WO2018076407A1 - 生长在镓酸锂衬底上的非极性纳米柱led及其制备方法 - Google Patents

生长在镓酸锂衬底上的非极性纳米柱led及其制备方法 Download PDF

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WO2018076407A1
WO2018076407A1 PCT/CN2016/105813 CN2016105813W WO2018076407A1 WO 2018076407 A1 WO2018076407 A1 WO 2018076407A1 CN 2016105813 W CN2016105813 W CN 2016105813W WO 2018076407 A1 WO2018076407 A1 WO 2018076407A1
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李国强
王文樑
杨美娟
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South China University of Technology SCUT
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H10H20/011—Manufacture or treatment of bodies, e.g. forming semiconductor layers
    • H10H20/013—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials
    • H10H20/0133—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials with a substrate not being Group III-V materials
    • H10H20/01335—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials with a substrate not being Group III-V materials the light-emitting regions comprising nitride materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/81—Bodies
    • H10H20/811—Bodies having quantum effect structures or superlattices, e.g. tunnel junctions
    • H10H20/812—Bodies having quantum effect structures or superlattices, e.g. tunnel junctions within the light-emitting regions, e.g. having quantum confinement structures
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/81—Bodies
    • H10H20/819—Bodies characterised by their shape, e.g. curved or truncated substrates
    • H10H20/821—Bodies characterised by their shape, e.g. curved or truncated substrates of the light-emitting regions, e.g. non-planar junctions

Definitions

  • the invention relates to the field of nano-array LED growth and preparation, in particular to a nano-column LED grown on a lithium gallate (LiGaO 2 ) substrate and a preparation method thereof.
  • LiGaO 2 lithium gallate
  • GaN and its related Group III nitrides have excellent electrical, optical and acoustic properties and have been widely used in the fabrication of light-emitting diodes (LEDs), laser diodes (LDs) and field effect transistors.
  • LEDs light-emitting diodes
  • LDs laser diodes
  • field effect transistors field effect transistors.
  • GaN-based nano-column LEDs have attracted much attention as a potential LED structure, because the nano-column LEDs have a high aspect ratio (area/volume) compared to planar LEDs, which can significantly reduce wear.
  • the nano-column LED can greatly improve the light-emitting efficiency of the LED and realize the coupling and exit of the light; finally, by controlling the size of the nano-column LED, the wavelength of the nano-column LED can be changed to prepare a single-chip multi-color illumination.
  • the nano-pillar LEDs have opened up new avenues for the preparation of low-cost white LEDs.
  • GaN-based nano-column LEDs are constructed based on their polar faces.
  • the quantum bound Stark effect (QCSE) of the polar surface causes the LED band to bend and tilt, which causes the separation of electrons and holes, which is seriously reduced.
  • the radiation recombination efficiency of the carriers causes the LED emission wavelength to be unstable.
  • the non-polar surface epitaxial GaN-based LED can suppress the wavelength shift caused by the bending and tilting of the energy band, overcome the separation of electrons and holes caused by the QCSE effect, and theoretically improve the luminous efficiency of the LED by nearly double.
  • the non-polar InGaN/GaN quantum well structure has been proven to have a special polarization characteristic, which can be used in screen display devices to remove the polarization filter, thereby reducing the loss caused by the polarization filter and improving the light uniformity of the screen. To achieve energy saving and improve the color tone.
  • the non-polar plane GaN is more likely to form defects during growth than the polar plane GaN. Therefore, the selection of non-polar GaN epitaxial substrates is particularly important.
  • commercial LEDs are mainly epitaxially grown on sapphire substrates.
  • the lattice mismatch between sapphire and GaN is high, resulting in the formation of GaN nanopillars.
  • the high dislocation density which reduces the carrier mobility of the material, ultimately affects device performance.
  • the lattice mismatch of LiGaO 2 substrate and non-polar GaN in the b and c directions is 0.1% and 4.0%, respectively, and the thermal expansion coefficient is very close (the thermal expansion coefficient of LiGaO2 substrate is 4.0 ⁇ 10 -6 K -1 , respectively).
  • GaN Compared with 3.8 ⁇ 10 -6 K -1 , GaN has thermal expansion coefficients of 5.59 ⁇ 10 -6 K -1 and 3.17 ⁇ 10 -6 K -1 , respectively, which is one of the best substrates for epitaxial non-polar plane GaN.
  • the chemical nature of the high temperature instability LiGaO 2 substrate, a LiGaO 2 substrate to make GaN-based nano-column LED is possible to realize large-scale applications, it is necessary to find a new method of growing a GaN-based nano-column LED on the substrate and process LiGaO 2 .
  • the object of the present invention is to provide a nano-pillar LED grown on a lithium gallate substrate and a preparation method thereof, wherein the selected lithium gallate substrate material has low cost and is prepared.
  • the nano-pillar array is controllable in size and uniform in orientation, and the obtained non-polar nano-pillar LED has low defect density and excellent electrical and optical properties.
  • Non-polar nanocolumn LEDs grown on a lithium gallate substrate including LiGaO 2 substrates, GaN nanopillar arrays grown on LiGaO 2 substrates, undoped GaN layers grown on GaN nanopillar arrays, grown An n-doped GaN layer on the undoped GaN layer, an InGaN/GaN quantum well grown on the n-doped GaN layer, and a p-doped GaN layer grown on the InGaN/GaN quantum well.
  • the GaN nanopillar array is a non-polar GaN nanopillar array.
  • the non-polar nano-pillar LED grown on the lithium gallate substrate further includes an isolation layer deposited on the sidewalls of the GaN nano-pillar array and the LiGaO 2 substrate not covered by the nano-pillar array.
  • the isolation layer is a SiN x , SiO 2 or Al 2 O 3 isolation layer. SiN x , x is 1 to 2.
  • the LiGaO 2 substrate has an epitaxial plane of 0.2 to 1° in a (100) plane (110) direction.
  • the GaN nanopillar array was prepared from a non-polar GaN buffer layer grown on a LiGaO 2 substrate.
  • the non-polar GaN buffer layer is a non-polar plane GaN, and the crystal epitaxial orientation relationship is such that the (1-100) plane of GaN is parallel to the (100) plane of LiGaO 2 . That is, the GaN nano-pillar array is a non-polar plane GaN, and the crystal epitaxial orientation relationship is such that the (1-100) plane of GaN is parallel to the (100) plane of LiGaO 2 .
  • the non-polar GaN buffer layer is formed by epitaxial growth on a LiGaO 2 substrate at a low temperature by using a PLD technology, which can effectively alleviate the high-temperature growth of Li atoms in the LiGaO 2 substrate and interact with the non-polar GaN buffer layer. A serious interface reaction occurs between them.
  • the GaN nano-pillar array is prepared by using TracePro software to optimize nano-column arrangement, and is prepared by using nano-imprint technology and etching on a non-polar GaN buffer layer, and the obtained nano-pillar array is uniform in size.
  • the GaN nano-pillar array grown on the LiGaO 2 substrate was transferred to a metal organic compound vapor deposition reaction chamber (MOCVD) for the preparation of nano-column LEDs by selective growth.
  • MOCVD metal organic compound vapor deposition reaction chamber
  • the GaN nano-pillar array has a height of 500 to 1000 nm, a pitch of 150 to 250 nm, and a diameter of 100 to 200 nm.
  • the undoped GaN layer has a thickness of 200 to 300 nm; and the n-type doped GaN layer has a doping concentration of 3 ⁇ 10 18 to 9 ⁇ 10 18 cm ⁇ 3 and a thickness of 2 to 4 ⁇ m.
  • the InGaN/GaN quantum well is an InGaN well layer/GaN barrier layer of 8 to 13 cycles, wherein the thickness of the InGaN well layer is 3 to 5 nm, and the thickness of the GaN barrier layer is 10 to 15 nm.
  • the p-type doped GaN layer has a doping concentration of 3 ⁇ 10 17 to 9 ⁇ 10 17 cm ⁇ 3 and a thickness of 300 to 350 nm.
  • the thickness of the isolation layer is 10 to 50 nm
  • the method for preparing the non-polar nano-pillar LED grown on a lithium gallate substrate comprises the following steps:
  • LiGaO 2 substrate is used, and the epitaxial plane is 0.2 to 1° in the (100) plane (110) direction.
  • the crystal epitaxial orientation relationship is: (1-100) plane of GaN. Parallel to the (100) plane of LiGaO 2 ;
  • the specific process of the annealing is: placing the substrate into the annealing chamber, and annealing the LiGaO 2 substrate in an air atmosphere at 800 to 900 ° C for 3 to 4 hours. Then air cooled to room temperature;
  • Non-polar GaN buffer layer epitaxial growth PLD technology, substrate temperature is 150-250 ° C, nitrogen plasma flow rate is 3 ⁇ 4.5sccm, RF activation power is 400 ⁇ 450W, non-polar growth a GaN buffer layer having a buffer layer thickness of 500 to 1000 nm; and a crystal epitaxial orientation relationship: a (1-100) plane of GaN is parallel to a (100) plane of LiGaO 2 ; and the substrate rotation speed is 10 r/min in the PLD technique.
  • the target distance is 5 cm
  • the laser wavelength is 248 nm
  • the laser energy is 250 mJ/p
  • the frequency is 20 Hz
  • the Ga source is a GaN target, and the purity thereof is 99.99%;
  • GaN nano-pillar array The nano-column arrangement was optimized by using TracePro software, and the non-polar GaN buffer layer on the LiGaO 2 substrate was etched down by nanoimprint technology and dry etching process.
  • a GaN nano-pillar array having a height of 500 to 1000 nm, a diameter of 100 to 200 nm, and a pitch of 150 to 250 nm; the height of the GaN nano-pillar array is the same as the height of the non-polar GaN buffer layer;
  • deposition of an isolation layer depositing an isolation layer on a sidewall of the nano-pillar in the GaN nano-pillar array and a substrate not covered by the nano-pillar array by chemical vapor deposition, atomic layer deposition or magnetron sputtering techniques,
  • the material of the isolation layer is SiN x , SiO 2 or Al 2 O 3 , and has a thickness of 10 to 50 nm;
  • Epitaxial growth of the n-type doped GaN layer raising the temperature of the reaction chamber to 1000 to 1500 ° C, and growing on the undoped GaN layer obtained in the step (6) under the condition that the reaction chamber pressure is 150 to 200 Torr. a doped GaN layer having a doping concentration of 3 ⁇ 10 18 to 9 ⁇ 10 18 cm ⁇ 3 and a thickness of 2 to 4 ⁇ m;
  • Epitaxial growth of InGaN/GaN multiple quantum wells the temperature of the reaction chamber is lowered to 700-780 ° C, and ammonia, nitrogen, trimethylgallium and trimethyl groups are introduced under the pressure of 150 to 200 Torr in the reaction chamber.
  • Indium an InGaN/GaN multiple quantum well is grown on the n-type doped GaN layer obtained in the step (7), and the InGaN/GaN quantum well is an 8 to 13-cycle InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer 3 to 5 nm, the thickness of the GaN barrier layer is 10 to 15 nm;
  • the Ga source is TMGa in the epitaxial growth of the undoped GaN layer;
  • the nitrogen source is NH 3 ;
  • the flow rate of the Ga source is 350-450 sccm, and the flow rate of the nitrogen source is 50-65 slm;
  • the doping source doped in the epitaxial growth of the n-type doped GaN layer in step (7) is silane; the Ga source is TMGa; the nitrogen source is NH 3 ; the flow rate of each source is: Ga source 350-450 sccm, nitrogen source 50 ⁇ 65slm, doping source 100 ⁇ 200sccm;
  • the flow rate of the ammonia gas in the step (8) is 25 to 35 slm, the flow rate of nitrogen gas is 25 to 35 slm, the flow rate of trimethyl gallium is 100 to 150 sccm, and the flow rate of trimethyl indium is 450 to 550 sccm;
  • the flow rate of the trimethylgallium in the step (9) is 350 to 450 sccm, the flow rate of the ammonia gas is 50 to 65 slm, the flow rate of the nitrogen gas is 50 to 65 slm, and the flow rate of the magnesium pentoxide is 150 to 250 sccm.
  • Step (1) polishing the surface of the substrate specifically: first polishing the surface of the LiGaO 2 substrate with a diamond slurry, and observing the surface of the substrate with an optical microscope until there is no scratch, and then polishing by chemical mechanical polishing. deal with.
  • the cleaning is specifically: the LiGaO 2 substrate is ultrasonically cleaned in deionized water at room temperature for 3 to 5 minutes, the surface of the LiGaO 2 substrate is removed, and then the surface organic matter is removed by washing with hydrochloric acid, acetone and ethanol. Dry with dry nitrogen.
  • the present invention has the following advantages and benefits:
  • the present invention uses LiGaO 2 as a substrate, and a LiGaO 2 substrate is easily obtained, which is inexpensive, and is advantageous in reducing production cost.
  • the present invention adopts nanoimprint technology and etching to obtain a high-quality nano-pillar array, and then transfers the nano-pillar array grown on the substrate to MOCVD to perform nano-column LED epitaxial material preparation by selective growth;
  • the difficulty of LED growth eliminates the adverse effects of introducing impurities by using a catalyst, and is advantageous for obtaining high-quality nano-pillar LEDs with controllable size and uniform orientation.
  • the present invention fully utilizes the respective advantages of PLD and MOCVD: firstly, a low-level (150-250 ° C) epitaxial growth of a layer of GaN or a buffer layer on a LiGaO 2 substrate is performed using a PLD technique, and the interface reaction is successfully suppressed.
  • One-step preparation of high-quality low-defect nano-pillar arrays is paved; then transferred to high-temperature epitaxial u-GaN, n-GaN, P-GaN, and quantum wells in MOCVD, giving full play to the advantages of MOCVD, increasing growth rate and productivity ;
  • the present invention uses LiGaO 2 (100) having a lattice mismatch with GaN and a low thermal mismatch as a substrate for growing non-polar nano-pillar LEDs, which can not only effectively reduce thermal stress and reduce formation of dislocations, but also Effectively eliminate the influence of the quantum bound Stark effect; the prepared high-quality non-polar nano-column LED epitaxial material can greatly improve the luminous efficiency of nitride devices such as semiconductor lasers, light-emitting diodes and solar cells.
  • FIG. 1 is a front elevational view of a nanopillar LED grown on a lithium gallate (LiGaO 2 ) substrate of the present invention
  • Example 2 is an XRD diffraction pattern of a non-polar GaN buffer layer prepared in Example 1;
  • Example 3 is a schematic cross-sectional view of a GaN nano-pillar array prepared in Example 1;
  • Example 4 is a plan view of a nano-pillar LED grown on a lithium gallate (LiGaO 2 ) substrate of Example 1.
  • FIG. 1 A front view of a nanopillar LED grown on a lithium gallate (LiGaO 2 ) substrate of the present invention is shown in FIG. 1 and includes a LiGaO 2 substrate 10 grown on a LiGaO 2 substrate 10 on a GaN nanopillar array 11
  • the GaN nano-pillar array is prepared by nanoimprinting and etching of a non-polar GaN buffer layer grown on a LiGaO 2 substrate, deposited on the sidewalls of the GaN nano-pillar array 11 and not covered by the nano-pillar array.
  • the InGaN/GaN quantum well 15 on the GaN layer 14 is doped, and the p-doped GaN layer 16 is grown on the InGaN/GaN quantum well 15.
  • the LiGaO 2 substrate has an epitaxial plane of 0.2 to 1° in a (100) plane (110) direction.
  • the GaN nano-pillar array is a non-polar plane GaN, and the crystal epitaxial orientation relationship is such that the (1-100) plane of GaN is parallel to the (100) plane of LiGaO 2 .
  • the GaN nano-pillar array has a height of 500 to 1000 nm, a pitch of 150 to 250 nm, and a diameter of 100 to 200 nm.
  • the undoped GaN layer has a thickness of 200 to 300 nm;
  • the n-type doped GaN layer has a thickness of 2 to 4 ⁇ m;
  • the InGaN/GaN quantum well has an 8 to 13 period of InGaN well layer/GaN barrier layer.
  • the thickness of the InGaN well layer is 3 to 5 nm, and the thickness of the GaN barrier layer is 10 to 15 nm;
  • the p-doped GaN layer has a thickness of 300 to 350 nm.
  • the separator has a thickness of 10 to 50 nm.
  • Substrate and its crystal orientation a LiGaO 2 substrate is used, and the (100) plane (110) direction is 0.6° as an epitaxial plane;
  • the specific process of the annealing is: placing the substrate into the annealing chamber, annealing the LiGaO 2 substrate in an air atmosphere at 880 ° C for 3 hours and then air cooling to room temperature ;
  • the surface of the substrate is polished, specifically: first, the surface of the LiGaO 2 substrate is polished with a diamond slurry, and the surface of the substrate is observed with an optical microscope until there is no scratch, and then polished by chemical mechanical polishing;
  • the cleaning is specifically: the LiGaO 2 substrate is ultrasonically cleaned in deionized water at room temperature for 3 minutes to remove the sticky particles on the surface of the LiGaO 2 substrate, and then washed successively with hydrochloric acid, acetone, ethanol to remove surface organic matter, and dried. Blow dry with nitrogen;
  • Non-polar buffer layer epitaxial growth using PLD technology, substrate temperature is 200 ° C, substrate rotation speed is 10 r / min, target base distance is 5 cm, laser wavelength is 248 nm, laser energy is 250 mJ / p, frequency is 20 Hz
  • the nitrogen plasma flow rate is 4 sccm
  • the RF activation power is 420 W
  • the non-polar GaN buffer layer is grown to a thickness of 500 nm
  • the crystal epitaxial orientation relationship is: (1-100) plane of GaN is parallel to LiGaO 2 (100) Surface
  • Ga source is a GaN target with a purity of 99.99%;
  • Nano-imprint technology By using TracePro software to optimize nano-column arrangement, nano-imprint technology and dry etching process are used to etch the non-polar GaN buffer layer on LiGaO 2 substrate to obtain GaN.
  • Nanocolumn array the height of the nanocolumn is 500 nm, the diameter is 200 nm, and the adjacent spacing is 250 nm;
  • a spacer layer is deposited on a sidewall of a nanocolumn and a substrate not covered by a nanocolumn in a GaN nanocolumn array by chemical vapor deposition, atomic layer deposition or magnetron sputtering, the nanometer
  • the material of the pillar sidewall isolation layer is SiN x and has a thickness of 10 nm;
  • n-type doped GaN layer Epitaxial growth of an n-type doped GaN layer: the reaction chamber temperature was raised to 1200 ° C, and n-type doped GaN was grown on the undoped GaN layer obtained in the step (6) under a reaction chamber pressure of 150 Torr.
  • the layer has a doping concentration of 3 ⁇ 10 18 cm -3 and a thickness of 2 ⁇ m; the doping source is silane; the Ga source is TMGa; the nitrogen source is NH 3 ; the gas flow rate of each source is: Ga source 380 sccm, nitrogen source 56 slm, Doping source 125sccm;
  • the InGaN/GaN multiple quantum well is grown on the obtained n-type doped GaN layer, and the InGaN/GaN quantum well is an 8-cell InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer is 3 nm, and the GaN barrier layer
  • the thickness of each source is 10 nm; the flow rate of each source is: 475 sccm of indium source, 140 sccm of gallium source, 27 slm of nitrogen source;
  • the XRD diffraction pattern of the non-polar GaN buffer layer prepared in Example 1 is shown in FIG. 2; as can be seen from FIG. 2, the non-polar buffer layer grown on the lithium gallate substrate prepared in this embodiment: GaN is the m-plane
  • FIG. 1 A schematic cross-sectional view of a GaN nano-array etched on a non-polar GaN buffer layer in this embodiment is shown in FIG.
  • FIG. 1 A top view of the nano-pillar LED grown on the lithium gallate substrate prepared in this embodiment is shown in FIG.
  • the specific process of the annealing is: placing the substrate into the annealing chamber, annealing the LiGaO 2 substrate in an air atmosphere at 800-900 ° C for 4 hours and then air cooling To room temperature;
  • the surface of the substrate is polished, specifically: first, the surface of the LiGaO 2 substrate is polished with a diamond slurry, and the surface of the substrate is observed with an optical microscope until there is no scratch, and then polished by chemical mechanical polishing;
  • the cleaning is specifically: the LiGaO 2 substrate is ultrasonically cleaned in deionized water at room temperature for 3 minutes to remove the sticky particles on the surface of the LiGaO 2 substrate, and then washed successively with hydrochloric acid, acetone, ethanol to remove surface organic matter, and dried. Blow dry with nitrogen;
  • Non-polar buffer layer epitaxial growth using PLD technology, the substrate temperature is adjusted to 150-250 ° C, the substrate rotation speed is 10 r / min, the target base distance is 5 cm, the laser wavelength is 248 nm, and the laser energy is 250 mJ / p The frequency of 20 Hz, the plasma flow rate of nitrogen is 3 to 4.5 sccm, the RF activation power is 400-450 W, and the non-polar GaN buffer layer is grown, the buffer layer thickness is 1000 nm; the crystal epitaxial orientation relationship is: GaN (1- 100) face parallel to the (100) plane of LiGaO 2 ; Ga source is a GaN target, the purity of which is 99.99%;
  • nano-imprint technology and dry etching process are used to etch the non-polar GaN buffer layer on LiGaO 2 substrate to obtain GaN.
  • a nanocolumn array having a height of 1000 nm, a diameter of 100 nm, and a pitch of 150 nm;
  • a spacer layer is deposited on the sidewall of the GaN nano-pillar array and the substrate not covered by the nano-pillar by chemical vapor deposition, atomic layer deposition or magnetron sputtering, the material of the isolation layer Is SiO 2 and has a thickness of 50 nm;
  • the reaction chamber temperature was raised to 1500 ° C, and n-type doped GaN was grown on the undoped GaN layer obtained in the step (6) under a reaction chamber pressure of 200 Torr.
  • the layer has a doping concentration of 9 ⁇ 10 18 cm -3 and a thickness of 4 ⁇ m; the doping source is silane; the Ga source is TMGa; the nitrogen source is NH 3 ; the gas flow rate of each source is Ga source 380 sccm, nitrogen source 56 slm, and doping Miscellaneous source 125sccm;
  • the InGaN/GaN multiple quantum well is grown on the obtained n-type doped GaN layer, and the InGaN/GaN quantum well is a 13-cycle InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer is 5 nm, and the GaN barrier layer
  • the thickness of the anode is 15 nm;
  • the flow rate of the indium source is 475 sccm, the flow rate of the gallium source is 140 sccm, and the flow rate of the nitrogen source is 27 slm;

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Abstract

一种生长在镓酸锂衬底上的纳米柱LED及其制备方法。生长在镓酸锂衬底上的非极性纳米柱LED包括LiGaO 2衬底（10），生长在LiGaO 2衬底上的GaN纳米柱阵列（11），生长在GaN纳米柱阵列上的非掺杂GaN层（13），生长在非掺杂GaN层上的n型掺杂GaN层（14），生长在n型掺杂GaN层上的InGaN/GaN量子阱（15），生长在InGaN/GaN量子阱上的p型掺杂GaN层（16）；GaN纳米柱阵列为非极性GaN纳米柱阵列。所选择的镓酸锂衬底材料成本低廉，所制备的纳米柱阵列尺寸可控，取向均一，所获得的非极性纳米柱LED的缺陷密度低、电学和光学性能优良。

Description

生长在镓酸锂衬底上的非极性纳米柱LED及其制备方法 技术领域
本发明涉及纳米阵列LED生长与制备领域，特别涉及生长在镓酸锂(LiGaO2)衬底上的纳米柱LED及其制备方法。
背景技术
GaN及其相关的III族氮化物在电学、光学以及声学上具有极其优异的性质，已经被广泛的应用于制备发光二极管(LEDs)、激光二极管(LDs)和场效应晶体管等器件。近年来，GaN基纳米柱LED作为一种具有潜力的LED结构而备受关注，这是由于与平面结构LED相比，首先纳米柱LED具有高的面容比(面积/体积)，能够显著降低穿透位错密度；其次，纳米柱LED可大幅度提高LED的出光效率，实现光的耦合出射；最后可通过控制纳米柱LED的尺寸，改变纳米柱LED的发光波长，制备出单芯片多色发光的纳米柱LED，为实现低成本白光LED的制备开辟了新的道路。
目前GaN基纳米柱LED大多基于其极性面构建而成，极性面存在的量子束缚斯塔克效应(QCSE)会造成LED能带弯曲、倾斜、从而引起电子与空穴的分离，严重降低载流子的辐射复合效率，并造成LED发光波长不稳定。采用非极性面外延GaN基LED，能够抑制能带弯曲和倾斜所引起的波长偏移，克服QCSE效应造成的电子与空穴分离，理论上提高近一倍的LED发光效率。同时，非极性InGaN/GaN量子阱结构被证明具有一种特殊的偏振特性，应用在屏幕显示器件中，能够去除偏振滤波片，从而降低偏振滤波片引起的损耗，同时提升屏幕的光线均匀性，达到节能、改善色调的作用。
非极性面GaN相比于极性面GaN，在生长过程中更容易形成缺陷。因此，非极性面GaN外延衬底的选择显得尤为重要，目前商业化的LED主要是在蓝宝石衬底上外延生长的，然而蓝宝石与GaN的晶格失配高，导致GaN纳米柱中形成很高的位错密度，从而降低材料的载流子迁移率，最终影响了器件的性能。LiGaO2衬底与非极性GaN在b、c轴方向上的晶格失配分别为0.1％和4.0％，热 膨胀系数很接近(LiGaO2衬底的热膨胀系数分别为4.0×10-6K-1和3.8×10-6K-1，GaN对应的热膨胀系数分别为5.59×10-6K-1和3.17×10-6K-1)，是外延非极性面GaN最佳衬底之一。但LiGaO2衬底高温下化学性质不稳定，要使LiGaO2衬底上GaN基纳米柱LED能够真正实现大规模应用，因此需要寻找LiGaO2衬底上生长GaN基纳米柱LED的新方法及工艺。
发明内容
为了克服现有技术的上述缺点与不足，本发明的目的在于提供一种生长在镓酸锂衬底上的纳米柱LED及制备方法，所选择的镓酸锂衬底材料成本低廉，所制备的纳米柱阵列尺寸可控，取向均一，所获得的非极性纳米柱LED的缺陷密度低、电学和光学性能优良。
本发明的目的通过以下技术方案实现：
生长在镓酸锂衬底上的非极性纳米柱LED，包括LiGaO2衬底，生长在LiGaO2衬底上的GaN纳米柱阵列，生长在GaN纳米柱阵列上的非掺杂GaN层，生长在非掺杂GaN层上的n型掺杂GaN层，生长在n型掺杂GaN层上的InGaN/GaN量子阱，生长在InGaN/GaN量子阱上的p型掺杂GaN层。所述GaN纳米柱阵列为非极性GaN纳米柱阵列。
所述生长在镓酸锂衬底上的非极性纳米柱LED还包括隔离层，所述隔离层沉积在GaN纳米柱阵列的侧壁和未被纳米柱阵列覆盖的LiGaO2衬底上。所述隔离层为SiNx、SiO2或者Al2O3隔离层。SiNx，x为1～2。
所述LiGaO2衬底以(100)面偏(110)方向0.2～1°为外延面。
所述GaN纳米柱阵列是由生长在LiGaO2衬底上的非极性GaN缓冲层制备而成的。
所述非极性GaN缓冲层是非极性面GaN，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面。即GaN纳米柱阵列是非极性面GaN，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面。
所述非极性GaN缓冲层是采用PLD技术来实现低温下在LiGaO2衬底上外延生长，能够有效缓解高温生长引起LiGaO2衬底中的Li原子逸出、并与非极性GaN缓冲层之间发生严重界面反应的问题。
所述GaN纳米柱阵列是通过采用TracePro软件优化纳米柱排布，利用纳米 压印技术和刻蚀在非极性GaN缓冲层上制备而成，所获得的纳米柱阵列尺寸均匀。将生长在LiGaO2衬底上的GaN纳米柱阵列转移到金属有机化合物气相沉积反应腔(MOCVD)中通过选区生长进行纳米柱LED的制备。
所述GaN纳米柱阵列的高度为500～1000nm，间距为150～250nm，直径为100～200nm。
所述非掺杂GaN层的厚度为200～300nm；所述n型掺杂GaN层的掺杂浓度为3×1018～9×1018cm-3，厚度为2～4μm。
所述InGaN/GaN量子阱为8～13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3～5nm，GaN垒层的厚度为10～15nm。
所述p型掺杂GaN层，掺杂浓度为3×1017～9×1017cm-3，厚度为300～350nm。
所述隔离层的厚度为10～50nm；
所述生长在镓酸锂衬底上的非极性纳米柱LED的制备方法，包括以下步骤：
(1)衬底及其晶向的选取：采用LiGaO2衬底，以(100)面偏(110)方向0.2～1°为外延面，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；
(2)衬底表面抛光、清洗以及退火处理，所述退火的具体过程为：将衬底放入退火室内，在800～900℃下空气氛围中对LiGaO2衬底进行退火处理3～4小时然后空冷至室温；
(3)非极性GaN缓冲层外延生长：采用PLD技术，衬底温度为150～250℃，氮的等离子体流量为3～4.5sccm，RF活化功率为400～450W的条件下生长非极性GaN缓冲层，缓冲层厚度为500～1000nm；，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；所述采用PLD技术中衬底转速为10r/min，靶基距为5cm，激光波长为248nm，激光能量为250mJ/p，频率20Hz；Ga源为GaN靶材，其纯度为99.99％；
(4)GaN纳米柱阵列的制备：通过采用TracePro软件优化纳米柱排布，利用纳米压印技术和干法刻蚀工艺对LiGaO2衬底上非极性GaN缓冲层进行向下刻蚀，得到GaN纳米柱阵列，其高度为500～1000nm，直径为100～200nm，间距为150～250nm；所述GaN纳米柱阵列的高度与非极性GaN缓冲层的高度相同；
(5)隔离层的沉积：利用化学气相沉积、原子层沉积或磁控溅射技术在GaN纳米柱阵列中纳米柱的侧壁以及未被纳米柱阵列覆盖的衬底上沉积隔离层，所述隔离层的材料为SiNx、SiO2或者Al2O3，厚度为10～50nm；
(6)非掺杂GaN层的外延生长：在MOCVD中，反应室温度为1000～1300℃，反应室的压力为150～200Torr，在GaN纳米柱阵列上生长非掺杂GaN层，厚度为200～300nm；
(7)n型掺杂GaN层的外延生长：将反应室温度升至1000～1500℃，在反应室压力为150～200Torr条件下，在步骤(6)得到的非掺杂GaN层上生长n型掺杂GaN层，掺杂浓度为3×1018～9×1018cm-3，厚度为2～4μm；
(8)InGaN/GaN多量子阱的外延生长：反应室温度降低至700～780℃，在反应室的压力为150～200Torr条件下，通入氨气、氮气、三甲基镓和三甲基铟，在步骤(7)得到的n型掺杂GaN层上生长InGaN/GaN多量子阱，InGaN/GaN量子阱为8～13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3～5nm，GaN垒层的厚度为10～15nm；
(9)p型掺杂GaN层的外延生长：反应室温度升高至900～1100℃，在反应室的压力为150～200Torr条件下，通入二茂镁、氨气、氮气、三甲基镓，在步骤(8)得到的InGaN/GaN多量子阱上生长p型掺杂GaN层，掺杂浓度为3×1017～9×1017cm-3，厚度为300～350nm。
步骤(6)所述非掺杂GaN层的外延生长中Ga源为TMGa；氮源为NH3；Ga源的流量为350～450sccm、氮源流量为50～65slm；
步骤(7)所述n型掺杂GaN层的外延生长中掺杂的掺杂源为硅烷；Ga源为TMGa；氮源为NH3；各源的流量为：Ga源350～450sccm、氮源50～65slm、掺杂源100～200sccm；
步骤(8)所述氨气的流量为25～35slm、氮气的流量为25～35slm、三甲基镓的流量为100～150sccm，三甲基铟的流量为450～550sccm；
步骤(9)所述三甲基镓的流量为350～450sccm、氨气的流量为50～65slm、氮气的流量为50～65slm、二茂镁的流量为150～250sccm。
步骤(1)所述衬底表面抛光，具体为：首先将LiGaO2衬底表面用金刚石泥浆进行抛光，配合光学显微镜观察衬底表面，直到没有划痕后，再采用化学 机械抛光的方法进行抛光处理。
所述清洗，具体为：将LiGaO2衬底放入去离子水中室温下超声清洗3～5分钟，去除LiGaO2衬底表面粘污颗粒，再依次经过盐酸、丙酮、乙醇洗涤，去除表面有机物，用干燥氮气吹干。
与现有技术相比，本发明具有以下优点和有益效果：
(1)本发明使用LiGaO2作为衬底，LiGaO2衬底容易获得，价格便宜，有利于降低生产成本。
(2)本发明采用纳米压印技术和刻蚀获得高质量纳米柱阵列，然后将生长在衬底上纳米柱阵列转移至MOCVD通过选区生长进行纳米柱LED外延材料的制备；既降低了纳米柱LED的生长难度，又消除了使用催化剂而引入杂质的不良影响，有利于获得尺寸可控，取向均一的高质量纳米柱LED。
(3)本发明充分利用了PLD和MOCVD的各自优势：首先使用PLD技术在LiGaO2衬底上采用低温(150～250℃)先外延生长一层GaN或缓冲层，成功抑制界面反应，为下一步制备高质量低缺陷的纳米柱阵列做好铺垫；随后转移至MOCVD中高温外延u-GaN、n-GaN、P-GaN和量子阱等，充分发挥了MOCVD的优势，提高了生长速率和产能；
(4)本发明采用与GaN晶格失配和热失配度低的LiGaO2(100)作为衬底生长非极性纳米柱LED，不仅能够有效地减少热应力，减少位错的形成，而且有效消除量子束缚斯塔克效应的影响；所制备出的高质量非极性纳米柱LED外延材料可大幅度提高氮化物器件如半导体激光器、发光二极管及太阳能电池的发光效率。
附图说明
图1是本发明的生长在镓酸锂(LiGaO2)衬底上的纳米柱LED的正视图；
图2是实施例1制备的非极性GaN缓冲层的XRD衍射图；
图3是实施例1制备的GaN纳米柱阵列的截面示意图；
图4是实施例1的生长在镓酸锂(LiGaO2)衬底上的纳米柱LED的俯视图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明的生长在镓酸锂(LiGaO2)衬底上的纳米柱LED的正视图如图1所示，包括LiGaO2衬底10，生长在LiGaO2衬底10上GaN纳米柱阵列11(所述GaN纳米柱阵列是由生长在LiGaO2衬底上的非极性GaN缓冲层经过纳米压印技术和刻蚀制备而成)，沉积在GaN纳米柱阵列11侧壁和未被纳米柱阵列覆盖的LiGaO2衬底10上的隔离层12，生长在GaN纳米柱阵列11上的非掺杂GaN层13，生长在非掺杂GaN层13上的n型掺杂GaN层14，生长在n型掺杂GaN层14上的InGaN/GaN量子阱15，生长在InGaN/GaN量子阱15上的p型掺杂GaN层16。
所述LiGaO2衬底以(100)面偏(110)方向0.2～1°为外延面。GaN纳米柱阵列是非极性面GaN，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面。
所述GaN纳米柱阵列的高度为500～1000nm，间距为150～250nm，直径为100～200nm。所述非掺杂GaN层的厚度为200～300nm；所述n型掺杂GaN层的厚度为2～4μm；所述InGaN/GaN量子阱为8～13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3～5nm，GaN垒层的厚度为10～15nm；
所述p型掺杂GaN层的厚度为300～350nm。所述隔离层的厚度为10～50nm。
实施例1
本实施例的生长在镓酸锂衬底上的纳米柱LED的制备方法，包括以下步骤：
(1)衬底以及其晶向的选取：采用LiGaO2衬底，以(100)面偏(110)方向0.6°为外延面；
(2)衬底表面抛光、清洗以及退火处理，所述退火的具体过程为：将衬底放入退火室内，在880℃下空气氛围中对LiGaO2衬底进行退火处理3小时然后空冷至室温；
所述衬底表面抛光，具体为：首先将LiGaO2衬底表面用金刚石泥浆进行抛光，配合光学显微镜观察衬底表面，直到没有划痕后，再采用化学机械抛光的方法进行抛光处理；
所述清洗，具体为：将LiGaO2衬底放入去离子水中室温下超声清洗3分钟，去除LiGaO2衬底表面粘污颗粒，再依次经过盐酸、丙酮、乙醇洗涤，去除表面有机物，用干燥氮气吹干；
(3)非极性缓冲层外延生长：采用PLD技术，衬底温度为200℃，衬底转速为10r/min，靶基距为5cm，激光波长为248nm，激光能量为250mJ/p，频率20Hz，氮的等离子体流量为4sccm，RF活化功率为420W的条件下生长非极性GaN缓冲层，厚度为500nm；晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；Ga源为GaN靶材，其纯度为99.99％；
(4)纳米柱阵列的制备：通过采用TracePro软件优化纳米柱排布，利用纳米压印技术和干法刻蚀工艺对LiGaO2衬底上非极性GaN缓冲层进行向下刻蚀，得到GaN纳米柱阵列，纳米柱的高度为500nm，直径为200nm，相邻间距为250nm；
(5)隔离层的沉积：利用化学气相沉积、原子层沉积或磁控溅射技术在GaN纳米柱阵列中纳米柱的侧壁和未被纳米柱覆盖的衬底上沉积隔离层，所述纳米柱侧壁隔离层的材料为SiNx，厚度为10nm；
(6)非掺杂GaN层的外延生长：在MOCVD中，反应室温度为1200℃，反应室的压力为150Torr，GaN纳米柱阵列上生长非掺杂GaN层，厚度为200nm；Ga源为TMGa；氮源为NH3；各源的气体流量为Ga源380sccm、氮源56slm；
(7)n型掺杂GaN层的外延生长：将反应室温度升至1200℃，在反应室压力为150Torr条件下，在步骤(6)得到的非掺杂GaN层上生长n型掺杂GaN层，掺杂浓度为3×1018cm-3，厚度为2μm；掺杂源为硅烷；Ga源为TMGa；氮源为NH3；各源的气体流量为：Ga源380sccm、氮源56slm、掺杂源125sccm；
(8)InGaN/GaN多量子阱的外延生长：反应室温度降低至720℃，在反应室的压力为150Torr条件下，通入氨气、氮气、三甲基镓和三甲基铟，在步骤(7)得到的n型掺杂GaN层上生长InGaN/GaN多量子阱，InGaN/GaN量子阱为8个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3nm，GaN垒层的厚度为10nm；各源的流量为：铟源475sccm、镓源140sccm、氮源27slm；
(9)p型掺杂GaN层的外延生长：反应室温度升高至900～1100℃，在反应室的压力为150Torr条件下，通入二茂镁、氨气、氮气和，三甲基镓流量为380sccm、氨气、氮气的流量分别56slm、二茂镁的流量为200sccm，在步骤(8)得到的InGaN/GaN多量子阱上生长p型掺杂GaN层，掺杂浓度为3×1017cm-3，厚度为300nm。
实施例1制备的非极性GaN缓冲层的XRD衍射图如图2所示；从图2可知，本实施例制备的生长在镓酸锂衬底上的非极性缓冲层：GaN是m面，XRD的衍射角2θ＝32.31°，即非极性面的GaN。
本实施例中在非极性GaN缓冲层上刻蚀成的GaN纳米阵列的截面示意图如图3所示。
本实施例制备的生长在镓酸锂衬底上的纳米柱LED的俯视图如图4所示。
实施例2
本实施例的生长在镓酸锂衬底上的纳米柱LED的制备方法，包括以下步骤：
(1)衬底以及其晶向的选取：采用LiGaO2衬底，以(100)面偏(110)方向0.5°为外延面；
(2)衬底表面抛光、清洗以及退火处理，所述退火的具体过程为：将衬底放入退火室，在800～900℃下空气氛围中对LiGaO2衬底进行退火处理4小时然后空冷至室温；
所述衬底表面抛光，具体为：首先将LiGaO2衬底表面用金刚石泥浆进行抛光，配合光学显微镜观察衬底表面，直到没有划痕后，再采用化学机械抛光的方法进行抛光处理；
所述清洗，具体为：将LiGaO2衬底放入去离子水中室温下超声清洗3分钟，去除LiGaO2衬底表面粘污颗粒，再依次经过盐酸、丙酮、乙醇洗涤，去除表面有机物，用干燥氮气吹干；
(3)非极性缓冲层外延生长：采用PLD技术，衬底温度调为150～250℃，衬底转速为10r/min，靶基距为5cm，激光波长为248nm，激光能量为250mJ/p，频率20Hz，氮的等离子体流量为3～4.5sccm，RF活化功率为400～450W的条件下生长非极性GaN缓冲层，缓冲层厚度为1000nm；晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；Ga源为GaN靶材，其纯度为99.99％；
(4)纳米柱阵列的制备：通过采用TracePro软件优化纳米柱排布，利用纳米压印技术和干法刻蚀工艺对LiGaO2衬底上非极性GaN缓冲层进行向下刻蚀，得到GaN纳米柱阵列，纳米柱的高度为1000nm，直径为100nm，间距为150nm；
(5)隔离层的沉积：利用化学气相沉积、原子层沉积或磁控溅射技术在 GaN纳米柱阵列的侧壁和未被纳米柱覆盖的衬底上沉积隔离层，所述隔离层的材料为SiO2，厚度为50nm；
(6)非掺杂GaN层的外延生长：在MOCVD中，反应室温度为1100℃，反应室的压力为200Torr，在GaN纳米柱阵列上生长非掺杂GaN层，厚度为300nm；Ga源为TMGa；氮源为NH3；各源的气体流量为Ga源380sccm、氮源56slm；
(7)n型掺杂GaN层的外延生长：将反应室温度升至1500℃，在反应室压力为200Torr条件下，在步骤(6)得到的非掺杂GaN层上生长n型掺杂GaN层，掺杂浓度为9×1018cm-3，厚度为4μm；掺杂源为硅烷；Ga源为TMGa；氮源为NH3；各源的气体流量为Ga源380sccm、氮源56slm、掺杂源125sccm；
(8)InGaN/GaN多量子阱的外延生长：反应室温度降低至750℃，在反应室的压力为200Torr条件下，通入氨气、氮气、三甲基镓和三甲基铟，在步骤(7)得到的n型掺杂GaN层上生长InGaN/GaN多量子阱，InGaN/GaN量子阱为13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为5nm，GaN垒层的厚度为15nm；铟源的流量为475sccm、镓源的流量为140sccm、氮源的流量为27slm；
(9)p型掺杂GaN层的外延生长：反应室温度升高至1000℃，在反应室的压力为150Torr条件下，通入二茂镁、氨气、氮气和三甲基镓，在步骤(8)得到的InGaN/GaN多量子阱上生长p型掺杂GaN层，掺杂浓度为9×1017cm-3，厚度为350nm；各源的气体流量为：Ga源380sccm、氮源56slm、掺杂源200sccm。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

  1. 生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：包括LiGaO2衬底，生长在LiGaO2衬底上的GaN纳米柱阵列，生长在GaN纳米柱阵列上的非掺杂GaN层，生长在非掺杂GaN层上的n型掺杂GaN层，生长在n型掺杂GaN层上的InGaN/GaN量子阱，生长在InGaN/GaN量子阱上的p型掺杂GaN层；所述GaN纳米柱阵列为非极性GaN纳米柱阵列。
  2. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述LiGaO2衬底以(100)面偏(110)方向0.2～1°为外延面。
  3. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述GaN纳米柱阵列是由生长在LiGaO2衬底上的非极性GaN缓冲层制备而成的；所述非极性GaN缓冲层是非极性面GaN，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；
    GaN纳米柱阵列是非极性面GaN，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面。
  4. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述GaN纳米柱阵列的高度为500～1000nm，间距为150～250nm，直径为100～200nm。
  5. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述非掺杂GaN层的厚度为200～300nm；所述n型掺杂GaN层的厚度为2～4μm；
    所述InGaN/GaN量子阱为8～13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3～5nm，GaN垒层的厚度为10～15nm；
    所述p型掺杂GaN层的厚度为300～350nm。
  6. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述n型掺杂GaN层的掺杂浓度为3×1018～9×1018cm-3；所述p型掺杂GaN层的掺杂浓度为3×1017～9×1017cm-3。
  7. 根据权利要求1所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述生长在镓酸锂衬底上的非极性纳米柱LED还包括隔离层，所述隔离层沉积在GaN纳米柱阵列的侧壁和未被纳米柱阵列覆盖的LiGaO2衬底 上。
  8. 根据权利要求7所述生长在镓酸锂衬底上的非极性纳米柱LED，其特征在于：所述隔离层的材料为SiNx、SiO2或者Al2O3；所述隔离层的厚度为10～50nm。
  9. 根据权利要求1～8任一项所述生长在镓酸锂衬底上的非极性纳米柱LED的制备方法，其特征在于：包括以下步骤：
    (1)衬底及其晶向的选取：采用LiGaO2衬底，以(100)面偏(110)方向0.2～1°为外延面，晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；
    (2)衬底表面抛光、清洗以及退火处理，所述退火的具体过程为：将衬底放入退火室内，在800～900℃下空气氛围中对LiGaO2衬底进行退火处理3～4小时然后空冷至室温；
    (3)非极性GaN缓冲层外延生长：采用PLD技术，衬底温度为150～250℃，氮的等离子体流量为3～4.5sccm，RF活化功率为400～450W的条件下生长非极性GaN缓冲层，缓冲层厚度为500～1000nm；晶体外延取向关系为：GaN的(1-100)面平行于LiGaO2的(100)面；所述采用PLD技术中衬底转速为10r/min，靶基距为5cm，激光波长为248nm，激光能量为250mJ/p，频率20Hz；Ga源为GaN靶材；
    (4)GaN纳米柱阵列的制备：通过采用TracePro软件优化纳米柱排布，利用纳米压印技术和干法刻蚀工艺对LiGaO2衬底上非极性GaN缓冲层进行向下刻蚀，得到GaN纳米柱阵列，其高度为500～1000nm，直径为100～200nm，间距为150～250nm；所述GaN纳米柱阵列的高度与非极性GaN缓冲层的高度相同；
    (5)隔离层的沉积：利用化学气相沉积、原子层沉积或磁控溅射技术在GaN纳米柱阵列中纳米柱的侧壁以及未被纳米柱阵列覆盖的衬底上沉积隔离层，所述隔离层的材料为SiNx、SiO2或者Al2O3，厚度为10～50nm；
    (6)非掺杂GaN层的外延生长：在MOCVD中，反应室温度为1000～1300℃，反应室的压力为150～200Torr，在GaN纳米柱阵列上生长非掺杂GaN层，厚度为200～300nm；
    (7)n型掺杂GaN层的外延生长：将反应室温度升至1000～1500℃，在反应室压力为150～200Torr条件下，在步骤(6)得到的非掺杂GaN层上生长n型掺杂GaN层，掺杂浓度为3×1018～9×1018cm-3，厚度为2～4μm；
    (8)InGaN/GaN多量子阱的外延生长：反应室温度降低至700～780℃，在反应室的压力为150～200Torr条件下，通入氨气、氮气、三甲基镓和三甲基铟，在步骤(7)得到的n型掺杂GaN层上生长InGaN/GaN多量子阱，InGaN/GaN量子阱为8～13个周期的InGaN阱层/GaN垒层，其中InGaN阱层的厚度为3～5nm，GaN垒层的厚度为10～15nm；
    (9)p型掺杂GaN层的外延生长：反应室温度升高至900～1100℃，在反应室的压力为150～200Torr条件下，通入二茂镁、氨气、氮气和三甲基镓，在步骤(8)得到的InGaN/GaN多量子阱上生长p型掺杂GaN层，掺杂浓度为3×1017～9×1017cm-3，厚度为300～350nm。
  10. 根据权利要求9所述生长在镓酸锂衬底上的非极性纳米柱LED的制备方法，其特征在于：步骤(6)所述非掺杂GaN层的外延生长中Ga源为TMGa；氮源为NH3；Ga源的流量为350～450sccm、氮源流量为50～65slm；
    步骤(7)所述n型掺杂GaN层的外延生长中掺杂的掺杂源为硅烷；Ga源为TMGa；氮源为NH3；各源的流量为：Ga源350～450sccm、氮源50～65slm、掺杂源100～200sccm；
    步骤(8)所述氨气的流量为25～35slm、氮气的流量为25～35slm、三甲基镓的流量为100～150sccm，三甲基铟的流量为450～550sccm；
    步骤(9)所述三甲基镓的流量为350～450sccm、氨气的流量为50～65slm、氮气的流量为50～65slm、二茂镁的流量为150～250sccm。
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