WO2020228336A1 - 一种基于GaN的LED外延片及其制备方法 - Google Patents

一种基于GaN的LED外延片及其制备方法 Download PDF

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WO2020228336A1
WO2020228336A1 PCT/CN2019/128054 CN2019128054W WO2020228336A1 WO 2020228336 A1 WO2020228336 A1 WO 2020228336A1 CN 2019128054 W CN2019128054 W CN 2019128054W WO 2020228336 A1 WO2020228336 A1 WO 2020228336A1
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epitaxial wafer
substrate
led epitaxial
based led
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高海
刘正伟
尹祥麟
张泽众
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夕心科技（上海）有限公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
    • 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
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
    • 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
    • H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
    • 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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  • the invention relates to an LED epitaxial wafer and a preparation method thereof, in particular to a GaN-based LED epitaxial wafer and a preparation method thereof.
  • LEDs Light-emitting diodes
  • the most ideal material for manufacturing blue/white LED chips is GaN and its related group III nitrides with excellent photoelectric properties.
  • the GaN-based LED chips epitaxially on the sapphire substrate are very mature, most of these chips are constructed based on polar planes, which will form a strong internal electric field (in the order of MV/cm) at the quantum well. It is easy to form electric dipoles and generate spontaneous polarization fields and piezoelectric polarization fields, which in turn causes the Quantum-confined Starker Effect (QCSE), and ultimately reduces the luminous efficiency of the LED.
  • QCSE Quantum-confined Starker Effect
  • the non-polar GaN epitaxial film has been proven to avoid or reduce the influence of the spontaneous polarization effect of the film itself, and greatly improve the luminous efficiency of the chip. It is the most effective method recognized internationally. Compared with the traditional polar surface film, it is more suitable for LED light-emitting devices.
  • the use of non-polar surface GaN-based materials to prepare LEDs can theoretically nearly double the luminous efficiency of LEDs; secondly, non-polar surface LEDs will not produce blue shift of the emission wavelength; finally, non-polar InGaN/GaN
  • the quantum well has polarization characteristics and improves the uniformity of light, achieving the effects of energy saving and improving color tone.
  • the epitaxy of the non-polar surface film is largely related to the choice of substrate material. Therefore, if the LED industry wants to obtain the core technology of epitaxial growth and improve the luminous efficiency of LEDs, it is necessary to find a new substrate to replace sapphire and realize the growth of non-polar GaN epitaxial materials.
  • LaAlO 3 crystal is a more suitable substrate material for growing non-polar GaN and its LED devices.
  • the LaAlO3 crystal at room temperature has a pseudo-cubic structure, which is very close to the ideal perovskite structure. Therefore, LaAlO3 single crystal has a good lattice matching to a variety of perovskite structure materials, and is an excellent substrate material for epitaxial growth of high-temperature superconducting films and giant magnetoresistive films. Its dielectric properties are suitable for low-loss microwave and dielectric resonance. Applications.
  • LaAlO 3 has been used as a substrate material for high-temperature superconducting films and giant magnetoresistive films for a long time.
  • the preparation technology is mature and the output is large. It is easy to obtain the substrate corresponding to the required crystal plane.
  • the technical problem to be solved by the present invention is to provide a GaN-based LED epitaxial wafer and a preparation method thereof, which can greatly shorten the crack length, reduce the defect density, and easily obtain a crack-free high-quality GaN film.
  • the technical solution adopted by the present invention to solve the above technical problems is to provide a GaN-based LED epitaxial wafer, including a substrate, wherein a GaN nanopillar insertion layer and an n-GaN layer are sequentially formed on the substrate.
  • the present invention also provides a method for preparing a GaN-based LED epitaxial wafer, which includes the following steps: S1) Using a plasma-enhanced metal organic chemical vapor deposition process to grow a GaN nano-pillar array insertion layer on a substrate ; S2) Using a plasma enhanced metal organic chemical vapor deposition process to grow an n-GaN layer on the GaN insertion layer.
  • the temperature of the reaction chamber is controlled to be 800° C.
  • the pressure of the reaction chamber is 200 Torr
  • 200 sccm ammonia gas, 100 sccm nitrogen gas and 380 sccm trimethyl gallium are introduced.
  • the temperature of the reaction chamber is controlled to be 1000° C.
  • the pressure of the reaction chamber is 200 Torr
  • 60 sccm of silane, 200 sccm of ammonia, 100 sccm of nitrogen, and 380 sccm of trimethylgallium are introduced.
  • the present invention has the following beneficial effects: the GaN insertion layer of the present invention adopts a nano-pillar array structure. Compared with a thin-film buffer layer, the contact area between the nano-pillar array buffer layer and the substrate is small, and the stress is easily released. The crack length is greatly shortened; the nano-pillar material has the defect self-elimination effect, which can greatly reduce the defect density. Optimizing the new LaAlO 3 substrate can greatly reduce the adverse effect of the Quantum-confined Starker Effect (QCSE) on the subsequent growth, and it is easier to obtain a crack-free high-quality GaN film in the subsequent growth.
  • QCSE Quantum-confined Starker Effect
  • FIG. 1 is a schematic diagram of the structure of a GaN-based LED epitaxial wafer in an embodiment of the present invention.
  • FIG. 2 is a top view of an insertion layer of a GaN nanopillar array in an embodiment of the present invention.
  • Fig. 3 is an x-ray diffraction pattern of GaN (0002) using a GaN nanopillar array insertion layer according to the present invention.
  • Fig. 4 is an x-ray diffraction pattern of GaN (0002) using a GaN thin film insertion layer according to the present invention.
  • Fig. 5 is an X-ray diffraction pattern of GaN (1012) using a GaN nanopillar array insertion layer according to the present invention.
  • Fig. 6 is an X-ray diffraction pattern of GaN (1012) using a GaN thin film insertion layer in the present invention.
  • FIG. 1 is a schematic diagram of the structure of a GaN-based LED epitaxial wafer in an embodiment of the present invention.
  • the GaN-based LED epitaxial wafer provided by the present invention includes a substrate 1 on which a GaN nanopillar array insertion layer 2 and an n-GaN layer 3 are sequentially formed.
  • the GaN insertion layer of the present invention adopts a nano-pillar array structure, and the contact area between the nano-pillar array buffer layer and the substrate is small compared to the thin-film buffer layer. If the contact area between the film and the substrate is 1, the maximum contact area between the nanopillar array and the substrate is 0.785, which is the area of the inscribed circle of a square with a side length of 1, so that the stress is easily released and can be greatly shortened Crack length.
  • the substrate includes sapphire, Si, SiC, GaN, ZnO, LiGaO 2 , LaSrAlTaO 6 , Al or Cu.
  • the thickness of the GaN nanopillar array in the present invention is 500-1500 nm.
  • the thickness of the n-GaN layer is 1500-3000 nm. If the thickness of the n-GaN layer is too low, it will increase the difficulty of subsequent LED chip processing. For example, thinning is required, and the etching process is more precise, which leads to a decrease in the chip yield; too thick n-GaN layer will cause n-GaN The internal stress in the medium increases, the crack of the epitaxial wafer deteriorates, and at the same time, it also extends the growth time and increases the production cost.
  • the Si doping concentration is 1 ⁇ 10 17 to 1 ⁇ 10 19 cm -3 . If the Si doping concentration is too low, the effective carriers available in n-GaN are insufficient, which will greatly reduce the electrical performance of the LED chip, such as a significant decrease in brightness; if the Si doping concentration is too high, defects in n-GaN will increase. The quality of the crystal will drop off the cliff, leading to a drop in the quality of the epitaxial wafer, and at the same time it will also reduce the electrical performance of the LED chip, such as increased leakage.
  • the preparation method of the GaN-based LED epitaxial wafer provided by the present invention includes:
  • GaN nanopillar array insertion layer growth step using a plasma-enhanced metal organic chemical vapor deposition process to grow a GaN nanopillar insertion layer on LaAlO 3 ;
  • the growth step of the n-GaN layer the n-GaN layer is grown on the GaN nano-insertion layer by using a plasma enhanced metal organic chemical vapor deposition process.
  • step S1) the specific process conditions are as follows:
  • the process conditions of the GaN insertion layer are: the temperature of the reaction chamber is 800°C, the pressure of the reaction chamber is 200 Torr, and 200sccm ammonia gas, 100sccm nitrogen gas and 380sccm trimethylgallium are introduced;
  • step S2) the specific process conditions are as follows:
  • the process conditions of the n-GaN layer are: the temperature of the reaction chamber is 1000°C, the pressure of the reaction chamber is 200 Torr, 60 sccm of silane, 200 sccm of ammonia, 100 sccm of nitrogen, and 380 sccm of trimethylgallium are introduced;
  • the LED epitaxial wafer structure of the present invention increases the crystal quality and electrical properties of the GaN epitaxial film by adding a GaN nanoarray insertion layer, which includes a LaAlO 3 substrate 1, a GaN nanoarray insertion layer with a thickness of 500 nm 2, a thickness of 1.5 ⁇ m, The n-GaN layer 3 with a Si doping concentration of 1 ⁇ 10 18 cm -3 .
  • XRD the abbreviation of X-ray diffraction
  • X-ray diffraction is a research method of X-ray diffraction, which analyzes the diffraction pattern of a material by X-ray diffraction to obtain information such as the composition of the material, the structure or morphology of the internal atoms or molecules of the material.
  • the comparative example uses substrate + GaN film + n-GaN layer, where the thickness of the GaN film is the same as the thickness of the GaN nanopillar insertion layer , Here are 500nm.
  • the crystal quality of the GaN film has been significantly improved: GaN (0002) increased by 200 arcsec, and GaN (1012) increased by 321 arcsec. , which shows that it is easier to obtain high-quality GaN thin film by using GaN nanoarray as the insertion layer.

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Abstract

本发明公开了一种基于GaN的LED外延片及其制备方法，所述LED外延片包括衬底，其中，所述衬底上依次形成有GaN纳米柱插入层和n-GaN层。本发明提供的基于GaN的LED外延片及其制备方法， GaN插入层采用纳米柱阵列结构，相对于薄膜型缓冲层，纳米柱阵列缓冲层与衬底的接触面积小，应力容易得到释放，可大大缩短裂纹长度；纳米柱材料有缺陷自排除效应，可大大降低缺陷密度，更易在后续生长中获得无裂纹高质量的GaN薄膜。

Description

一种基于GaN的LED外延片及其制备方法 技术领域
本发明涉及一种LED外延片及其制备方法，尤其涉及一种基于GaN的LED外延片及其制备方法。
背景技术
发光二极管(light-emitting diode，LED)因具有高效、节能环保、长寿命、体积小等优点，有望代替传统的白炽灯、荧光灯及气体放电灯成为新一代的照明光源，引起了产业及科研领域的广泛关注。自1962年第一只LED诞生至今，LED的各方面性能都得到了极大的提升，应用领域也越来越广。
发明概述
技术问题
目前，用于制造蓝/白光LED芯片最理想材料是具有优异光电性能的GaN及其相关III族氮化物。虽然外延在蓝宝石衬底上的GaN基LED芯片已十分成熟，但是这种芯片大都基于极性面构建而成，这会在量子阱处形成很强的内电场(量级为MV/cm)，容易形成电偶极子并产生自发极化场和压电极化场，进而引起量子束缚斯塔克效应(Quantum-confined Starker Effect，QCSE)，最终降低LED的发光效率。事实上，非极性面的GaN外延薄膜已被证实能避免或减弱薄膜自身自发极化效应的影响，大大提高芯片的发光效率，是国际上公认的最有效方法。与传统的极性面薄膜相比，它更适用应用于LED发光器件。首先，采用非极性面GaN基材料制备LED，理论上可使LED发光效率提高近一倍；其次，非极性面LED不会产生发光波长蓝移的现象；最后，非极性InGaN/GaN量子阱具有偏振特性，并提升光线均匀性，达到节能、改善色调的作用。而非极性面薄膜的外延又很大程度上同衬底材料的选择有关。因此LED产业要获得外延生长的核心技术，提高LED发光效率，势必要寻找一种替代蓝宝石的新型衬底，并实现非极性GaN外延材料的生长。
相比之下，LaAlO 3晶体是生长非极性面GaN及其LED器件更为合适的衬底材料 。研究者发现，LaAlO3化学性质稳定，室温下为单斜晶系结构，空间群为R-3c(No.167)，其晶胞参数为：
Figure PCTCN2019128054-appb-000001
室温下的LaAlO3晶体具有赝立方结构，和理想的钙钛矿结构十分接近。因此LaAlO3单晶对多种钙钛矿结构材料晶格匹配好，是外延生长高温超导薄膜和巨磁阻薄膜极好的衬底材料，其介电性能适合于低损耗微波及介电共振方面的应用。此外，长期以来，LaAlO 3作为高温超导薄膜和巨磁阻薄膜的衬底材料，制备技术成熟，产量大，容易获得所需要的晶面对应的衬底。
问题的解决方案
技术解决方案
本发明所要解决的技术问题是提供一种基于GaN的LED外延片及其制备方法，能够大大缩短裂纹长度，降低缺陷密度，更易获得无裂纹高质量的GaN薄膜。
本发明为解决上述技术问题而采用的技术方案是提供一种基于GaN的LED外延片，包括衬底，其中，所述衬底上依次形成有GaN纳米柱插入层和n-GaN层。
本发明为解决上述技术问题而还提供一种基于GaN的LED外延片的制备方法，其中，包括如下步骤：S1)采用等离子增强金属有机化学气相沉积工艺在衬底上生长GaN纳米柱阵列插入层；S2)采用等离子增强金属有机化学气相沉积工艺在GaN插入层上生长n-GaN层。
进一步地，所述步骤S1中控制反应室温度为800℃，反应室压力为200Torr，通入200sccm氨气、100sccm氮气和380sccm三甲基镓。
进一步地，所述步骤S2中控制反应室温度为1000℃，反应室压力为200Torr，通入60sccm的硅烷、200sccm的氨气、100sccm的氮气、380sccm的三甲基镓。
本发明对比现有技术有如下的有益效果：本发明的GaN插入层采用纳米柱阵列结构，相对于薄膜型缓冲层，纳米柱阵列缓冲层与衬底的接触面积小，应力容易得到释放，可大大缩短裂纹长度；纳米柱材料有缺陷自排除效应，可大大降低缺陷密度。优选新型LaAlO 3衬底，能大大降低量子束缚斯塔克效应(Quantum-confined Starker Effect，QCSE)对后续生长的不利影响，更易在后续生长中获得无裂纹高质量的GaN薄膜。
发明的有益效果
对附图的简要说明
附图说明
图1为本发明实施例中基于GaN的LED外延片结构示意图。
图2为本发明实施例中GaN纳米柱阵列插入层的俯视图。
图3为本发明采用GaN纳米柱阵列插入层的GaN(0002)的x射线衍射图谱。
图4为本发明采用GaN薄膜插入层的GaN(0002)的x射线衍射图谱。
图5为本发明采用GaN纳米柱阵列插入层的GaN(1012)的x射线衍射图谱。
图6为本发明采用GaN薄膜插入层的GaN(1012)的x射线衍射图谱。
发明实施例
本发明的实施方式
下面结合附图和实施例对本发明作进一步的描述，需要说明的是，在不相冲突的前提下，以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。除特殊说明的之外，本实施例中所采用到的材料及设备均可从市场购得。
图1为本发明实施例中基于GaN的LED外延片结构示意图。
请参见图1，本发明提供的基于GaN的LED外延片，包括衬底1，在衬底1上依次形成GaN纳米柱阵列插入层2和n-GaN层3。
本发明的GaN插入层采用纳米柱阵列结构，相对于薄膜型缓冲层，纳米柱阵列缓冲层与衬底的接触面积小。如果薄膜与衬底的接触面积是1的话，那么纳米柱阵列与衬底的接触面积最大是0.785，即边长为1的正方形的内切圆的面积，从而使得应力容易得到释放，可大大缩短裂纹长度。作为优选的实施方式，所述衬底包括蓝宝石、Si、SiC、GaN、ZnO、LiGaO 2、LaSrAlTaO 6、Al或Cu。
对于GaN纳米柱阵列插入层2的厚度选择，插入层厚度过低，会减弱纳米柱本身的缺陷自排除效应，使其缺陷密度增加，不利于后续生长高质量的的n-GaN；插入层厚度过高，纳米柱容易发生弯曲、断裂，使纳米柱的密度、取向均匀性下降，不利于后续生长高质量的n-GaN。作为优选的实施方式，本发明中所述GaN纳米柱阵列的厚度为500～1500nm。
进一步地所述n-GaN层的厚度为1500-3000 nm。n-GaN层厚度过低，会给后续LED芯片的加工增加较大难度，比如要求减薄、刻蚀工艺更加精准，导致芯片良品率下降；n-GaN层厚度过厚，会使n-GaN中的内应力增加，外延片裂纹情况恶化，同时，也会延长生长时间，增加生产成本。
进一步地，Si掺杂浓度为1×10 17～1×10 19cm -3。Si掺杂浓度过低，n-GaN中所能提供的有效载流子不足，会大大降低LED芯片的电学性能，比如亮度降低明显；Si掺杂浓度过高，n-GaN中的缺陷增多，晶体质量会断崖式下降，导致外延片的质量下降，同时也会降低LED芯片的电学性能，比如漏电增加。
本发明提供的基于GaN的LED外延片，制备方法包括：
S1)GaN纳米柱阵列插入层生长步骤：采用等离子体增强金属有机化学气相沉积工艺在LaAlO 3上生长GaN纳米柱插入层；
S2)n-GaN层的生长步骤：采用等离子体增强金属有机化学气相沉积工艺在GaN纳米插入层上生长n-GaN层。
作为优选的实施方式，
步骤S1)中，具体工艺条件如下：
GaN插入层的工艺条件为：反应室温度为800℃，反应室压力为200Torr，通入200sccm氨气、100sccm氮气和380sccm三甲基镓；
步骤S2)中，具体工艺条件如下：
n-GaN层的工艺条件为：反应室温度为1000℃，反应室压力为200Torr，通入60sccm的硅烷、200sccm的氨气、100sccm的氮气、380sccm的三甲基镓；
本发明通过增加GaN纳米阵列插入层来增加GaN外延膜的晶体质量和电学性能的LED外延片结构，其包括LaAlO 3衬底1、厚度为500nm的GaN纳米阵列插入层2、厚度为1.5μm、Si掺杂浓度为1×10 18cm -3的n-GaN层3。
性能检测：
1、XRD，即X-ray diffraction的缩写，是X射线衍射，通过对材料进行X射线衍射，分析其衍射图谱，获得材料的成分、材料内部原子或分子的结构或形态等信息的研究手段。
请继续参照图3-6，横坐标：衍射角度(度)，纵坐标：衍射强度；对比例采用衬底+GaN薄膜+n-GaN层，其中GaN薄膜的厚度与GaN纳米柱插入层厚度相同，此处均为500nm。相对于对比例采用GaN薄膜作为插入层，本发明实施例采用GaN纳米阵列作为插入层之后，GaN薄膜的晶体质量有了显著的提升：GaN(0002)提升了200arcsec，GaN(1012)提升了321arcsec，说明采用GaN纳米阵列作为插入层更易获得高质量的GaN薄膜。
虽然本发明已以较佳实施例揭示如上，然其并非用以限定本发明，任何本领域技术人员，在不脱离本发明的精神和范围内，当可作些许的修改和完善，因此本发明的保护范围当以权利要求书所界定的为准。

Claims (7)

  1. 一种基于GaN的LED外延片，包括衬底，其特征在于，所述衬底上依次形成有GaN纳米柱插入层和n-GaN层。
  2. 如权利要求1所述的基于GaN的LED外延片，其特征在于，所述衬底为LaAlO 3衬底、蓝宝石衬底或SiC衬底。
  3. 如权利要求1所述的基于GaN的LED外延片，其特征在于，所述GaN纳米柱阵列插入层的厚度为500-1500nm。
  4. 如权利要求1所述的基于GaN的LED外延片，其特征在于，所述n-GaN层的厚度为1500～3000nm，Si掺杂浓度为1×10 17～1×10 19cm -3。
  5. 一种如权利要求1～4任一项所述的基于GaN的LED外延片的制备方法，其特征在于，包括如下步骤：
    S1)采用等离子增强金属有机化学气相沉积工艺在衬底上生长GaN纳米柱阵列插入层；
    S2)采用等离子增强金属有机化学气相沉积工艺在GaN插入层上生长n-GaN层。
  6. 如权利要求5所述的基于GaN的LED外延片的制备方法，其特征在于，所述步骤S1中控制反应室温度为800℃，反应室压力为200Torr，通入200sccm氨气、100sccm氮气和380sccm三甲基镓。
  7. 如权利要求5所述的基于GaN的LED外延片的制备方法，其特征在于，所述步骤S2中控制反应室温度为1000℃，反应室压力为200Torr，通入60sccm的硅烷、200sccm的氨气、100sccm的氮气、380sccm的三甲基镓。
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