the heating rate from room temperature to the purification temperature is preferably 70-100 ℃/min, more preferably 80 ℃/min.
After the purified substrate is obtained, the U-GaN layer is prepared on the surface of the substrate. In the present invention, the method of preparing the UGaN layer is preferably MOCVD. In the present invention, the preparation parameters when the U-GaN layer is prepared by MOCVD preferably include: the deposition temperature is preferably 1000-1100 ℃, and more preferably 1050 ℃; the deposition atmosphere is preferably a mixed atmosphere of nitrogen, hydrogen and ammonia, the flow ratio of the nitrogen, the hydrogen and the ammonia is preferably (60-80): 100-200): 40-80, and more preferably 75:150: 56; the pressure of the mixed atmosphere is preferably 350-600 Torr, and more preferably 450 Torr; the rotating speed of the rotating disc during deposition is preferably 1000-2000 r/min, and more preferably 1100 r/min. The invention has no special requirements on the deposition time.
The invention takes trimethyl gallium (TMGa) as a Ga source and ammonia (NH)3) And depositing a U-GaN layer for the N source, wherein in the specific embodiment of the invention, the thickness of the U-GaN layer is preferably 1000-2500 nm.
After the U-GaN layer is obtained, the N-GaN layer is prepared on the surface of the U-GaN layer. In the present invention, the method of preparing the N-GaN layer is preferably MOCVD. In the present invention, the preparation parameters when the N-GaN layer is prepared by MOCVD preferably include: the deposition temperature is preferably 1000-1100 ℃, more preferably 1050 ℃, the deposition atmosphere is preferably a mixed atmosphere of nitrogen, hydrogen and ammonia, the flow ratio of the nitrogen, the hydrogen and the ammonia is preferably (60-80): 100-200): 40-80, more preferably 64:120:50, the pressure of the mixed atmosphere is preferably 150-400 Torr, more preferably 200Torr, and the rotating speed of the rotating disc during deposition is preferably 1000-2000 r/min, more preferably 1100r/min, and the invention has no special requirement on the deposition time.
In the specific embodiment of the invention, the N-GaN layer is preferably a Si-doped gallium nitride layer, and the invention takes trimethyl gallium (TMGa) as a Ga source and ammonia (NH)3) Deposition for N source with simultaneous incorporation of silaneAnd doping Si to obtain the U-GaN layer, wherein the doping amount of the Si is not specially required. In the invention, the thickness of the N-GaN layer is preferably 800-1500 nm.
After the N-GaN layer is obtained, the quantum well barrier light-emitting layer is prepared on the surface of the N-GaN layer, the quantum well barrier light-emitting layer is prepared and comprises a quantum well layer and a quantum barrier layer which are prepared in an interval laminating mode, the number of layers of the quantum well layer is the same as that of the quantum barrier layer, the quantum well layer positioned on the outer layer is prepared on the surface of the N-type GaN layer, the quantum well layer is prepared through a metal organic chemical vapor deposition method, and the quantum barrier layer is prepared through a molecular beam epitaxy method.
In the invention, the quantum well layer positioned on the outer layer is prepared on the surface of the N-GaN layer, the method for preparing the quantum well layer is MOCVD, and the preparation parameters when the MOCVD is adopted to prepare the quantum well layer on the outer layer preferably comprise: the deposition temperature is preferably 750-770 ℃, the deposition atmosphere is preferably a mixed atmosphere of nitrogen and ammonia, the flow ratio of the nitrogen to the ammonia is preferably (60-80): 10-50), and more preferably 72:40, the pressure of the mixed atmosphere is preferably 150-300 Torr, and more preferably 200Torr, the rotating speed of a rotating disc during deposition is preferably 1000-2000 r/min, and more preferably 1100r/min, and the invention has no special requirement on the deposition time.
The quantum well layer is prepared by preferably using TEGA and TMIN as raw materials; in the present invention, the material of the quantum well layer is preferably InxGa1-xN, 0 < x < 1, and In one embodiment of the present invention, the quantum well layer is In0.25Ga0.75N; in the invention, the thickness of the single quantum well layer is preferably 4-7 nm, and more preferably 5-6 nm.
After the quantum well layer positioned on the outer layer is obtained, the quantum well positioned on the outer layer is preferably cooled, nitrogen and ammonia gas are preferably introduced into the reaction chamber for cooling, and the flow ratio of the nitrogen to the ammonia gas is preferably (60-80): 10-50, and more preferably 72: 40. After the temperature is reduced to room temperature, the semi-finished product LED prepared is taken out from the reaction chamber.
To obtain the outer layerAfter the quantum well layer of the layer is formed, the quantum barrier layer is prepared on the surface of the quantum well of the outer layer, the method for preparing the quantum barrier layer is a molecular beam epitaxy method, and in the invention, the preparation of the quantum barrier layer preferably comprises the sequential lamination preparation of a first GaN layer, an AlN layer and AlXGa1-XAn N layer and a second GaN layer.
In the present invention, the first GaN layer is prepared on the surface of the quantum well layer, in the present invention, the method for preparing the first GaN layer is a molecular beam epitaxy method, and in the present invention, the preparation parameters when the first GaN layer is prepared by the molecular beam epitaxy method preferably include: the temperature is preferably 260-750 ℃, more preferably 250-420 ℃, the atmosphere is preferably a vacuum atmosphere, and the pressure of the vacuum atmosphere is preferably 1 x 10-8~5×10-8Torr, the present invention has no special requirement on the preparation time.
In an embodiment of the present invention, the thickness of the first GaN layer is preferably 0.5 to 1.5nm, and more preferably 0.8 to 1.2 nm.
After the first GaN layer is obtained, the AlN layer is prepared on the surface of the first GaN layer, in the invention, the method for preparing the AlN layer is a molecular beam epitaxy method, and in the invention, the preparation parameters when the AlN layer is prepared by the molecular beam epitaxy method preferably include: the temperature is preferably 260-750 ℃, more preferably 250-420 ℃, the atmosphere is preferably a vacuum atmosphere, and the pressure of the vacuum atmosphere is preferably 1 x 10-8~5×10-8Torr, the present invention has no special requirement on the preparation time.
In the present invention, the AlN layer has a thickness of preferably 0.5 to 1nm, more preferably 0.6 to 0.8 nm.
After an AlN layer is obtained, the Al is prepared on the surface of the AlN layerXGa1-XN layer, in the present invention, the Al is preparedXGa1-XThe method of the N layer is a molecular beam epitaxy method, and in the invention, the Al layer is prepared by the molecular beam epitaxy methodXGa1-XThe preparation parameters for the N layer preferably include: the temperature is preferably 260-750 ℃, more preferably 250-420 ℃, the atmosphere is preferably a vacuum atmosphere, and the pressure of the vacuum atmosphere is preferably 1 x 10-8~5×10-8Torr, the present invention has no special requirement on the preparation time.
In the present invention, the AlXGa1-XIn the N layer, 0. ltoreq. x < 1, preferably 0.1. ltoreq. x < 0.15, and in a specific embodiment of the present invention, the AlXGa1-XN is specifically Al0.1Ga0.9N; in the present invention, the AlXGa1-XThe thickness of the N layer is preferably 0.5 to 5nm, and more preferably 0.8 to 3 nm.
To obtain AlXGa1-XAfter N layer, the invention is on the AlXGa1-XPreparing the second GaN layer on the surface of the N layer, wherein the method for preparing the second GaN layer is a molecular beam epitaxy method, and the preparation parameters when the molecular beam epitaxy method is adopted for preparing the second GaN layer preferably comprise the following steps: the temperature is preferably 260-750 ℃, more preferably 250-420 ℃, the atmosphere is preferably a vacuum atmosphere, and the pressure of the vacuum atmosphere is preferably 1 x 10-8~5×10-8Torr, the present invention has no special requirement on the preparation time.
In the present invention, the thickness of the second GaN layer is preferably 6 to 8nm, more preferably 6.5 to 7.5nm, and the time for the preparation is preferably one.
In the invention, the thickness of the single-layer quantum barrier layer is preferably 2-16 nm, and more preferably 2.5-15 nm.
After the quantum well layer and the quantum barrier layer are obtained, on the surface of the quantum barrier layer, the preparation processes of the quantum well layer and the quantum barrier layer are repeated, the quantum well layer and the quantum barrier layer are prepared at intervals in a laminated mode, the quantum well barrier light-emitting layer is obtained, the number of layers of the quantum well layer and the quantum barrier layer is the same, the number of layers of the quantum barrier layer is preferably 3-20, more preferably 4-15, and most preferably 5 or 6.
In the invention, the thickness of each quantum well layer and each quantum barrier layer can be the same or different.
After the quantum well barrier light-emitting layer is obtained, preparing the electron barrier layer on the surface of the quantum well barrier light-emitting layer; in the present invention, the method for preparing the electron blocking layer is preferably MOCVD, and in the present invention, the preparation parameters when MOCVD is used for preparing the electron blocking layer preferably include: the deposition temperature is preferably 900-1050 ℃, the deposition atmosphere is preferably a mixed atmosphere of nitrogen and ammonia, the flow ratio of the nitrogen to the ammonia is preferably (80-120): 5-20), more preferably 105:10, the pressure of the mixed atmosphere is preferably 150-300 Torr, more preferably 200Torr, the rotating speed of the rotating disc during deposition is preferably 1000-2000 r/min, more preferably 1100r/min, and the invention has no special requirement on the deposition time.
In the present invention, the material of the electron blocking layer is preferably AlxGa1-xN, x is more than 0 and less than 1; the invention takes trimethyl gallium (TMGa) as a Ga source, AlN as an Al source and ammonia (NH)3) Deposition of Al for N sourcexGa1-xAn N layer, wherein in one embodiment of the present invention, the electron blocking layer is made of Al0.12Ga0.88N; in the invention, the thickness of the electron blocking layer is preferably 100-130 nm, and more preferably 110-120 nm.
After the electron blocking layer is obtained, preparing the P-GaN layer on the surface of the electron blocking layer; in the present invention, the method for preparing the P-GaN layer is preferably MOCVD, and in the present invention, the preparation parameters when MOCVD is used to prepare the P-GaN layer preferably include: the deposition temperature is preferably 950-1100 ℃, the deposition atmosphere is preferably a mixed atmosphere of nitrogen, hydrogen and ammonia, the flow ratio of the nitrogen, the hydrogen and the ammonia is preferably (60-80): 100-200): 40-80, and more preferably 64:120:50, the pressure of the mixed atmosphere is preferably 150-400 Torr, more preferably 200Torr, and the rotating speed of the rotating disc during deposition is preferably 1000-2000 r/min, more preferably 1100r/min, and the invention has no special requirement on the preparation time.
In the invention, the P-GaN layer is preferably Mg-doped P-type GaN, trimethyl gallium (TMGa) is taken as a Ga source, CP2MG is taken as a Mg source, and ammonia (NH) is taken3) The method comprises the step of depositing a P-GaN layer for an N source, wherein the thickness of the P-GaN layer is preferably 150-350 nm.
According to the preparation method provided by the invention, the quantum well layer with high quality is prepared by adopting MOCVD, and then the quantum barrier layer is prepared by adopting a Molecular Beam Epitaxy (MBE) method with the preparation temperature lower than that of MOCVD, so that the defect that the quantum well layer forms a V-shaped pit when the quantum barrier layer is prepared in a high-temperature environment can be effectively avoided, the adverse effect of the defect of the quantum well on the growth structure of the quantum barrier is reduced, and the crystal quality of the quantum barrier is improved; meanwhile, the quantum barrier layer prepared by the MBE method can effectively cover the V-shaped pit defect of the quantum well layer, the overall performance of the LED crystal structure is improved, the blue shift and the half-peak width of the obtained LED are not obviously increased along with the increase of the working current, and the light-emitting concentration of the light-emitting diode is improved, so that the light-emitting brightness is improved.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 300 deg.C, and a 1nm first GaN layer, a 1nmAl N layer, and a 3nmAl layer were grown in this order0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 530nm, the working voltage is 2.8V, the light-emitting brightness is 15mW, the half-peak width is 32.5nm, the blue shift is 9nm, the working current is adjusted to 30mA, the light-emitting wavelength of the test core particle is 531nm, the working voltage is 2.81V, the light-emitting brightness is 15.2mW, the half-peak width is 32.7nm, and the blue shift is 9.1 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.85V, the luminescence brightness was 15.5mW, the half-peak width was 33nm, and the blue-shift was 9.3 nm.
Example 2
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 350 ℃, and a 1nm first GaN layer, a 1nmAl N layer, and a 3nmAl layer were grown in this order0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 529.5nm, the working voltage is 2.8V, the light-emitting brightness is 15.5mW, the half-peak width is 32nm, the blue shift is 8.8nm, the working current is adjusted to 30mA, the light-emitting wavelength of the test core particle is 530nm, the working voltage is 2.81V, the light-emitting brightness is 15.7mW, the half-peak width is 32.5nm, and the blue shift is 9 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 531nm, the working voltage was 2.84V, the luminescence brightness was 16mW, the half-peak width was 33nm, and the blue-shift was 9.1 nm.
Example 3
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 400 ℃ in this orderA first GaN layer of 1nm length, a 1nmAl N layer, and a 3nmAl layer0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 528.5nm, the working voltage is 2.8V, the light-emitting brightness is 16mW, the half-peak width is 32.5nm, the blue shift is 8.9nm, the working current is adjusted to 30mA, the light-emitting wavelength of the test core particle is 529.5nm, the working voltage is 2.81V, the light-emitting brightness is 16.5mW, the half-peak width is 32.4nm, and the blue shift is 9 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.85V, the luminescence brightness was 16.9mW, the half-peak width was 32.8nm, and the blue shift was 9.2 nm.
Example 4
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of (2) was 56L/min, the pressure in the reaction chamber was 450Torr, and the carrier plate rotation speed was controlledThe U-GaN layer of undoped gallium nitride with the thickness of 1200nm is grown at 1100 r/min.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 500 deg.C, and a 1nm first GaN layer, a 1nmAl N layer, and a 3nmAl layer were grown in this order0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 528nm, the working voltage is 2.8V, the light-emitting brightness is 14.5mW, the half-peak width is 32nm, the blue shift is 9nm, the working current is adjusted to 30mA, the light-emitting wavelength of the tested core particle is 532nm, the working voltage is 2.82V, the light-emitting brightness is 15mW, the half-peak width is 33.5nm, and the blue shift is 9.5 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.84V, the luminescence brightness was 15.7mW, the half-peak width was 35nm, and the blue-shift was 10.5 nm.
Example 5
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 650 ℃ to grow a 1nm first GaN layer, a 1nmAl N layer, and a 3nmAl layer in this order0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 530nm, the working voltage is 2.8V, the light-emitting brightness is 14.5mW, the half-peak width is 32nm, the blue shift is 9nm, the working current is adjusted to 30mA, the light-emitting wavelength of the tested core particle is 532nm, the working voltage is 2.82V, the light-emitting brightness is 15mW, the half-peak width is 33.5nm, and the blue shift is 9.5 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.84V, the luminescence brightness was 15.7mW, the half-peak width was 35nm, and the blue-shift was 10.5 nm.
Example 6
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of (2) was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was carried out.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of120L/min,NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N, after the growth is finished, N is added2Flow rate of 72L/min, NH3The flow rate is 5L/min, the temperature of the cavity is reduced, and the epitaxial wafer is taken out after the temperature is reduced to the normal temperature.
Putting the epitaxial wafer of the quantum barrier to be grown into molecular beam epitaxy equipment, and setting the vacuum of the cavity at 3 multiplied by 10- 8Torr, the substrate temperature was set at 750 deg.C, and a 1nm first GaN layer, a 1nmAl N layer, and a 3nmAl layer were grown in this order0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm. After the growth is finished, the N2 is introduced for cooling, and the epitaxial wafer is taken out.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (1) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and AL was grown0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were performed on the light emitting diode of this example:
the light-emitting diode prepared in the embodiment is manufactured into a chip with the size of 171 mu m multiplied by 214 mu m, 20mA of current is introduced, the light-emitting wavelength is 527nm, the working voltage is 2.8V, the light-emitting brightness is 13mW, the half-peak width is 34.5nm, the blue shift is 9.8nm, the working current is adjusted to 30mA, the light-emitting wavelength of the test core particle is 531nm, the working voltage is 2.81V, the light-emitting brightness is 13.2mW, the half-peak width is 34.7nm, and the blue shift is 10 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.85V, the luminescence brightness was 13.5mW, the half-peak width was 35.8nm, and the blue shift was 10.5 nm.
Comparative example 1
Placing a sapphire (PSS) substrate in an MOCVD reaction chamber, H2The flow rate of the reaction chamber was 120L/min, the pressure in the reaction chamber was 200Torr, the temperature was raised to 1080 ℃ at 80 ℃/min, and the substrate was stabilized for 300 seconds, and high-temperature cleaning was performed.
The temperature of the reaction chamber is raised to 1050 ℃, N2Flow rate of 75L/min, H2Flow rate of 150L/min, NH3The flow rate of the reaction chamber is 56L/min, the pressure of the reaction chamber is 450Torr, the rotating speed of the carrier disc is controlled at 1100r/min, and an undoped gallium nitride U-GaN layer with the thickness of 1200nm is grown.
The temperature was maintained at 1050 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of (A) was 50L/min, the pressure in the reaction chamber was controlled at 200Torr, and an N-type gallium nitride N-GaN layer having a thickness of 1000nm was grown.
Controlling the temperature at 750 ℃ and N2Flow rate of 72L/min, NH3The flow rate of (2) was 40L/min, the pressure IN the reaction chamber was 200Torr, and a quantum well was grown at 750 ℃ with a quantum well layer of IN grown to a thickness of 5.0nm0.25GA0.75N。
Controlling the temperature to be 850-880 ℃, N2Flow rate of 72L/min, NH3The flow rate of (2) was 60L/min, the pressure in the reaction chamber was 200Torr, and 1nm of the first GaN layer, 1nmAl N layer, and 3nmAl layer were grown in this order at ℃0.1GA0.9The quantum barrier layer comprises an N layer and a 6nm second GaN layer, and the total thickness of the quantum barrier layer is 11 nm.
And repeatedly growing the quantum well layer and the quantum barrier layer at intervals, and growing 6 quantum well layers and 6 quantum barrier layers in total to obtain the quantum well barrier light-emitting layer.
Putting the epitaxial wafer on which the quantum well barrier light-emitting layer grows into the MOCVD equipment again, raising the temperature to 900 ℃, and raising the temperature to N2Flow rate of 105L/min, NH3The flow rate of (A) was 10L/min, the pressure in the reaction chamber was controlled at 200Torr, and the reaction was carried outLong AL0.12GA0.88And N layers, wherein the thickness is controlled to be 120 nm.
The temperature is raised to 950 ℃ N2Flow rate of 64L/min, H2Flow rate of 120L/min, NH3The flow rate of the reaction chamber was 50L/min, the pressure of the reaction chamber was controlled at 200Torr, and a Mg-doped P-type gallium nitride P-GaN layer was grown to a thickness of 200 nm.
The following tests were carried out on the light emitting diode of this comparative example:
the light emitting diode prepared by the comparative example was fabricated into a 171 μm × 214 μm chip, and a current of 20mA was applied, the light emitting wavelength was 530nm, the operating voltage was 2.8V, the light emitting luminance was 14.5mW, the half-peak width was 32nm, the blue shift was 9nm, the operating current was adjusted to 30mA, the light emitting wavelength of the test core particle was 532nm, the operating voltage was 2.82V, the light emitting luminance was 15mW, the half-peak width was 33.5nm, and the blue shift was 9.5 nm. The working current was adjusted to 40mA, the luminescence wavelength of the test core particle was 532nm, the working voltage was 2.84V, the luminescence brightness was 15.7mW, the half-peak width was 35nm, and the blue-shift was 10.5 nm.
The performance test results of the products prepared in the embodiments 1 to 6 and the comparative example 1 show that when the working current fluctuates, the blue shift and the half-peak width of the product prepared in the embodiment 1 are obviously changed, and the light emitting brightness of the LED is ensured.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. A preparation method of a light emitting diode is characterized in that a non-doped GaN layer, an N-type GaN layer, a quantum well barrier light emitting layer, an electronic barrier layer and a P-type GaN layer are sequentially prepared on the surface of a substrate, the preparation method of the quantum well barrier light emitting layer is characterized in that the quantum well layer and the quantum barrier layer are prepared at intervals in a laminated mode, the quantum well layer and the quantum barrier layer are the same in layer number, the quantum well layer in contact with the N-type GaN layer is located on the outer layer, the preparation method of the quantum well layer is a metal organic chemical vapor deposition method, and the preparation method of the quantum barrier layer is a molecular beam epitaxy method.
2. The method according to claim 1, wherein the temperature for preparing the quantum well layer is 750-770 ℃ and the temperature for preparing the quantum barrier layer is 260-750 ℃ independently.
3. The method according to claim 1, wherein the temperature for preparing the quantum barrier layer is 250to 420 ℃.
4. The preparation method of claim 1, wherein the number of quantum barrier layers is 3-20.
5. The production method according to claim 1 or 4, wherein the quantum barrier layer comprises a first GaN layer, an AlN layer, and Al layer stacked in this orderXGa1-XN layer and second GaN layer, the AlxGa1-xIn the N layer, x is more than or equal to 0 and less than 1.
6. The method according to claim 5, wherein the first GaN layer has a thickness of 0.5 to 1.5nm, the AlN layer has a thickness of 0.5 to 1nm, and the Al layer isXGa1-XThe thickness of the N layer is 0.5-5 nm, and the thickness of the second GaN layer is 6-8 nm.
7. The method according to claim 5, wherein the Al isXGa1-XIn the N layer, x is more than or equal to 0.1 and less than 0.15.
8. The method as claimed in claim 1 or 4, wherein each of the quantum barrier layers has a thickness of 2 to 16 nm.
9. The method according to claim 1, wherein the thickness of each quantum well layer is 4 to 7 nm.
10. The method according to claim 1, wherein the substrate has a thickness of 650 to 660 μm, the undoped GaN layer has a thickness of 1000 to 2500nm, the N-type GaN layer has a thickness of 800 to 1500nm, the electron blocking layer has a thickness of 100 to 130nm, and the P-GaN layer has a thickness of 150 to 350 nm.
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