CN109560172B - Semi-polar gallium-nitrogen epitaxial wafer and preparation method thereof - Google Patents
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 229910004205 SiNX Inorganic materials 0.000 claims abstract description 16
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 15
- 239000010980 sapphire Substances 0.000 claims abstract description 15
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 230000000087 stabilizing effect Effects 0.000 claims description 17
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000001963 growth medium Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 229910052581 Si3N4 Inorganic materials 0.000 abstract 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000000927 vapour-phase epitaxy Methods 0.000 abstract 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 30
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 230000007547 defect Effects 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
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- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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 materials, and particularly relates to a high-quality semipolar (11-22) gallium-nitrogen (GaN) epitaxial wafer and a preparation method thereof. The method adopts the metal organic chemical vapor phase epitaxy technologyThe preparation method of the epitaxial wafer comprises the following steps: firstly, growing silicon nitride (SiN) on an m-plane sapphire substratex) A thin layer as a nano-mask layer; then in SiNxGrowing high-temperature GaN islands on the thin layer; then controlling conditions to enable the islands to be asymmetrically combined; and finally, continuously adopting asymmetric growth conditions to grow (11-22) GaN thin films. The high-quality semi-polar (11-22) GaN epitaxial wafer prepared by the method can be used for preparing high-efficiency Light Emitting Diodes (LEDs) from purple light to infrared bands.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a semi-polar gallium-nitrogen (GaN) epitaxial wafer and a preparation method thereof.
Background
Conventional c-plane III-nitride materials can be used to fabricate high-efficiency LEDs and high-power Lasers (LDs) [1 ]. However growing c-plane heterostructure InGaN/GaN (AlGaN/GaN) materials faces: 1. phase separation, 2, high density penetration defects, 3, strong polarization fields, etc., and thus new techniques are needed to solve or improve the above problems, thereby further improving the working efficiency of the existing devices and reducing the energy consumption. One such method is to grow a quantum well structure on the semipolar face of the group III nitride material. The semipolar plane has the advantages of low polarization field and large growth window, so it can be used to prepare high-efficiency LEDs and high-power LDs [2 ].
The most recently used for research and production are the (11-22) plane and (20-21) plane group III nitrides. Growing (20-21) plane III-nitride materials requires the use of costly homoepitaxial substrates or chemically etched patterned substrates [3 ]; while (11-22) plane III-nitride materials can be grown on heteroepitaxial substrates, and thus low cost semipolar (11-22) plane III-nitrides are expected. The grown semipolar group III nitride thin film has high penetrating defect density and rough surface due to the lattice mismatch between the (11-22) plane group III nitride and a foreign substrate and the like, and cannot meet the requirement of high-performance device preparation at present [4 ]. It is therefore of great interest to improve and develop growth techniques to achieve high quality semipolar (11-22) plane III-nitride and semipolar III-nitride LEDs.
Reference documents:
[1]Science 2005, 308, 1274−1278; Science 1997, 386, 351−359; Science1998, 281, 956; Mater. Today 2011, 14, 408−415.
[2]MRS Bulletin 2009, 34, 318−323; MRS Bulletin 2009, 34, 334−340;Appl. Phys. Lett. 2012, 100, 201108; Phys. Rev. Lett. 2015, 115, 085503.
[3]Appl. Phys. Lett. 2014, 104, 262105; ACS Appl. Mater. Interfaces2017, 9, 14088.
[4]Jpn. J. Appl. Phys., 2006, 45, L154–L157; Phys. Status Solidi C,2008, 5, 1815–1817; Jpn. J. Appl. Phys., Part 1, 2007, 46, 4089–4095; J.Appl. Phys. 2016, 119, 145303; Appl. Phys. Lett. 2009, 94, 161109; Sci. Rep.2016, 6, 20787。
disclosure of Invention
The invention aims to provide a preparation method of a high-quality semipolar (11-22) gallium-nitrogen (GaN) epitaxial wafer.
The invention provides a preparation method of a high-quality semi-polar (11-22) GaN epitaxial wafer, which adopts an MOCVD technology and comprises the following specific steps:
(1) growth of SiN on m-plane sapphire substratexThin layer, as a nano-mask layer:
placing the m-plane sapphire substrate into an MOCVD reaction chamber, cleaning and nitriding the surface of the m-plane sapphire substrate at high temperature, and then growing SiNxA thin layer; SiNxThe growth conditions of the thin layer are as follows: the pressure in the MOCVD reaction chamber is in the range of 350-580Torr, the substrate temperature is controlled at 450-650 ℃, and SiH is introduced4As a silicon source, SiH control4The flow rate of the growth medium is in the range of 0-200sccm, and the growth time is 50-300 s;
(2) in SiNxGrowing high-temperature GaN islands on the thin layer:
the pressure in the reaction chamber is stabilized within the range of 400-550Torr, the substrate temperature is controlled at 500-600 ℃ and ammonia (NH) is introduced3) And trimethylgaalane (TMGa) as nitrogen source and gallium source, NH3The ratio of TMGa is 500-; then raising the temperature to anneal the GaN nucleating layer, wherein the annealing temperature is 1000-1100 ℃;
growing on a low temperature GaN nucleation layerGrowing the high temperature GaN islands; adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 200-500Torr, controlling the substrate temperature at 1150 ℃ and introducing NH3And TMGa, NH3The TMGa ratio is 2000-4000, and the growth time is 500-800 s;
(3) controlling conditions to enable asymmetrical combination among islands:
adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 30-100Torr, controlling the substrate temperature at 1000 ℃ and 1150 ℃, and introducing NH3And TMGa, NH3The TMGa ratio is 400-2000, and the growth time is 700-1300 s;
(4) growing (11-22) GaN thin films using asymmetric growth conditions:
adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 60-150Torr, controlling the substrate temperature at 1000-3And TMGa, NH3the/TMGa ratio is 400-2000 and the growth time is 4500s or more.
The epitaxial structure of the semi-polar GaN epitaxial wafer grown by this method is shown in fig. 1.
The method of the present invention can be used for (11-22) GaN films grown on silicon substrates, in addition to (11-22) GaN films grown on sapphire substrates. The invention is characterized in that the transmission of penetrating defects in the semi-polar GaN material is blocked by combining asymmetrical islands, thereby improving the quality of the (11-22) GaN thin film crystal grown subsequently; the quality of the GaN film crystal grown by the technology is obviously improved.
On the basis of the epitaxial wafer prepared by the invention, a luminous indium gallium nitride (InGaN) quantum well epitaxial wafer can be further prepared, and one epitaxial structure of the luminous indium gallium nitride (InGaN) quantum well epitaxial wafer is shown in figure 2. On the basis of the prepared luminescent InGaN quantum well epitaxial wafer, high-efficiency semi-polar GaN-based LEDs such as Light Emitting Diodes (LEDs) from purple light to infrared wave bands can be further prepared. One such epitaxial structure is shown in figure 3.
Drawings
Fig. 1 shows the epitaxial structure of a semipolar (11-22) GaN epitaxial wafer.
Fig. 2 is an epitaxial structure of a semipolar (11-22) light emitting InGaN/GaN quantum well epitaxial wafer.
FIG. 3 is an epitaxial structure of a semi-polar (11-22) GaN-based LED.
Fig. 4 is a Scanning Electron Microscope (SEM) image of the GaN epitaxial wafer prepared in example 1.
Fig. 5 is an X-ray diffraction pattern (XRD) pattern of the GaN epitaxial wafer prepared in example 1.
Fig. 6 is a cathode fluorescence (CL) spectrum of the GaN epitaxial wafer prepared in example 1.
Fig. 7 is XRD of the GaN epitaxial wafer prepared in example 2.
Fig. 8 is XRD of the GaN epitaxial wafer prepared in example 3.
Fig. 9 shows CL of the InGaN epitaxial wafer prepared in example 3.
Detailed Description
Example 1: preparation of high quality semipolar (11-22) GaN thin films
(1) Growth of SiN on m-plane sapphire substratexThin layer:
placing the m-plane sapphire substrate into an MOCVD reaction chamber, cleaning and nitriding the surface of the m-plane sapphire substrate at high temperature, and then growing SiNxA thin layer. SiNxThe growth conditions of the thin layer are as follows: the pressure in the MOCVD reaction chamber is 500Torr, the substrate temperature is controlled at 570 ℃, and SiH is introduced4As a silicon source, SiH control4The flow rate of (2) was 40sccm, and the growth time was 200 s.
(2) In SiNxGrowing high-temperature GaN islands on the thin layer:
stabilizing the pressure in the reaction chamber at 500Torr, controlling the substrate temperature at 550 ℃, and introducing NH3And TMGa as nitrogen source and gallium source, NH3The ratio of/TMGa is 2200, and a low-temperature GaN nucleating layer is grown; then heating and annealing the GaN nucleating layer, wherein the annealing temperature is 1050 ℃;
growing a high-temperature GaN island on the low-temperature GaN nucleating layer; adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 250Torr, controlling the substrate temperature at 1050 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 2600 and the growth time was 600 s.
(3) Controlling conditions to enable asymmetrical combination among islands:
adjust the pressure in the reaction chamber andstabilizing at 50Torr, controlling the substrate temperature at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 1100 and the growth time was 1000 s.
(4) Growing (11-22) GaN thin films using asymmetric growth conditions:
adjusting the pressure in the reaction chamber and stabilizing at 100Torr, controlling the substrate temperature at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 1100 and the growth time was 5500 s.
The surface topography of the sample exhibited a typical striated topography as shown in fig. 4. X-rays are respectively incident along two directions of [ -1-123] and [1-100], and the full widths at half maximum of XRD peaks of the GaN epitaxial wafer are respectively 0.03 degrees (110 arcsec) and 0.13 degrees (465 arcsec); the data diagram is shown in fig. 5. The low-temperature emission of the epitaxial wafer is shown in fig. 6, in which GaN excitons emit light strongly and defects emit light weakly.
Example 2: preparation of high quality semipolar (11-22) GaN thin films
(1) Growth of SiN on m-plane sapphire substratexThin layer:
placing the m-plane sapphire substrate into an MOCVD reaction chamber, cleaning and nitriding the surface of the m-plane sapphire substrate at high temperature, and then growing SiNxA thin layer. SiNxThe growth conditions of the thin layer are as follows: the pressure in the MOCVD reaction chamber is 500Torr, the substrate temperature is controlled at 570 ℃, and SiH is introduced4As a silicon source, SiH control4The flow rate of (2) was 40sccm, and the growth time was 200 s.
(2) In SiNxGrowing high-temperature GaN islands on the thin layer:
stabilizing the pressure in the reaction chamber at 500Torr, controlling the substrate temperature at 550 ℃, and introducing NH3And TMGa as nitrogen source and gallium source, NH3The ratio of/TMGa is 2100, and a low-temperature GaN nucleating layer is grown; then heating and annealing the GaN nucleating layer, wherein the annealing temperature is 1030 ℃;
growing a high-temperature GaN island on the low-temperature GaN nucleating layer; adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 250Torr, controlling the temperature of the substrate at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 2500 and the growth time was 600 s.
(3) Controlling conditions to enable asymmetrical combination among islands:
adjusting the pressure in the reaction chamber and stabilizing at 50Torr, controlling the substrate temperature at 1010 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 1000 and the growth time was 1000 s.
(4) Growing (11-22) GaN thin films using asymmetric growth conditions:
adjusting the pressure in the reaction chamber and stabilizing at 100Torr, controlling the substrate temperature at 1010 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 1000 and the growth time was 5500 s.
X-rays are respectively incident along two directions of [ -1-123] and [1-100], and the full widths at half maximum of XRD peaks of the GaN epitaxial wafer are respectively 0.06 degree (216 arcsec) and 0.17 degree (612 arcsec); the data diagram is shown in fig. 7.
Example 3: InGaN quantum wells fabricated using semipolar (11-22) GaN as substrate
The epitaxial structure of the InGaN quantum well epitaxial wafer prepared in the example is shown in fig. 2.
(1) Growth of SiN on m-plane sapphire substratexThin layer:
placing the m-plane sapphire substrate into an MOCVD reaction chamber, cleaning and nitriding the surface of the m-plane sapphire substrate at high temperature, and then growing SiNxA thin layer. SiNxThe growth conditions of the thin layer are as follows: the pressure in the MOCVD reaction chamber is 500Torr, the substrate temperature is controlled at 570 ℃, and SiH is introduced4As a silicon source, SiH control4The flow rate of (2) was 40sccm, and the growth time was 200 s.
(2) In SiNxGrowing high-temperature GaN islands on the thin layer:
stabilizing the pressure in the reaction chamber at 500Torr, controlling the substrate temperature at 550 ℃, and introducing NH3And TMGa as nitrogen source and gallium source, NH3The ratio of/TMGa is 2200, and a low-temperature GaN nucleating layer is grown; then heating and annealing the GaN nucleating layer, wherein the annealing temperature is 1030 ℃;
growing a high-temperature GaN island on the low-temperature GaN nucleating layer; adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 250Torr, controlling the temperature of the substrate at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 1100 and the growth time was 600 s.
(3) Controlling conditions to enable asymmetrical combination among islands:
adjusting the pressure in the reaction chamber and stabilizing at 100Torr, controlling the substrate temperature at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 950 and the growth time was 800 s.
(4) Growing (11-22) GaN thin films using asymmetric growth conditions:
adjusting the pressure in the reaction chamber and stabilizing at 60Torr, controlling the substrate temperature at 1030 ℃, and introducing NH3And TMGa, NH3the/TMGa ratio was 950 and the growth time was 5500 s.
X-rays are respectively incident along two directions of [ -1-123] and [1-100], and the full widths at half maximum of XRD peaks of the GaN epitaxial wafer are respectively 0.05 degrees (180 arcsec) and 0.16 degrees (576 arcsec); the data diagram is shown in fig. 8.
(5) InGaN/GaN quantum wells are grown on the GaN template.
Growth parameters of the quantum well:
the growth temperature of the GaN layer is 860 ℃, and the growth thickness is 9.0 nm;
the growth temperature of the InGaN layer is 740 ℃, and the growth thickness is 4.5 nm.
The CL spectrum is shown in FIG. 9, and the central wavelength of the luminescence peak is 500 nm (cyan-green light).
The foregoing is a further description of the invention with reference to preferred embodiments, and the examples described are some, but not all, examples of the invention. It will be apparent to those skilled in the art that various modifications, additions, substitutions, and other embodiments can be made without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of a semi-polar gallium-nitrogen epitaxial wafer is characterized in that an MOCVD technology is adopted, and the preparation method comprises the following specific steps:
(1) growth of SiN on a substratexThin layer, as a nano-mask layer:
placing the substrate into a MOCVD reaction chamber, cleaning and nitriding the surface of the substrate at high temperature, and then growing SiNxA thin layer; SiNxThe growth conditions of the thin layer are as follows: the pressure in the MOCVD reaction chamber is in the range of 350-580Torr, the substrate temperature is controlled to be 450-650 ℃, and SiH is introduced4As a silicon source, SiH control4The flow rate of the growth medium is 0-200sccm, and the growth time is 50-300 s;
(2) in SiNxGrowing high-temperature GaN islands on the thin layer:
the pressure in the reaction chamber is stabilized within the range of 400-550Torr, the substrate temperature is controlled at 500-600 ℃ and NH is introduced3And tri-TMGa as nitrogen source and gallium source, NH3The ratio of TMGa is 500-; then raising the temperature to anneal the GaN nucleating layer, wherein the annealing temperature is 1000-1100 ℃;
growing a high-temperature GaN island on the low-temperature GaN nucleating layer; adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 200-3And TMGa, NH3The TMGa ratio is 2000-4000, and the growth time is 500-800 s;
(3) controlling conditions to enable asymmetrical combination among islands:
adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 30-100Torr, controlling the substrate temperature at 1000-3And TMGa, NH3The TMGa ratio is 400-2000, and the growth time is 700-1300 s;
(4) growing (11-22) GaN thin films using asymmetric growth conditions:
adjusting the pressure in the reaction chamber and stabilizing the pressure in the range of 60-150Torr, controlling the substrate temperature at 1000-3And TMGa, NH3the/TMGa ratio is 400-2000 and the growth time is 4500s or more.
2. The method for preparing the semi-polar gallium-nitrogen epitaxial wafer according to claim 1, wherein the substrate material is m-plane sapphire or silicon.
3. A semipolar GaN epitaxial wafer obtained by the production method according to claim 1 or 2.
4. Use of a semi-polar GaN epitaxial wafer according to claim 3 in the preparation of a light emitting InGaN quantum well epitaxial wafer.
5. Use of the semi-polar GaN epitaxial wafer of claim 3 in the preparation of semi-polar GaN-based LEDs.
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