CN110517949B - By using SiO2Method for preparing nonpolar a-plane GaN epitaxial layer as substrate - Google Patents
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Abstract
The invention belongs to the technical field of semiconductor material preparation, and provides a method for preparing SiO by using a Metal Organic Chemical Vapor Deposition (MOCVD) process2A method for preparing a nonpolar a-plane GaN epitaxial layer on a substrate. Firstly, SiO is added2The substrate is subjected to nitridation treatment under the conditions of 1200-1300 ℃ high-temperature large ammonia gas 4000-4500sccm flow, and SiO is treated2a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer; and growing an a-plane oriented GaN crystal nucleus layer on the thin layer, and finally growing an a-plane GaN epitaxial layer on the basis of the nonpolar crystal nucleus. Compared with the polar c-plane GaN which is widely applied at present, the nonpolar a-plane GaN-based device eliminates the quantum confinement Stark effect caused by the polarization effect, and has the advantages of high internal quantum efficiency, no luminescence wavelength drift under high current density and the like.
Description
Technical Field
The invention belongs to the technical field of semiconductor material preparation, and particularly relates to a method for preparing a semiconductor material by using a Metal Organic Chemical Vapor Deposition (MOCVD) process and SiO2A method for preparing a nonpolar a-plane GaN epitaxial layer on a substrate.
Background
Gallium nitride (GaN) materials have the advantages of direct wide forbidden band, stable chemical properties, high melting point (2300 ℃), and the like, and have wide application in solid-state lighting, solar cells, sterilization, lasers, and the like. GaN of a wurtzite structure belongs to a non-centrosymmetric crystal, and the polar axis of the GaN is the c axis. Researchers typically grow polar c-plane GaN thin films epitaxially on polar c-plane sapphire substrates. However, a polarization electric field exists in the polar plane GaN, and under the action of the polarization electric field, electrons and holes in the quantum well are spatially separated, so that the recombination probability is greatly reduced, namely, the Quantum Confinement Stark Effect (QCSE). QCSE causes a reduction in the quantum efficiency within the device, severely hampering the application of high power GaN-based LEDs.
One way to eliminate the effects of gallium nitride polarization effects is to grow the device structure along non-polar faces of the crystal, such as the a-plane (11-20) and the m-plane (10-10). When the current direction of a device made of the GaN-based material is vertical to the nonpolar surface of the GaN, because no polarization electric field exists in the direction, the problem of the separation of electrons and holes in space caused by polarization is solved, the radiation recombination efficiency of the electrons and the holes can be improved under the condition of a wider quantum well, and the problem that the light-emitting wavelength fluctuates along with the change of the magnitude of the injected current is avoided. Therefore, the preparation of the GaN with the non-polar surface is significant to the improvement of the efficiency and the operation stability of the LED device.
At present, the nonpolar GaN film is generally on the r (1-102) plane of sapphire and LiAlO2(100) And growing on a surface, SiC or other heterogeneous substrate. gamma-LiAlO was first found by Shanghai optical institution of Chinese academy of sciences in 19982(100) The m-GaN is prepared by MOCVD (see gamma-LiAlO)2A novel substrate for GaN epitoxy, Journal of Crystal Growth, 1998, 193, 127.). M.D. Craven et al prepared a-GaN on r-plane sapphire substrates using the MOCVD process (see Structure characterization of non-polar (110) a-plane GaN thin growth on (102) r-plane sapphire, Applied Physics Letters, 2002, 81(3): 469-. 2008, U.S. X.Ni et al prepared m-GaN on an m-plane 6H-SiC substrate by MOCVD method (see Epitaxial substrate) overgrowth of (1100) m-plane GaN on m-plane 6H-SiC by metalorganic chemical vapor deposition[J]Proc. of SPI, 2008, 6894, 201-. Adopts sapphire and LiAlO2And SiC and other substrates have high cost for preparing nonpolar GaN, and the quality of the film is still to be further improved.
Disclosure of Invention
The invention aims to solve the defects of the method and provide a method for preparing SiO2A method for preparing a high-quality nonpolar a-plane GaN epitaxial layer on a substrate.
The invention is realized by the following technical scheme: by SiO2The method for preparing nonpolar a-plane GaN epitaxial layer on substrate comprises preparing SiO2The substrate is subjected to nitridation treatment under the conditions of 1200-1300 ℃ high temperature and 4000-4500sccm ammonia gas flow, and SiO is treated2a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer; and growing an a-plane oriented GaN crystal nucleus layer on the thin layer, and finally growing an a-plane GaN epitaxial layer on the basis of the nonpolar crystal nucleus.
The method comprises the following specific steps:
(1)SiO2cleaning the surface of the substrate, and nitriding: mixing SiO2 The substrate is placed in a metal organic vapor deposition MOCVD reaction chamber and cleaned at the temperature of 1200-1300 ℃ in the hydrogen atmosphere; performing nitridation treatment for 10-15min by ammonia gas with the flow rate of 4000-; nitrided SiO2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 2-10 nm;
(2) growing an a-surface GaN crystal nucleus layer: after the step (1), cooling to 1000-;
(3) growth of a-surface GaN epitaxial layer: after the step (2), the temperature is raised to 1250-.
SiO treated by nitriding in step (1)2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 2-10 nm.
The invention has the following beneficial effects:
the invention adopts SiO2As a cheap substrate, by applying to SiO2Nitriding to form a-Si with a close-packed hexagonal structure on the surface3N4And continuously epitaxially growing a high-quality nonpolar a-plane GaN epitaxial layer with a wurtzite structure (hexagonal close-packed) on the thin layer. The growth of the high-quality nonpolar a-plane GaN epitaxial layer has important significance for realizing no luminescence wavelength drift of the LED device under high current density.
Drawings
FIG. 1 the present invention is on SiO2A growth process flow schematic diagram of preparing an a-surface GaN epitaxial layer on a substrate;
FIG. 2 is an Atomic Force Microscope (AFM) image of the surface of the growth sample of example 1;
FIG. 3 is an X-ray diffraction pattern (XRD) of the sample grown in example 1.
Detailed Description
The technical solution and effect of the present invention can be further illustrated by the following drawings and examples.
Example 1: by SiO2The method for preparing the nonpolar a-plane GaN epitaxial layer as the substrate comprises the steps of firstly preparing SiO2The substrate is subjected to nitridation treatment under the conditions of high temperature of 1200-1300 ℃ and large ammonia gas flow of 4000-4500sccm, and SiO is treated2a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer; and growing an a-plane oriented GaN crystal nucleus layer on the thin layer, and finally growing an a-plane GaN epitaxial layer on the basis of the nonpolar crystal nucleus.
The method comprises the following specific steps:
(1)SiO2cleaning the surface of the substrate, and nitriding: mixing SiO2 Placing the substrate in a Metal Organic Chemical Vapor Deposition (MOCVD) reaction chamber, and cleaning the substrate at 1250 ℃ in a hydrogen atmosphere; at the same temperatureNitriding with ammonia gas of 4000 sccm for 10min at the temperature of 150 mbar in the reaction chamber; nitrided SiO2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 2 nm;
(2) growing an a-surface GaN crystal nucleus layer: after the step (1), cooling to 1000 ℃, introducing a gallium source with the flow rate of 40sccm and ammonia gas with the flow rate of 200 sccm into the reaction chamber, wherein the V/III ratio is 100, and growing for 40s under the condition that the reaction pressure is 150 mbar to generate an a-plane GaN crystal nucleus layer;
(3) growing an a-surface GaN epitaxial layer; after the step (2), the temperature is raised to 1270 ℃, and the a-plane GaN epitaxial layer is grown for 2h under the conditions that the flow rate of ammonia gas is 1500 sccm, the flow rate of a gallium source is 40sccm, the V/III ratio is 800, and the pressure is kept at 400 mbar.
FIG. 2 is an Atomic Force Microscopy (AFM) image of the surface of the sample grown in example 1, from which it can be seen that the atomic level step laminar flow reflects a very flat surface with a root mean square Roughness (RMS) measurement of only 0.34 nm. Fig. 3 shows XRD 2 theta-omega scan of a-plane GaN epitaxial layer sample. The scanning result shows that the diffraction peak at 57.6 ℃ corresponds to the (11-20) diffraction peak of the a-plane GaN film, and no other diffraction peaks appear in addition, which shows that the diffraction peak at the SiO2Only a single-orientation a-plane GaN film is grown on the substrate. Furthermore, the maximum half-value width of the (11-20) a-plane diffraction peak of GaN is narrow, which indicates that the crystal quality of the film is high.
Example 2: in SiO2The method for preparing the nonpolar a-plane GaN epitaxial layer on the substrate comprises the following specific steps:
(1)SiO2cleaning the surface of the substrate, and nitriding: mixing SiO2 Placing the substrate in a Metal Organic Chemical Vapor Deposition (MOCVD) reaction chamber, and cleaning the substrate at 1300 ℃ in a hydrogen atmosphere; nitriding with ammonia gas at 4500sccm flow rate at the same temperature for 15min, and reaction chamber pressure of 200 mbar; nitrided SiO2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 10 nm;
(2) growing an a-surface GaN crystal nucleus layer: after the step (1), cooling to 1050 ℃, introducing a gallium source of 50sccm and ammonia gas of 400sccm into the reaction chamber, wherein the V/III ratio is 200, and growing for 35 s under the condition that the reaction pressure is 200mbar to generate an a-plane GaN crystal nucleus layer;
(3) growth of a-surface GaN epitaxial layer: after the step (2), the temperature is raised to 1300 ℃, and the a-plane GaN epitaxial layer is grown for 2h under the conditions that the flow rate of ammonia gas is 2000sccm, the flow rate of a gallium source is 45 sccm, the V/III ratio is 1000, and the pressure is kept at 300 mbar.
Example 3: in SiO2The method for preparing the nonpolar a-plane GaN epitaxial layer on the substrate comprises the following specific steps:
(1)SiO2cleaning the surface of the substrate, and nitriding: mixing SiO2 Placing the substrate in a Metal Organic Chemical Vapor Deposition (MOCVD) reaction chamber, and cleaning the substrate at 1200 ℃ in a hydrogen atmosphere; nitriding with ammonia gas with the flow of 4300 sccm for 12 min at the same temperature, wherein the pressure of the reaction chamber is 100 mbar; nitrided SiO2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 6 nm;
(2) growing an a-surface GaN crystal nucleus layer: after the step (1), cooling to 1100 ℃, introducing 45 sccm gallium source and 300 sccm ammonia gas into the reaction chamber, wherein the V/III ratio is 150, and growing for 45s under the condition of keeping the pressure of 100 mbar to generate an a-plane GaN crystal nucleus layer;
(3) growth of a-surface GaN epitaxial layer: after step (2), the temperature is raised to 1250 ℃, and the a-plane GaN epitaxial layer is grown for 2h under the conditions that the flow rate of ammonia gas is 1800 sccm, the flow rate of a gallium source is 50sccm, the V/III ratio is 900 and the pressure is kept at 350 mbar.
Claims (3)
1. SiO by using Metal Organic Chemical Vapor Deposition (MOCVD) process2The method for preparing the nonpolar a-plane GaN epitaxial layer on the substrate is characterized by comprising the following steps: mixing SiO2The substrate is placed in MOCVD, and is subjected to nitridation treatment under the conditions of high temperature of 1200-1300 ℃ and large ammonia flow of 4000-4500sccm, and SiO is treated2a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer; a GaN crystal nucleus layer with a-plane orientation is grown on the thin layer,and finally, growing an a-surface GaN epitaxial layer on the basis of the nonpolar crystal nucleus.
2. The method of claim 1, wherein the SiO is formed by a Metal Organic Chemical Vapor Deposition (MOCVD) process2The method for preparing the nonpolar a-plane GaN epitaxial layer on the substrate is characterized by comprising the following steps: the method comprises the following specific steps:
(1)SiO2cleaning the surface of the substrate, and nitriding: mixing SiO2The substrate is placed in an MOCVD reaction chamber and cleaned at the temperature of 1200-1300 ℃ in the hydrogen atmosphere; performing nitridation treatment on ammonia gas with the flow rate of 4000-;
(2) growing an a-surface GaN crystal nucleus layer: after the step (1), cooling to 1000-;
(3) growth of a-surface GaN epitaxial layer: after the step (2), the temperature is raised to 1250-.
3. The method of claim 2, wherein the SiO is formed by a Metal Organic Chemical Vapor Deposition (MOCVD) process2The method for preparing the nonpolar a-plane GaN epitaxial layer on the substrate is characterized by comprising the following steps: SiO treated by nitriding in step (1)2A layer of a-Si with a close-packed hexagonal structure is formed on the surface of the substrate3N4A thin layer with a thickness of 2-10 nm.
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