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CN115472720B - Light emitting diode epitaxial wafer, preparation method thereof and light emitting diode - Google Patents

Light emitting diode epitaxial wafer, preparation method thereof and light emitting diode Download PDF

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CN115472720B
CN115472720B CN202211341605.8A CN202211341605A CN115472720B CN 115472720 B CN115472720 B CN 115472720B CN 202211341605 A CN202211341605 A CN 202211341605A CN 115472720 B CN115472720 B CN 115472720B
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CN115472720A (en
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张彩霞
印从飞
程金连
刘春杨
胡加辉
金从龙
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Jiangxi Zhao Chi Semiconductor Co Ltd
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10HINORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80Constructional details
    • H10H20/81Bodies
    • H10H20/815Bodies having stress relaxation structures, e.g. buffer layers
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05FSTATIC ELECTRICITY; NATURALLY-OCCURRING ELECTRICITY
    • H05F1/00Preventing the formation of electrostatic charges
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10HINORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01Manufacture or treatment
    • H10H20/011Manufacture or treatment of bodies, e.g. forming semiconductor layers
    • H10H20/013Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials
    • H10H20/0133Manufacture 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
    • H10H20/01335Manufacture 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

本发明公开了一种发光二极管外延片及其制备方法、发光二极管,所述发光二极管外延片包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;所述插入层包括SixN1‑x裂纹层、Al1‑yScyN预处理层和GaN帽层,所述SixN1‑x裂纹层、Al1‑yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x的取值范围为0.1‑0.4;y的取值范围为0.1‑0.3。本发明制得的发光二极管外延片的工作电压更低,具有更好的抗静电能力。

Figure 202211341605

The invention discloses a light-emitting diode epitaxial wafer, a preparation method thereof, and a light-emitting diode. The light-emitting diode epitaxial wafer includes a substrate, a buffer layer sequentially stacked on the substrate, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, multi-quantum well layer, electron blocking layer, P-type GaN layer; the insertion layer includes Six N 1-x crack layer, Al 1-y Sc y N pretreatment layer and GaN cap layer, the Six The N 1‑x crack layer, the Al 1‑y Sc y N pretreatment layer and the GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein the value range of x is 0.1‑0.4; the value range of y is 0.1-0.3. The light-emitting diode epitaxial wafer prepared by the invention has lower operating voltage and better antistatic ability.

Figure 202211341605

Description

发光二极管外延片及其制备方法、发光二极管Light-emitting diode epitaxial wafer and preparation method thereof, light-emitting diode

技术领域technical field

本发明涉及光电技术领域,尤其涉及一种发光二极管外延片及其制备方法、发光二极管。The invention relates to the field of photoelectric technology, in particular to a light-emitting diode epitaxial wafer, a preparation method thereof, and a light-emitting diode.

背景技术Background technique

目前,GaN基发光二极管已经大量应用于固态照明领域以及显示领域,吸引着越来越多的人关注。GaN基发光二极管已经实现工业化生产、在背光源、照明、景观灯等方面都有应用。At present, GaN-based light-emitting diodes have been widely used in the fields of solid-state lighting and display, attracting more and more people's attention. GaN-based light-emitting diodes have been industrialized and used in backlights, lighting, and landscape lights.

对于常规结构的LED器件,在N型半导体层生长过程中,N型掺杂的浓度非常高,GaN材料的结晶完整性会随着N型掺杂的并入而降低,并且高的N型掺杂会引入很大的应力。而且,由于本征GaN的生长温度很高,从缓冲层累积的应力在生长N型GaN层时达到了最大值,导致在生长N型掺杂时翘曲很大,应力累积使得N型掺杂困难,尤其是外延片边缘位置,常常会导致N型掺杂不均匀,从而导致工作电压升高,并且容易出现由于翘曲大而导致的外延片表面雾化等缺陷,晶格质量变差,影响发光二极管的抗静电能力。For LED devices with conventional structures, during the growth of N-type semiconductor layers, the concentration of N-type doping is very high, and the crystalline integrity of GaN materials will decrease with the incorporation of N-type doping, and high N-type doping Miscellaneous can introduce great stress. Moreover, due to the high growth temperature of intrinsic GaN, the stress accumulated from the buffer layer reaches the maximum when growing the N-type GaN layer, resulting in a large warp when growing the N-type doped layer, and the stress accumulation makes the N-type doped Difficulties, especially the edge position of the epitaxial wafer, often lead to uneven N-type doping, which leads to an increase in operating voltage, and is prone to defects such as fogging on the surface of the epitaxial wafer due to large warpage, and the quality of the lattice deteriorates. Affect the antistatic ability of light-emitting diodes.

发明内容Contents of the invention

本发明所要解决的技术问题在于,提供一种发光二极管外延片,其能够释放底层应力,增加了外延层平整度,增加N型掺杂的均匀性,从而降低工作电压,增加发光二极管的抗静电能力。The technical problem to be solved by the present invention is to provide a light-emitting diode epitaxial wafer, which can release the underlying stress, increase the flatness of the epitaxial layer, increase the uniformity of N-type doping, thereby reducing the operating voltage and increasing the antistatic properties of the light-emitting diode. ability.

本发明所要解决的技术问题还在于,提供一种发光二极管外延片的制备方法,其工艺简单,生产良品率高。The technical problem to be solved by the present invention is also to provide a method for preparing a light-emitting diode epitaxial wafer, which has a simple process and a high production yield.

为了解决上述技术问题,本发明提供了一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;In order to solve the above technical problems, the present invention provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, and a multi-quantum well layer sequentially stacked on the substrate. , electron blocking layer, P-type GaN layer;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3.

在一种实施方式中,所述插入层的厚度为50nm-70nm;In one embodiment, the thickness of the insertion layer is 50nm-70nm;

其中,所述SixN1-x裂纹层的厚度为10nm-20nm;Wherein, the thickness of the Six N 1-x crack layer is 10nm-20nm;

所述Al1-yScyN预处理层的厚度为20nm-30nm;The thickness of the Al 1-y Sc y N pretreatment layer is 20nm-30nm;

所述GaN帽层的厚度为20nm-30nm。The thickness of the GaN cap layer is 20nm-30nm.

在一种实施方式中,所述缓冲层的厚度为10nm-100nm;In one embodiment, the thickness of the buffer layer is 10nm-100nm;

所述本征GaN层的厚度为300nm-800nm;The thickness of the intrinsic GaN layer is 300nm-800nm;

所述N型GaN层的厚度为1μm-3μm,所述N型GaN层为Si掺杂,所述Si的掺杂浓度为5×1018-1×1019cm-3The thickness of the N-type GaN layer is 1 μm-3 μm, the N-type GaN layer is doped with Si, and the doping concentration of Si is 5×10 18 -1×10 19 cm -3 ;

所述P型GaN层的厚度为10nm-50nm,所述P型GaN层为Mg掺杂,所述Mg的掺杂浓度为5×1017-1×1020cm-3The thickness of the P-type GaN layer is 10nm-50nm, the P-type GaN layer is doped with Mg, and the doping concentration of Mg is 5×10 17 -1×10 20 cm -3 .

在一种实施方式中,所述多量子阱层包括交替堆叠的InGaN量子阱层和GaN量子垒层,堆叠周期数为3-15;In one embodiment, the multi-quantum well layer includes alternately stacked InGaN quantum well layers and GaN quantum barrier layers, and the number of stacking periods is 3-15;

所述InGaN量子阱层的厚度为2nm-4nm;The thickness of the InGaN quantum well layer is 2nm-4nm;

所述GaN量子垒层的厚度为9nm-11nm。The thickness of the GaN quantum barrier layer is 9nm-11nm.

在一种实施方式中,所述电子阻挡层包括交替堆叠的AlGaN层和InGaN层,堆叠周期数为3-15;In one embodiment, the electron blocking layer includes alternately stacked AlGaN layers and InGaN layers, and the number of stacking periods is 3-15;

所述AlGaN层的厚度为5nm-7nm;The thickness of the AlGaN layer is 5nm-7nm;

所述InGaN层的厚度为5nm-7nm。The thickness of the InGaN layer is 5nm-7nm.

为解决上述问题,本发明还提供了一种发光二极管外延片的制备方法,包括以下步骤:In order to solve the above problems, the present invention also provides a method for preparing a light-emitting diode epitaxial wafer, comprising the following steps:

准备衬底;Prepare the substrate;

在所述衬底上依次沉积缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层和P型GaN层;sequentially depositing a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P-type GaN layer on the substrate;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3.

在一种实施方式中,采用下述方法完成所述SixN1-x裂纹层的沉积:In one embodiment, the deposition of the Si x N 1-x crack layer is accomplished by the following method:

将反应室温度控制在1100℃-1150℃,压力为50Torr-100Torr,通入H2/N2做载气,通入NH3做N源,通入SiH4作为Si源,完成沉积。The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 50Torr-100Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and SiH 4 is fed as Si source to complete the deposition.

在一种实施方式中,采用下述方法完成所述Al1-yScyN预处理层的沉积:In one embodiment, the deposition of the Al 1-y S y N pretreatment layer is accomplished by the following method:

将反应室温度控制在200℃-1000℃,压力为5mTorr-10mTorr,通入Ar做载气,通入N2做反应气,以ScAl合金靶材为溅射靶材,完成沉积。The temperature of the reaction chamber is controlled at 200°C-1000°C, the pressure is 5mTorr-10mTorr, Ar is passed in as the carrier gas, N 2 is passed in as the reaction gas, and the ScAl alloy target is used as the sputtering target to complete the deposition.

在一种实施方式中,采用下述方法完成所述GaN帽层的沉积:In one embodiment, the deposition of the GaN cap layer is accomplished by the following method:

将反应室温度控制在900℃-1000℃,压力为100Torr-300Torr,通入H2/N2做载气,通入NH3做N源,通入TMGa作为Ga源,完成沉积。The temperature of the reaction chamber is controlled at 900°C-1000°C, the pressure is 100Torr-300Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and TMGa is fed as Ga source to complete the deposition.

在一种实施方式中,采用下述方法完成在所述衬底的正面沉积所述缓冲层:In one embodiment, the buffer layer is deposited on the front side of the substrate by the following method:

将反应室温度控制在500℃-700℃,压力为200Torr-400Torr,通入TMAl作为Al源,通入NH3作为N源,完成在所述衬底的正面沉积缓冲层;The temperature of the reaction chamber is controlled at 500°C-700°C, the pressure is 200Torr-400Torr, TMAl is introduced as the Al source, NH3 is introduced as the N source, and the buffer layer is deposited on the front side of the substrate;

和/或,采用下述方法完成在所述缓冲层上沉积所述本征GaN层:And/or, the following method is used to complete the deposition of the intrinsic GaN layer on the buffer layer:

将反应室温度控制在1100℃-1150℃,压力为100Torr-500Torr,通入NH3作为N源,通入TMGa作为Ga源,完成在所述缓冲层上沉积所述本征GaN层;Control the temperature of the reaction chamber at 1100°C-1150°C, the pressure at 100Torr-500Torr, feed NH 3 as the N source, and feed TMGa as the Ga source, and complete the deposition of the intrinsic GaN layer on the buffer layer;

和/或,采用下述方法完成在所述插入层上沉积所述N型GaN层:And/or, the following method is used to finish depositing the N-type GaN layer on the insertion layer:

将反应室温度控制在1100℃-1150℃,压力为100Torr-500Torr,通入SiH4作为Si源,通入NH3作为N源,通入TMGa作为Ga源,完成在所述插入层上沉积所述N型GaN层;The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 100Torr-500Torr, SiH 4 is introduced as the Si source, NH 3 is introduced as the N source, and TMGa is introduced as the Ga source to complete the deposition on the insertion layer. The N-type GaN layer;

和/或,采用下述方法完成在所述电子阻挡层上沉积所述P型GaN层:And/or, the following method is used to finish depositing the P-type GaN layer on the electron blocking layer:

将反应室温度控制在800℃-1000℃,压力为100Torr-300Torr,通入NH3作为N源,通入TMGa作为Ga源,通入CP2Mg作为Mg源,完成在所述电子阻挡层上沉积所述P型GaN层。The temperature of the reaction chamber is controlled at 800°C-1000°C, the pressure is 100Torr-300Torr, and NH 3 is introduced as the N source, TMGa as the Ga source, and CP 2 Mg as the Mg source, and completed on the electron blocking layer. The P-type GaN layer is deposited.

在一种实施方式中,采用下述方法完成在所述N型GaN层上沉积所述多量子阱层:In one embodiment, the following method is used to complete the deposition of the multiple quantum well layer on the N-type GaN layer:

在所述N型GaN层上交替沉积InGaN量子阱层和GaN量子垒层,堆叠层数在3~15;Alternately depositing InGaN quantum well layers and GaN quantum barrier layers on the N-type GaN layer, the number of stacked layers is 3-15;

其中,所述InGaN量子阱层的沉积步骤包括:Wherein, the deposition step of the InGaN quantum well layer comprises:

将反应室温度控制在700℃-800℃,压力为100Torr-500Torr,通入TMIn作为In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积;Control the temperature of the reaction chamber at 700°C-800°C, the pressure at 100Torr-500Torr, feed TMIn as the In source, NH3 as the N source, and TMGa as the Ga source to complete the deposition;

所述GaN量子垒层的沉积步骤包括:The deposition steps of the GaN quantum barrier layer include:

将反应室温度控制在800℃-900℃,压力为100Torr-500Torr,通入NH3作为N源,通入TMGa作为Ga源,完成沉积。The temperature of the reaction chamber is controlled at 800°C-900°C, the pressure is 100Torr-500Torr, NH 3 is fed in as the N source, and TMGa is fed in as the Ga source to complete the deposition.

在一种实施方式中,采用下述方法完成在所述多量子阱层上沉积所述电子阻挡层:In one embodiment, the following method is used to complete depositing the electron blocking layer on the multiple quantum well layer:

在所述多量子阱层上交替沉积AlGaN层和InGaN层,堆叠层数在3~15;AlGaN layers and InGaN layers are alternately deposited on the multi-quantum well layer, and the number of stacked layers is 3 to 15;

其中,所述AlGaN层的沉积步骤包括:Wherein, the deposition step of the AlGaN layer includes:

将反应室温度控制在900℃-1000℃,压力为100Torr-500Torr,通入TMAl作为Al源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积;The temperature of the reaction chamber is controlled at 900°C-1000°C, the pressure is 100Torr-500Torr, and the deposition is completed by feeding TMAl as the Al source, NH3 as the N source, and TMGa as the Ga source;

所述InGaN层的沉积步骤包括:The deposition steps of the InGaN layer include:

将反应室温度控制在900℃-1000℃,压力为100Torr-500Torr,通入TMIn作为In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积。Control the temperature of the reaction chamber at 900°C-1000°C, the pressure at 100Torr-500Torr, feed TMIn as the In source, NH3 as the N source, and TMGa as the Ga source to complete the deposition.

相应地,本发明还提供了一种发光二极管,所述发光二极管包括所述的发光二极管外延片。Correspondingly, the present invention also provides a light emitting diode, which includes the light emitting diode epitaxial wafer.

实施本发明,具有如下有益效果:Implement the present invention, have following beneficial effect:

本发明提供的发光二极管外延片,在本征GaN层和N型半导体层中间加入插入层,在重掺杂的N型GaN半导体生长之前,充分释放了底层应力,增加了外延层平整度,减少了N型重掺生长的应力,增加N型掺杂的均匀性,并且增加了N型掺杂的并入,成功降低了工作电压,增加了外延片表面平整度,增加了发光二极管的抗静电能力。In the light-emitting diode epitaxial wafer provided by the present invention, an insertion layer is added between the intrinsic GaN layer and the N-type semiconductor layer, and before the heavily doped N-type GaN semiconductor grows, the underlying stress is fully released, the flatness of the epitaxial layer is increased, and the Reduce the stress of N-type heavy doping growth, increase the uniformity of N-type doping, and increase the incorporation of N-type doping, successfully reduce the operating voltage, increase the surface flatness of epitaxial wafers, and increase the antistatic of light-emitting diodes ability.

附图说明Description of drawings

图1为本发明提供的发光二极管外延片的结构示意图,其中,衬底为1、缓冲层为2、本征GaN层为3、SixN1-x裂纹层41、Al1-yScyN预处理层42、GaN帽层43、N型GaN层为5、多量子阱层为6、电子阻挡层为7、P型GaN层为8。Fig. 1 is a schematic structural diagram of a light-emitting diode epitaxial wafer provided by the present invention, wherein, the substrate is 1, the buffer layer is 2, the intrinsic GaN layer is 3, the Six N 1-x crack layer 41, Al 1-y Sc y N pretreatment layer 42 , GaN cap layer 43 , N-type GaN layer is 5 , multi-quantum well layer is 6 , electron blocking layer is 7 , and P-type GaN layer is 8 .

具体实施方式Detailed ways

为使本发明的目的、技术方案和优点更加清楚,下面对本发明作进一步地详细描述。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below.

除非另外说明或存在矛盾之处,本文中使用的术语或短语具有以下含义:Unless otherwise stated or contradictory, terms and phrases used herein have the following meanings:

本发明中,所使用的“其组合”、“其任意组合”、“其任意组合方式”等中包括所列项目中任两个或任两个以上项目的所有合适的组合方式。In the present invention, "its combination", "any combination thereof", "any combination thereof" and the like include all suitable combinations of any two or more of the listed items.

本发明中,“优选”仅为描述效果更好的实施方式或实施例,应当理解,并不构成对本发明保护范围的限制。In the present invention, "preferred" is only to describe an implementation or an example with better effects, and it should be understood that it does not constitute a limitation to the protection scope of the present invention.

本发明中,以开放式描述的技术特征中,包括所列举特征组成的封闭式技术方案,也包括包含所列举特征的开放式技术方案。In the present invention, the technical features described in open form include closed technical solutions consisting of the enumerated features, as well as open technical solutions including the enumerated features.

本发明中,涉及到数值区间,如无特别说明,则包括数值区间的两个端点。In the present invention, when referring to a numerical interval, unless otherwise specified, both endpoints of the numerical interval are included.

目前,传统N型半导体层,生长时累计应力很多,翘曲很大,容易出现表面雾化,晶格质量差,影响发光二极管的抗静电能力。并且由于翘曲大,从而N型掺杂不均匀,导致发光二极管的工作电压高。At present, the traditional N-type semiconductor layer has a lot of cumulative stress during growth, large warpage, prone to surface atomization, and poor lattice quality, which affects the antistatic ability of light-emitting diodes. Moreover, due to the large warpage, the N-type doping is uneven, resulting in a high working voltage of the light emitting diode.

为解决上述问题,本发明提供了一种发光二极管外延片,如图1所示,包括衬底1及依次层叠于所述衬底1上的缓冲层2、本征GaN层3、插入层4、N型GaN层5、多量子阱层6、电子阻挡层7、P型GaN层8;In order to solve the above problems, the present invention provides a light emitting diode epitaxial wafer, as shown in FIG. , N-type GaN layer 5, multiple quantum well layer 6, electron blocking layer 7, P-type GaN layer 8;

所述插入层4包括SixN1-x裂纹层41、Al1-yScyN预处理层42和GaN帽层43,所述SixN1-x裂纹层41、Al1-yScyN预处理层42和GaN帽层43依次层叠于所述本征GaN层3上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer 4 includes a Six N 1-x crack layer 41, an Al 1-y Sc y N pretreatment layer 42 and a GaN cap layer 43, and the Six N 1-x crack layer 41, Al 1-y Sc The y N pretreatment layer 42 and the GaN cap layer 43 are sequentially laminated on the intrinsic GaN layer 3 , wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3.

本发明提供的发光二极管外延片,在本征GaN层3和N型GaN层5中间加入插入层4,在重掺杂的N型GaN半导体生长之前,充分释放了底层应力,增加了外延层平整度,减少了N型重掺生长的应力,增加N型掺杂的均匀性,并且增加了N型掺杂的并入,成功降低了工作电压,增加了外延片表面平整度,增加了发光二极管的抗静电能力。In the light-emitting diode epitaxial wafer provided by the present invention, an insertion layer 4 is added between the intrinsic GaN layer 3 and the N-type GaN layer 5, and before the heavily doped N-type GaN semiconductor grows, the underlying stress is fully released and the flatness of the epitaxial layer is increased. degree, reducing the stress of N-type heavy doping growth, increasing the uniformity of N-type doping, and increasing the incorporation of N-type doping, successfully reducing the operating voltage, increasing the surface flatness of the epitaxial wafer, and increasing the light-emitting diode antistatic ability.

需要说明的是,本发明先在不掺杂的本征GaN层上生长SixN1-x裂纹层,SiN材料在Si掺杂较高,低压较高温生长状态下,平整度高,但是容易出现轻微裂纹,轻微的纳米级的裂纹在发生过程中,是对外延层前期累积应力的释放。然后生长Al1-yScyN预处理层,在Sc掺杂在10-30%时,AlScN材料和GaN材料有着非常好的晶格匹配,可以作为SiN和GaN之间的过渡层所存在,进一步地,采用PVD法生长的AlScN平整度更高,能很好填平SiN材料产生的细微裂纹。如果仅加入SixN1-x裂纹层,则未愈合的裂纹会使得晶格质量变得更差,从而起到反向效果。最后,在Al1-yScyN预处理层后叠加GaN帽层,防止Sc原子进入N型半导体层,影响N型掺杂。在N型层生长之前,底层应力得到了很好的释放,翘曲小,表面平整度较高,有利于N型掺杂的并入和均匀分布。It should be noted that the present invention first grows the Si x N 1-x crack layer on the undoped intrinsic GaN layer. SiN material has high flatness under the condition of high Si doping, low pressure and high temperature growth state, but it is easy to Slight cracks appear, and the slight nano-scale cracks are the release of the accumulated stress in the early stage of the epitaxial layer during the occurrence process. Then grow the Al 1-y Sc y N pretreatment layer. When the Sc doping is 10-30%, the AlScN material and the GaN material have very good lattice matching, and can exist as a transition layer between SiN and GaN. Further, AlScN grown by PVD method has higher flatness, which can well fill up the fine cracks generated by SiN material. If only the Six N 1-x crack layer is added, the unhealed cracks will make the lattice quality worse, which has the opposite effect. Finally, a GaN cap layer is stacked after the Al 1-y Sc y N pretreatment layer to prevent Sc atoms from entering the N-type semiconductor layer and affecting N-type doping. Before the growth of the N-type layer, the underlying stress is well released, the warpage is small, and the surface flatness is high, which is conducive to the incorporation and uniform distribution of N-type doping.

在一种实施方式中,所述插入层的厚度为50nm-70nm;其中,所述SixN1-x裂纹层的厚度为10nm-20nm;所述Al1-yScyN预处理层的厚度为20nm-30nm;所述GaN帽层的厚度为20nm-30nm。优选地,所述插入层的厚度为56nm-64nm;其中,所述SixN1-x裂纹层的厚度为12nm-18nm;所述Al1-yScyN预处理层的厚度为22nm-28nm;所述GaN帽层的厚度为22nm-28nm。In one embodiment, the thickness of the insertion layer is 50nm-70nm; wherein, the thickness of the Six N 1-x crack layer is 10nm-20nm; the Al 1-y Sc y N pretreatment layer The thickness is 20nm-30nm; the thickness of the GaN cap layer is 20nm-30nm. Preferably, the thickness of the insertion layer is 56nm-64nm; wherein, the thickness of the Six N 1-x crack layer is 12nm-18nm; the thickness of the Al 1-y Sc y N pretreatment layer is 22nm- 28nm; the thickness of the GaN cap layer is 22nm-28nm.

具体地,所述发光二极管外延片包括以下层状结构。在一种实施方式中,所述缓冲层为AlGaN缓冲层或AlN缓冲层。所述缓冲层主要用于提供晶种,缓解衬底和外延层的晶格失配,提升外延片晶格质量。在一种实施方式中,所述缓冲层的厚度为10nm-100nm。Specifically, the light emitting diode epitaxial wafer includes the following layered structure. In one embodiment, the buffer layer is an AlGaN buffer layer or an AlN buffer layer. The buffer layer is mainly used to provide crystal seeds, alleviate the lattice mismatch between the substrate and the epitaxial layer, and improve the lattice quality of the epitaxial wafer. In one embodiment, the buffer layer has a thickness of 10 nm-100 nm.

所述本征GaN层为未掺杂的GaN层,在一种实施方式中,所述本征GaN层的厚度为300nm-800nm。The intrinsic GaN layer is an undoped GaN layer, and in one embodiment, the thickness of the intrinsic GaN layer is 300nm-800nm.

所述N型GaN层主要提供电子,在一种实施方式中,所述N型GaN层的厚度为1μm-3μm,所述N型GaN层为Si掺杂,所述Si的掺杂浓度为5×1018-1×1019cm-3;所述P型GaN层主要提供空穴,在一种实施方式中,所述P型GaN层的厚度为10nm-50nm,所述P型GaN层为Mg掺杂,所述Mg的掺杂浓度为5×1017-1×1020cm-3The N-type GaN layer mainly provides electrons. In one embodiment, the thickness of the N-type GaN layer is 1 μm-3 μm, the N-type GaN layer is doped with Si, and the doping concentration of Si is 5 μm. ×10 18 -1×10 19 cm -3 ; the P-type GaN layer mainly provides holes. In one embodiment, the thickness of the P-type GaN layer is 10nm-50nm, and the P-type GaN layer is Mg doping, the Mg doping concentration is 5×10 17 -1×10 20 cm -3 .

所述多量子阱层为发光二极管发光的核心结构。在一种实施方式中,所述多量子阱层包括交替堆叠的InGaN量子阱层和GaN量子垒层,堆叠周期数为3-15;所述InGaN量子阱层的厚度为2nm-4nm;所述GaN量子垒层的厚度为9nm-11nm。The multi-quantum well layer is the core structure of the light-emitting diode. In one embodiment, the multi-quantum well layer includes alternately stacked InGaN quantum well layers and GaN quantum barrier layers, and the number of stacking cycles is 3-15; the thickness of the InGaN quantum well layer is 2nm-4nm; the The thickness of the GaN quantum barrier layer is 9nm-11nm.

所述电子阻挡层主要用来阻挡电子,防止电子溢流,在一种实施方式中,所述电子阻挡层包括交替堆叠的AlGaN层和InGaN层,堆叠周期数为3-15;所述AlGaN层的厚度为5nm-7nm;所述InGaN层的厚度为5nm-7nm。The electron blocking layer is mainly used to block electrons and prevent electron overflow. In one embodiment, the electron blocking layer includes alternately stacked AlGaN layers and InGaN layers, and the number of stacking cycles is 3-15; the AlGaN layer The thickness of the InGaN layer is 5nm-7nm; the thickness of the InGaN layer is 5nm-7nm.

相应地,本发明还提供了上述发光二极管外延片的制备方法,包括以下步骤:Correspondingly, the present invention also provides a method for preparing the above-mentioned light-emitting diode epitaxial wafer, comprising the following steps:

S1、准备衬底;S1. Prepare the substrate;

在一种实施方式中,所述衬底选用蓝宝石衬底。然后,控制反应室温度为1000℃~1200℃,控制反应室压力为200 Torr -600Torr,在H2气氛下对衬底进行5min-8min的高温退火,对衬底表面的颗粒和氧化物进行清洁。In one embodiment, the substrate is a sapphire substrate. Then, control the temperature of the reaction chamber at 1000°C~1200°C, control the pressure of the reaction chamber at 200 Torr-600Torr, and perform high-temperature annealing on the substrate for 5min-8min in H2 atmosphere to clean the particles and oxides on the substrate surface .

S2、在所述衬底上依次沉积缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层和P型GaN层;S2, sequentially depositing a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multiple quantum well layer, an electron blocking layer, and a P-type GaN layer on the substrate;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3.

在一种实施方式中,所述步骤S2包含以下步骤:In one embodiment, the step S2 includes the following steps:

S21、采用下述方法完成在所述衬底的正面沉积所述缓冲层:S21. Depositing the buffer layer on the front side of the substrate by the following method:

在一种实施方式中,所述缓冲层为AlGaN缓冲层或AlN缓冲层。优选地,所述缓冲层为AlN缓冲层,所述AlN缓冲层采用下述方法制得:将反应室温度控制在500℃-700℃,压力为200Torr-400Torr,通入TMAl作为Al源,通入NH3作为N源,完成在所述衬底的正面沉积缓冲层。In one embodiment, the buffer layer is an AlGaN buffer layer or an AlN buffer layer. Preferably, the buffer layer is an AlN buffer layer, and the AlN buffer layer is prepared by the following method: the temperature of the reaction chamber is controlled at 500°C-700°C, the pressure is 200Torr-400Torr, and TMAl is introduced as the Al source. Inject NH 3 as the N source to complete the deposition of the buffer layer on the front side of the substrate.

S22、采用下述方法完成在所述缓冲层上沉积所述本征GaN层:S22. Depositing the intrinsic GaN layer on the buffer layer by using the following method:

将反应室温度控制在1100℃-1150℃,压力为100Torr-500Torr,通入NH3作为N源,通入TMGa作为Ga源,完成在所述缓冲层上沉积所述本征GaN层。The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 100Torr-500Torr, NH 3 is fed in as the N source, and TMGa is fed in as the Ga source to complete the deposition of the intrinsic GaN layer on the buffer layer.

S23、采用下述方法完成所述SixN1-x裂纹层的沉积:S23. The deposition of the Six N 1-x crack layer is completed by the following method:

将反应室温度控制在1100℃-1150℃,压力为50Torr-100Torr,通入H2/N2做载气,通入NH3做N源,通入SiH4作为Si源,完成沉积。The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 50Torr-100Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and SiH 4 is fed as Si source to complete the deposition.

需要说明的是,本发明先在所述本征GaN层上生长SixN1-x裂纹层,在上述方法中,优选地,压力为60Torr-80Torr,反应室温度控制在1140℃-1150℃,x的取值范围为0.2-0.4。SiN材料在Si掺杂较高,低压较高温生长状态下,平整度高,但会出现轻微裂纹,轻微的纳米级的裂纹的产生过程也是对外延层前期累积应力的释放。SixN1-x裂纹层的设置有利于在重掺杂的N型GaN半导体生长之前,充分释放了底层应力,增加了外延层平整度,减少N型重掺生长的应力,增加N型掺杂的均匀性。It should be noted that in the present invention, a Six N 1-x crack layer is first grown on the intrinsic GaN layer. In the above method, preferably, the pressure is 60 Torr-80 Torr, and the temperature of the reaction chamber is controlled at 1140°C-1150°C , the value range of x is 0.2-0.4. The SiN material has high flatness under the condition of high Si doping, low pressure and high temperature growth, but slight cracks will appear. The process of slight nanoscale cracks is also the release of the accumulated stress in the early stage of the epitaxial layer. The setting of the Six N 1-x crack layer is conducive to fully releasing the underlying stress before the growth of the heavily doped N-type GaN semiconductor, increasing the flatness of the epitaxial layer, reducing the stress of N-type heavily doped growth, and increasing the N-type doped growth. Mixed uniformity.

但是如果仅加入SixN1-x裂纹层,则未愈合的裂纹会使得晶格质量变得更差,从而起到反向效果。针对这一问题,本申请引入了Al1-yScyN预处理层。However, if only the Six N 1-x crack layer is added, the unhealed cracks will make the lattice quality worse, thus playing the opposite effect. To solve this problem, the present application introduces an Al 1-y Sc y N pretreatment layer.

S24、采用下述方法完成所述Al1-yScyN预处理层的沉积:S24. Complete the deposition of the Al 1-y Sc y N pretreatment layer by the following method:

将反应室温度控制在200℃-1000℃,压力为5mTorr-10mTorr,通入Ar做载气,通入N2做反应气,以ScAl合金靶材为溅射靶材,完成沉积。The temperature of the reaction chamber is controlled at 200°C-1000°C, the pressure is 5mTorr-10mTorr, Ar is passed in as the carrier gas, N 2 is passed in as the reaction gas, and the ScAl alloy target is used as the sputtering target to complete the deposition.

优选地,将外延片转移至PVD,即磁控溅射设备中完成Al1-yScyN预处理层的沉积。所述Al1-yScyN预处理层中Sc掺杂在10-30%时,AlScN材料和GaN材料有着非常好的晶格匹配,可以作为SiN和GaN之间的过渡层所存在,进一步地,采用PVD法生长的AlScN平整度更高,能很好填平SiN材料产生的细微裂纹。Preferably, the epitaxial wafer is transferred to PVD, that is, the deposition of the Al 1-y Sc y N pretreatment layer is completed in a magnetron sputtering device. When the Sc doping in the Al 1-y Sc y N pretreatment layer is 10-30%, the AlScN material and the GaN material have very good lattice matching, and can exist as a transition layer between SiN and GaN, further Therefore, AlScN grown by PVD method has higher flatness, which can well fill up the fine cracks produced by SiN materials.

S25、采用下述方法完成所述GaN帽层的沉积:S25, using the following method to complete the deposition of the GaN cap layer:

将反应室温度控制在900℃-1000℃,压力为100Torr-300Torr,通入H2/N2做载气,通入NH3做N源,通入TMGa作为Ga源,完成沉积。The temperature of the reaction chamber is controlled at 900°C-1000°C, the pressure is 100Torr-300Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and TMGa is fed as Ga source to complete the deposition.

优选地,将外延片转移回MOCVD设备中完成GaN帽层的沉积。Preferably, the epitaxial wafer is transferred back to the MOCVD equipment to complete the deposition of the GaN cap layer.

在Al1-yScyN预处理层后叠加GaN帽层,能够防止Sc原子进入N型半导体层影响N型掺杂。这样,在N型层生长之前,底层应力得到了很好的释放,翘曲小,表面平整度较高,有利于N型掺杂的并入和均匀分布。The GaN cap layer is stacked after the Al 1-y Sc y N pretreatment layer, which can prevent Sc atoms from entering the N-type semiconductor layer and affecting the N-type doping. In this way, before the growth of the N-type layer, the stress of the bottom layer is well released, the warpage is small, and the surface flatness is high, which is conducive to the incorporation and uniform distribution of N-type doping.

S26、采用下述方法完成在所述插入层上沉积所述N型GaN层:S26. Depositing the N-type GaN layer on the insertion layer by using the following method:

将反应室温度控制在1100℃-1150℃,压力为100Torr-500Torr,通入SiH4作为Si源,通入NH3作为N源,通入TMGa作为Ga源,完成在所述插入层上沉积所述N型GaN层;The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 100Torr-500Torr, SiH 4 is introduced as the Si source, NH 3 is introduced as the N source, and TMGa is introduced as the Ga source to complete the deposition on the insertion layer. The N-type GaN layer;

S27、采用下述方法完成在所述N型GaN层上沉积所述多量子阱层:S27. Depositing the multiple quantum well layer on the N-type GaN layer by using the following method:

在所述N型GaN层上交替沉积InGaN量子阱层和GaN量子垒层,堆叠层数在3~15;Alternately depositing InGaN quantum well layers and GaN quantum barrier layers on the N-type GaN layer, the number of stacked layers is 3-15;

其中,所述InGaN量子阱层的沉积步骤包括:Wherein, the deposition step of the InGaN quantum well layer comprises:

将反应室温度控制在700℃-800℃,压力为100Torr-500Torr,通入TMIn作为In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积;Control the temperature of the reaction chamber at 700°C-800°C, the pressure at 100Torr-500Torr, feed TMIn as the In source, NH3 as the N source, and TMGa as the Ga source to complete the deposition;

所述GaN量子垒层的沉积步骤包括:The deposition steps of the GaN quantum barrier layer include:

将反应室温度控制在800℃-900℃,压力为100Torr-500Torr,通入NH3作为N源,通入TMGa作为Ga源,完成沉积。The temperature of the reaction chamber is controlled at 800°C-900°C, the pressure is 100Torr-500Torr, NH 3 is fed in as the N source, and TMGa is fed in as the Ga source to complete the deposition.

S28、采用下述方法完成在所述多量子阱层上沉积所述电子阻挡层:S28. Depositing the electron blocking layer on the multiple quantum well layer by using the following method:

在所述多量子阱层上交替沉积AlGaN层和InGaN层,堆叠层数在3~15;AlGaN layers and InGaN layers are alternately deposited on the multi-quantum well layer, and the number of stacked layers is 3 to 15;

其中,所述AlGaN层的沉积步骤包括:Wherein, the deposition step of the AlGaN layer includes:

将反应室温度控制在900℃-1000℃,压力为100Torr-500Torr,通入TMAl作为Al源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积;The temperature of the reaction chamber is controlled at 900°C-1000°C, the pressure is 100Torr-500Torr, and the deposition is completed by feeding TMAl as the Al source, NH3 as the N source, and TMGa as the Ga source;

所述InGaN层的沉积步骤包括:The deposition steps of the InGaN layer include:

将反应室温度控制在900℃-1000℃,压力为100Torr-500Torr,通入TMIn作为In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积。Control the temperature of the reaction chamber at 900°C-1000°C, the pressure at 100Torr-500Torr, feed TMIn as the In source, NH3 as the N source, and TMGa as the Ga source to complete the deposition.

S29、采用下述方法完成在所述电子阻挡层上沉积所述P型GaN层:S29. Depositing the P-type GaN layer on the electron blocking layer by the following method:

将反应室温度控制在800℃-1000℃,压力为100Torr-300Torr,通入NH3作为N源,通入TMGa作为Ga源,通入CP2Mg作为Mg源,完成在所述电子阻挡层上沉积所述P型GaN层。The temperature of the reaction chamber is controlled at 800°C-1000°C, the pressure is 100Torr-300Torr, and NH 3 is introduced as the N source, TMGa as the Ga source, and CP 2 Mg as the Mg source, and completed on the electron blocking layer. The P-type GaN layer is deposited.

相应地,本发明还提供了一种发光二极管,所述发光二极管包括所述的发光二极管外延片。Correspondingly, the present invention also provides a light emitting diode, which includes the light emitting diode epitaxial wafer.

以上采用MOCVD设备或PVD设备完成沉积过程,本发明对沉积方法不作限定。并且,以上Al源、N源、Ga源、Si源、Mg源、Sc源、In源为示范性说明,不限于上述列举。Above, MOCVD equipment or PVD equipment is used to complete the deposition process, and the present invention does not limit the deposition method. Moreover, the above Al source, N source, Ga source, Si source, Mg source, Sc source, and In source are exemplary descriptions, and are not limited to the above-mentioned enumerations.

下面以具体实施例进一步说明本发明:Further illustrate the present invention with specific embodiment below:

实施例1Example 1

本实施例提供一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;This embodiment provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P layer sequentially stacked on the substrate. type GaN layer;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x为0.3;y为0.2。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein x is 0.3; y is 0.2.

上述发光二极管外延片的制备方法,包括以下步骤:The method for preparing the above-mentioned light-emitting diode epitaxial wafer includes the following steps:

S1、准备衬底;所述衬底选用蓝宝石衬底。S1. Prepare a substrate; the substrate is a sapphire substrate.

S2、在所述衬底上依次沉积缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;S2, sequentially depositing a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multiple quantum well layer, an electron blocking layer, and a P-type GaN layer on the substrate;

具体地,S2包括以下步骤:Specifically, S2 includes the following steps:

S21、采用下述方法完成在所述衬底的正面沉积所述缓冲层:S21. Depositing the buffer layer on the front side of the substrate by the following method:

将反应室温度控制在600℃,通入TMAl作为Al源,通入NH3作为N源,在所述衬底的正面沉积缓冲层,完成沉积并控制所沉积的所述缓冲层的厚度为30nm。Control the temperature of the reaction chamber at 600°C, feed TMAl as the Al source, feed NH3 as the N source, deposit a buffer layer on the front side of the substrate, complete the deposition and control the thickness of the deposited buffer layer to be 30nm .

S22、采用下述方法完成在所述缓冲层上沉积所述本征GaN层:S22. Depositing the intrinsic GaN layer on the buffer layer by using the following method:

将反应室温度控制在1150℃,通入NH3作为N源,通入TMGa作为Ga源,完成沉积并控制沉积厚度为400nm;Control the temperature of the reaction chamber at 1150°C, feed NH 3 as the N source, and feed TMGa as the Ga source, complete the deposition and control the deposition thickness to 400nm;

S23、采用下述方法完成所述SixN1-x裂纹层的沉积:S23. The deposition of the Six N 1-x crack layer is completed by the following method:

将反应室温度控制在1050℃,压力为70Torr,通入H2/N2做载气,通入NH3做N源,通入SiH4作为Si源,完成沉积并控制所沉积的所述SixN1-x裂纹层的厚度为15nm。The temperature of the reaction chamber is controlled at 1050°C, the pressure is 70 Torr, H 2 /N 2 is introduced as the carrier gas, NH 3 is introduced as the N source, and SiH 4 is introduced as the Si source to complete the deposition and control the deposited Si The thickness of the x N 1-x crack layer is 15 nm.

S24、采用下述方法完成所述Al1-yScyN预处理层的沉积:S24. Complete the deposition of the Al 1-y Sc y N pretreatment layer by the following method:

在PVD设备中将反应室温度控制在600℃,压力为7mTorr,通入Ar做载气,通入N2做反应气,以ScAl合金靶材为溅射靶材,完成沉积并控制所沉积的所述Al1-yScyN预处理层的厚度为25nm。In the PVD equipment, the temperature of the reaction chamber is controlled at 600 ° C, the pressure is 7 mTorr, Ar is introduced as the carrier gas, N 2 is introduced as the reaction gas, and the ScAl alloy target is used as the sputtering target to complete the deposition and control the deposition. The thickness of the Al 1-y Sc y N pretreatment layer is 25nm.

S25、采用下述方法完成所述GaN帽层的沉积:S25, using the following method to complete the deposition of the GaN cap layer:

将反应室温度控制在950℃,压力为200Torr,通入H2/N2做载气,通入NH3做N源,通入TMGa作为Ga源,完成沉积并控制所沉积的所述GaN帽层的厚度为25nm。The temperature of the reaction chamber is controlled at 950°C, the pressure is 200 Torr, H 2 /N 2 is introduced as the carrier gas, NH 3 is introduced as the N source, and TMGa is introduced as the Ga source to complete the deposition and control the deposited GaN cap The thickness of the layer is 25 nm.

S26、采用下述方法完成在所述插入层上沉积所述N型GaN层:S26. Depositing the N-type GaN layer on the insertion layer by using the following method:

将反应室温度控制在1050℃,通入SiH4作为Si源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积并控制沉积厚度为2μm,Si掺杂浓度为1*1019cm-3Control the temperature of the reaction chamber at 1050°C, feed SiH 4 as the Si source, NH 3 as the N source, and TMGa as the Ga source, complete the deposition and control the deposition thickness to 2 μm, and the Si doping concentration to 1*10 19 cm -3 ;

S24、采用下述方法完成在所述N型GaN层上沉积所述多量子阱层:S24. Depositing the multiple quantum well layer on the N-type GaN layer by using the following method:

在所述N型GaN层上交替沉积InGaN量子阱层和GaN量子垒层,堆叠层数在10;Alternately depositing InGaN quantum well layers and GaN quantum barrier layers on the N-type GaN layer, the number of stacked layers is 10;

其中,所述InGaN量子阱层的沉积步骤包括:Wherein, the deposition step of the InGaN quantum well layer comprises:

将反应室温度控制在800℃,通入In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积并控制沉积厚度为3nm;Control the temperature of the reaction chamber at 800°C, feed In source, feed NH 3 as N source, feed TMGa as Ga source, complete the deposition and control the deposition thickness to 3nm;

所述GaN量子垒层的沉积步骤包括:The deposition steps of the GaN quantum barrier layer include:

将反应室温度控制在800℃,通入NH3作为N源,通入TMGa作为Ga源,完成沉积并控制沉积厚度为10nm。Control the temperature of the reaction chamber at 800°C, feed NH 3 as the N source, and feed TMGa as the Ga source, complete the deposition and control the deposition thickness to 10nm.

S28、采用下述方法完成在所述多量子阱层上沉积所述电子阻挡层:S28. Depositing the electron blocking layer on the multiple quantum well layer by using the following method:

在所述多量子阱层上交替沉积AlGaN层和InGaN层,堆叠层数在8;AlGaN layers and InGaN layers are alternately deposited on the multi-quantum well layer, and the number of stacked layers is 8;

其中,所述AlGaN层的沉积步骤包括:Wherein, the deposition step of the AlGaN layer includes:

将反应室温度控制在950℃,压力为300Torr,通入TMAl作为Al源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积控制沉积厚度为6nm;Control the temperature of the reaction chamber at 950°C and the pressure at 300 Torr, feed TMAl as the Al source, feed NH 3 as the N source, feed TMGa as the Ga source, complete the deposition and control the deposition thickness to 6nm;

所述InGaN层的沉积步骤包括:The deposition steps of the InGaN layer include:

将反应室温度控制在950℃,压力为300Torr,通入TMIn作为In源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积控制沉积厚度为6nm。The temperature of the reaction chamber is controlled at 950°C, the pressure is 300 Torr, TMIn is introduced as the In source, NH 3 is introduced as the N source, and TMGa is introduced as the Ga source, and the deposition thickness is controlled to be 6nm.

S29、采用下述方法完成在所述电子阻挡层上沉积所述P型GaN层:S29. Depositing the P-type GaN layer on the electron blocking layer by the following method:

将反应室温度控制在850℃,通入Mg源作为掺杂源,通入NH3作为N源,通入TMGa作为Ga源,完成沉积并控制沉积厚度为4nm,Mg掺杂浓度为5*1019cm-3Control the temperature of the reaction chamber at 850°C, feed Mg source as the dopant source, feed NH 3 as the N source, feed TMGa as the Ga source, complete the deposition and control the deposition thickness to 4nm, and the Mg doping concentration to 5*10 19 cm -3 .

实施例2Example 2

本实施例提供一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;This embodiment provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P layer sequentially stacked on the substrate. type GaN layer;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x为0.4;y为0.1。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein x is 0.4; y is 0.1.

上述发光二极管外延片的制备方法,参照实施例1。For the preparation method of the above-mentioned light-emitting diode epitaxial wafer, refer to Example 1.

实施例3Example 3

本实施例提供一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;This embodiment provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P layer sequentially stacked on the substrate. Type GaN layer;

所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x为0.1;y为0.3。The insertion layer includes a Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, the Six N 1-x crack layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein x is 0.1; y is 0.3.

上述发光二极管外延片的制备方法,参照实施例1。For the preparation method of the above-mentioned light-emitting diode epitaxial wafer, refer to Example 1.

对比例1Comparative example 1

本对比例提供一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、SixN1-x裂纹层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层,其中,x为0.3;y为0.2。This comparative example provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, a Si x N 1-x crack layer, an N-type GaN layer, and a multi-quantum well layer sequentially stacked on the substrate. , an electron blocking layer, and a P-type GaN layer, wherein x is 0.3; y is 0.2.

上述发光二极管外延片的制备方法,参照实施例1。For the preparation method of the above-mentioned light-emitting diode epitaxial wafer, refer to Example 1.

对比例2Comparative example 2

本对比例提供一种发光二极管外延片,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层。This comparative example provides a light-emitting diode epitaxial wafer, including a substrate and a buffer layer, an intrinsic GaN layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P-type GaN layer sequentially stacked on the substrate. .

上述发光二极管外延片的制备方法,参照实施例1。For the preparation method of the above-mentioned light-emitting diode epitaxial wafer, refer to Example 1.

以实施例1-3和对比例1-2制得发光二极管外延片制作芯片进行性能测试,测试结果如表1所示。The light-emitting diode epitaxial wafers prepared in Examples 1-3 and Comparative Examples 1-2 were used to make chips for performance testing, and the test results are shown in Table 1.

表1为实施例1-3和对比例1-2制得发光二极管外延片性能测试结果Table 1 shows the performance test results of light-emitting diode epitaxial wafers prepared in Examples 1-3 and Comparative Examples 1-2

Figure 554786DEST_PATH_IMAGE001
Figure 554786DEST_PATH_IMAGE001

由上述结果可知,本发明提出的发光二极管外延片具有特定的插入层结构,使得外延片平整度更高,工作电压更低,也具有更好的抗静电能力。如果仅加入SiN裂纹层,则未愈合的裂纹会使得晶格质量变得更差,从而起到反向效果。From the above results, it can be known that the light-emitting diode epitaxial wafer proposed by the present invention has a specific insertion layer structure, which makes the epitaxial wafer have higher flatness, lower working voltage, and better antistatic ability. If only the SiN crack layer is added, the unhealed cracks will make the lattice quality worse, which has the opposite effect.

以上所述是发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也视为本发明的保护范围。The above is the preferred embodiment of the invention, it should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications are also considered as protection scope of the present invention.

Claims (10)

1.一种发光二极管外延片,其特征在于,包括衬底及依次层叠于所述衬底上的缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层、P型GaN层;1. A light-emitting diode epitaxial wafer, characterized in that, comprises a substrate and a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, and an electron blocking layer stacked sequentially on the substrate , P-type GaN layer; 所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1- yScyN预处理层和GaN帽层由下至上依次层叠于所述本征GaN层上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer includes a Six N 1-x cracked layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, and the Six N 1-x cracked layer, an Al 1- y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer from bottom to top, wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3. 2.如权利要求1所述的发光二极管外延片,其特征在于,所述插入层的厚度为50nm-70nm;2. The light-emitting diode epitaxial wafer according to claim 1, wherein the thickness of the insertion layer is 50nm-70nm; 其中,所述SixN1-x裂纹层的厚度为10nm-20nm;Wherein, the thickness of the Six N 1-x crack layer is 10nm-20nm; 所述Al1-yScyN预处理层的厚度为20nm-30nm;The thickness of the Al 1-y Sc y N pretreatment layer is 20nm-30nm; 所述GaN帽层的厚度为20nm-30nm。The thickness of the GaN cap layer is 20nm-30nm. 3.如权利要求1所述的发光二极管外延片,其特征在于,所述缓冲层的厚度为10nm-100nm;3. The light-emitting diode epitaxial wafer according to claim 1, wherein the thickness of the buffer layer is 10nm-100nm; 所述本征GaN层的厚度为300nm-800nm;The thickness of the intrinsic GaN layer is 300nm-800nm; 所述N型GaN层的厚度为1μm-3μm,所述N型GaN层为Si掺杂,所述Si的掺杂浓度为5×1018-1×1019cm-3The thickness of the N-type GaN layer is 1 μm-3 μm, the N-type GaN layer is doped with Si, and the doping concentration of Si is 5×10 18 -1×10 19 cm -3 ; 所述P型GaN层的厚度为10nm-50nm,所述P型GaN层为Mg掺杂,所述Mg的掺杂浓度为5×1017-1×1020cm-3The thickness of the P-type GaN layer is 10nm-50nm, the P-type GaN layer is doped with Mg, and the doping concentration of Mg is 5×10 17 -1×10 20 cm -3 . 4.如权利要求1所述的发光二极管外延片,其特征在于,所述多量子阱层包括交替堆叠的InGaN量子阱层和GaN量子垒层,堆叠周期数为3-15;4. The light-emitting diode epitaxial wafer according to claim 1, wherein the multi-quantum well layer comprises alternately stacked InGaN quantum well layers and GaN quantum barrier layers, and the number of stacking cycles is 3-15; 所述InGaN量子阱层的厚度为2nm-4nm;The thickness of the InGaN quantum well layer is 2nm-4nm; 所述GaN量子垒层的厚度为9nm-11nm。The thickness of the GaN quantum barrier layer is 9nm-11nm. 5.如权利要求1所述的发光二极管外延片,其特征在于,所述电子阻挡层包括交替堆叠的AlGaN层和InGaN层,堆叠周期数为3-15;5. The light-emitting diode epitaxial wafer according to claim 1, wherein the electron blocking layer comprises alternately stacked AlGaN layers and InGaN layers, and the number of stacking cycles is 3-15; 所述AlGaN层的厚度为5nm-7nm;The thickness of the AlGaN layer is 5nm-7nm; 所述InGaN层的厚度为5nm-7nm。The thickness of the InGaN layer is 5nm-7nm. 6.一种如权利要求1~5任一项所述的发光二极管外延片的制备方法,其特征在于,包括以下步骤:6. A method for preparing a light-emitting diode epitaxial wafer according to any one of claims 1 to 5, comprising the following steps: 准备衬底;Prepare the substrate; 在所述衬底上依次沉积缓冲层、本征GaN层、插入层、N型GaN层、多量子阱层、电子阻挡层和P型GaN层;sequentially depositing a buffer layer, an intrinsic GaN layer, an insertion layer, an N-type GaN layer, a multi-quantum well layer, an electron blocking layer, and a P-type GaN layer on the substrate; 所述插入层包括SixN1-x裂纹层、Al1-yScyN预处理层和GaN帽层,所述SixN1-x裂纹层、Al1- yScyN预处理层和GaN帽层依次层叠于所述本征GaN层上,其中,x的取值范围为0.1-0.4;y的取值范围为0.1-0.3。The insertion layer includes a Six N 1-x cracked layer, an Al 1-y Sc y N pretreatment layer and a GaN cap layer, and the Six N 1-x cracked layer, an Al 1- y Sc y N pretreatment layer and a GaN cap layer are sequentially stacked on the intrinsic GaN layer, wherein the value range of x is 0.1-0.4; the value range of y is 0.1-0.3. 7.如权利要求6所述的发光二极管外延片的制备方法,其特征在于,采用下述方法完成所述SixN1-x裂纹层的沉积:7. The preparation method of light-emitting diode epitaxial wafer as claimed in claim 6, is characterized in that, adopts following method to finish the deposition of described Six N 1-x crack layer: 将反应室温度控制在1100℃-1150℃,压力为50Torr-100Torr,通入H2/N2做载气,通入NH3做N源,通入SiH4作为Si源,完成沉积。The temperature of the reaction chamber is controlled at 1100°C-1150°C, the pressure is 50Torr-100Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and SiH 4 is fed as Si source to complete the deposition. 8.如权利要求6所述的发光二极管外延片的制备方法,其特征在于,采用下述方法完成所述Al1-yScyN预处理层的沉积:8. The preparation method of light-emitting diode epitaxial wafer as claimed in claim 6, is characterized in that, adopts following method to finish the deposition of described Al 1-y Sc y N pretreatment layer: 将反应室温度控制在200℃-1000℃,压力为5mTorr-10mTorr,通入Ar做载气,通入N2做反应气,以ScAl合金靶材为溅射靶材,完成沉积。The temperature of the reaction chamber is controlled at 200°C-1000°C, the pressure is 5mTorr-10mTorr, Ar is passed in as the carrier gas, N 2 is passed in as the reaction gas, and the ScAl alloy target is used as the sputtering target to complete the deposition. 9.如权利要求6所述的发光二极管外延片的制备方法,其特征在于,采用下述方法完成所述GaN帽层的沉积:9. The preparation method of light-emitting diode epitaxial wafer as claimed in claim 6, is characterized in that, adopts following method to finish the deposition of described GaN cap layer: 将反应室温度控制在900℃-1000℃,压力为100Torr-300Torr,通入H2/N2做载气,通入NH3做N源,通入TMGa作为Ga源,完成沉积。The temperature of the reaction chamber is controlled at 900°C-1000°C, the pressure is 100Torr-300Torr, and H 2 /N 2 is fed as carrier gas, NH 3 is fed as N source, and TMGa is fed as Ga source to complete the deposition. 10.一种发光二极管,其特征在于,所述发光二极管包括如权利要求1-5中任一所述的发光二极管外延片。10. A light emitting diode, characterized in that the light emitting diode comprises the light emitting diode epitaxial wafer according to any one of claims 1-5.
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