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CN115116828B - Homoepitaxial structure based on nitride single crystal substrate and uniformity regulating and controlling method thereof - Google Patents

Homoepitaxial structure based on nitride single crystal substrate and uniformity regulating and controlling method thereof Download PDF

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CN115116828B
CN115116828B CN202210759553.XA CN202210759553A CN115116828B CN 115116828 B CN115116828 B CN 115116828B CN 202210759553 A CN202210759553 A CN 202210759553A CN 115116828 B CN115116828 B CN 115116828B
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王国斌
闫其昂
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Jiangsu Third Generation Semiconductor Research Institute Co Ltd
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Abstract

The application discloses a homoepitaxial structure based on a nitride single crystal substrate and a uniformity regulating and controlling method thereof. The uniformity control method comprises the following steps: providing a nitride single crystal substrate containing a second group III element; growing an interfacial relaxation layer on the substrate, the interfacial relaxation layer comprising a binary nitride layer comprising a first group III element, the first group III element being different from the second group III element to create a compressive or tensile stress to balance warpage of the substrate; and growing a warp-controlling layer on the interface relaxation layer, wherein the warp-controlling layer comprises a ternary nitride layer or a superlattice structure containing the ternary nitride layer. The application realizes the controllable warp and high uniformity growth of the homoepitaxial structure by the controllable growth of the interfacial relaxation layer and the warp regulating layer on the substrate; meanwhile, the prepared homoepitaxial structure is smoother, and has wide application prospect in photoelectric devices or electronic devices.

Description

基于氮化物单晶衬底的同质外延结构及其均匀性调控方法Homoepitaxial structure based on nitride single crystal substrate and its uniformity control method

技术领域Technical Field

本申请涉及一种半导体发光结构,具体涉及一种基于氮化物单晶衬底的同质外延结构及其均匀性调控方法,属于半导体技术领域。The present application relates to a semiconductor light-emitting structure, specifically to a homoepitaxial structure based on a nitride single crystal substrate and a method for regulating its uniformity, and belongs to the field of semiconductor technology.

背景技术Background technique

GaN基器件的生长大多基于蓝宝石、硅等异质衬底,需要从衬底通过生长过渡层来消除失配,从而获得GaN外延层。同时,其过渡层也是调整外延片的凹凸性,进而达到调节外延片生长均匀性的重要手段。比如在蓝光LED的外延生长中,在生长有源区量子阱时,In组分决定了发光波长,而In的融入与温度相关,如果外延片不平温度就会不均匀,造成In的分布不均,进而降低了波长的均匀性。此时,通常可以通过调整过渡层来实现调节翘曲,使得在量子阱生长过程中外延片尽可能的平,从而保证波长均匀性。The growth of GaN-based devices is mostly based on heterogeneous substrates such as sapphire and silicon. It is necessary to eliminate the mismatch from the substrate by growing a transition layer to obtain a GaN epitaxial layer. At the same time, its transition layer is also an important means to adjust the unevenness of the epitaxial wafer, thereby adjusting the uniformity of the epitaxial wafer growth. For example, in the epitaxial growth of blue light LEDs, when growing the quantum wells in the active area, the In component determines the emission wavelength, and the incorporation of In is related to temperature. If the epitaxial wafer is uneven, the temperature will be uneven, resulting in uneven distribution of In, thereby reducing the uniformity of the wavelength. At this time, the warping can usually be adjusted by adjusting the transition layer, so that the epitaxial wafer is as flat as possible during the quantum well growth process, thereby ensuring wavelength uniformity.

而基于GaN单晶衬底的同质外延生长,由于衬底已经是GaN材料层,不需要任何过渡层,所以在后期的生长中无法通过过渡层来调整翘曲值。而随着不同掺杂浓度的外延层材料以及GaN单晶衬底本身在高温下翘曲变化,都会影响到生长时外延片所受的温度,进而影响到外延片的均匀性。但是,目前的常规生长方法没有任何技术和办法对此进行调控。Homoepitaxial growth based on GaN single crystal substrates does not require any transition layer because the substrate is already a GaN material layer. Therefore, the warpage value cannot be adjusted through the transition layer in the later growth. The warpage changes of epitaxial layer materials with different doping concentrations and the GaN single crystal substrate itself at high temperatures will affect the temperature of the epitaxial wafer during growth, and thus affect the uniformity of the epitaxial wafer. However, the current conventional growth methods do not have any technology or method to regulate this.

发明内容Summary of the invention

本申请的主要目的在于提供一种基于氮化物单晶衬底的同质外延结构及其均匀性调控方法,以克服现有技术中的不足。The main purpose of the present application is to provide a homoepitaxial structure based on a nitride single crystal substrate and a method for controlling its uniformity, so as to overcome the deficiencies in the prior art.

为实现前述发明目的,本申请采用的技术方案包括:In order to achieve the aforementioned invention objectives, the technical solutions adopted in this application include:

本申请的一个方面提供了一种基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其包括:One aspect of the present application provides a method for controlling the uniformity of a homoepitaxial structure based on a nitride single crystal substrate, comprising:

提供氮化物单晶衬底,所述衬底包括第二III族元素;providing a nitride single crystal substrate, the substrate comprising a second Group III element;

在所述衬底上生长界面弛豫层,所述界面弛豫层包括二元氮化物层,所述二元氮化物层包括第一III族元素,所述第一III族元素与所述第二III族元素不同,以产生压应力或张应力,从而平衡所述衬底的翘曲;Growing an interface relaxation layer on the substrate, the interface relaxation layer comprising a binary nitride layer, the binary nitride layer comprising a first Group III element, the first Group III element being different from the second Group III element to generate compressive stress or tensile stress, thereby balancing the warpage of the substrate;

在所述界面弛豫层上生长翘曲调控层,所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构,所述三元氮化物层包括第一III族元素和第二III族元素。A warp regulation layer is grown on the interface relaxation layer, the surface of the warp regulation layer is flat, the warp regulation layer comprises a ternary nitride layer or a superlattice structure comprising a ternary nitride layer, and the ternary nitride layer comprises a first group III element and a second group III element.

本申请的一个方面提供了一种基于氮化物单晶衬底的同质外延结构,其特征在于,包括:One aspect of the present application provides a homoepitaxial structure based on a nitride single crystal substrate, characterized in that it includes:

氮化物单晶衬底,Nitride single crystal substrate,

界面弛豫层,其生长在所述衬底上,所述界面弛豫层包括二元氮化层,所述二元氮化层的组成材料与所述衬底的组成材料晶格失配,以产生压应力或张应力,从而平衡所述衬底的翘曲;An interface relaxation layer grown on the substrate, the interface relaxation layer comprising a binary nitride layer, the constituent material of the binary nitride layer being lattice mismatched with the constituent material of the substrate to generate compressive stress or tensile stress, thereby balancing the warping of the substrate;

翘曲调控层,其生长在所述界面弛豫层上,所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构。A warp regulation layer is grown on the interface relaxation layer, the surface of the warp regulation layer is flat, and the warp regulation layer includes a ternary nitride layer or a superlattice structure including the ternary nitride layer.

本申请的另又一个方面提供了所述基于氮化物单晶衬底的同质外延结构在制备UV-LED器件或GaN基器件中的用途。Another aspect of the present application provides use of the homoepitaxial structure based on a nitride single crystal substrate in preparing a UV-LED device or a GaN-based device.

相较于现有技术,本申请通过在氮化物单晶衬底上先进行界面弛豫层和翘曲调控层的可控生长(具体通过界面弛豫层和翘曲调控层的组分和厚度进行调整),从而实现同质外延结构的高均匀性生长;同时制备的同质外延结构更加平整,在光电器件或者电子器件中有广泛的应用前景。Compared with the prior art, the present application realizes highly uniform growth of a homoepitaxial structure by first performing controllable growth of an interface relaxation layer and a warp regulation layer on a nitride single crystal substrate (specifically by adjusting the composition and thickness of the interface relaxation layer and the warp regulation layer); at the same time, the prepared homoepitaxial structure is smoother and has broad application prospects in optoelectronic devices or electronic devices.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

为了更清楚地说明本申请实施例中的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本申请的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

图1a-图1b分别为本申请一典型实施例方案中同质外延结构的示意图。FIG. 1a - FIG. 1b are schematic diagrams of a homoepitaxial structure in a typical embodiment of the present application.

图2为本申请实施例1中制备的同质外延结构样品A的光致发光PL测试图谱;FIG2 is a photoluminescence PL test spectrum of the homoepitaxial structure sample A prepared in Example 1 of the present application;

图3为本申请对比例1中制备的同质外延结构样品B的光致发光PL测试图谱;FIG3 is a photoluminescence PL test spectrum of the homoepitaxial structure sample B prepared in Comparative Example 1 of the present application;

图4位本申请一典型实施例方案中在制备界面弛豫层和翘曲调控层时第一III族源、第二III族源及氮源通入装置示意图。4 is a schematic diagram of a device for introducing a first Group III source, a second Group III source and a nitrogen source when preparing an interface relaxation layer and a warpage regulation layer in a typical embodiment of the present application.

具体实施方式Detailed ways

鉴于现有技术的不足,本案发明人经长期研究和实践,得以提出本申请的技术方案,如下将予以更为详细的说明。In view of the deficiencies in the prior art, the inventor of this case, after long-term research and practice, was able to propose the technical solution of this application, which will be described in more detail below.

本申请的一些实施例提供的一种基于氮化物单晶衬底的同质外延结构的均匀性调控方法包括:Some embodiments of the present application provide a method for controlling the uniformity of a homoepitaxial structure based on a nitride single crystal substrate, including:

提供氮化物单晶衬底,所述衬底包括第二III族元素;providing a nitride single crystal substrate, the substrate comprising a second Group III element;

在所述衬底上生长界面弛豫层,所述界面弛豫层包括二元氮化物层,所述二元氮化物层包括第一III族元素,所述第一III族元素与所述第二III族元素不同,以产生压应力或张应力,从而平衡所述衬底的翘曲;Growing an interface relaxation layer on the substrate, the interface relaxation layer comprising a binary nitride layer, the binary nitride layer comprising a first Group III element, the first Group III element being different from the second Group III element to generate compressive stress or tensile stress, thereby balancing the warpage of the substrate;

在所述界面弛豫层上生长翘曲调控层,所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构,所述三元氮化物层包括第一III族元素和第二III族元素。A warp regulation layer is grown on the interface relaxation layer, the surface of the warp regulation layer is flat, the warp regulation layer comprises a ternary nitride layer or a superlattice structure comprising a ternary nitride layer, and the ternary nitride layer comprises a first group III element and a second group III element.

在一个实施例中,所述二元氮化物层的组成材料的晶格常数大于所述氮化物单晶衬底的组成材料的晶格常数,以产生张应力;或者,所述二元氮化物层的组成材料的晶格常数小于所述氮化物单晶衬底的组成材料的晶格常数,以产生压应力。In one embodiment, the lattice constant of the constituent material of the binary nitride layer is greater than the lattice constant of the constituent material of the nitride single crystal substrate to generate tensile stress; or, the lattice constant of the constituent material of the binary nitride layer is less than the lattice constant of the constituent material of the nitride single crystal substrate to generate compressive stress.

在一个实施例中,所述第一III族元素为Al或In,第二III族元素为Ga。In one embodiment, the first Group III element is Al or In, and the second Group III element is Ga.

在一个实施例中,所述第一III族元素与第二III族元素相邻。In one embodiment, the first Group III element is adjacent to the second Group III element.

在一个实施例中,所述氮化物单晶衬底的厚度在1μm以上。In one embodiment, the thickness of the nitride single crystal substrate is greater than 1 μm.

进一步地,所述氮化物单晶衬底的厚度为1-2.5μm。Furthermore, the thickness of the nitride single crystal substrate is 1-2.5 μm.

在一个实施例中,所述界面弛豫层的厚度为1-10nm。In one embodiment, the thickness of the interface relaxation layer is 1-10 nm.

在一个实施例中,所述三元氮化物层的厚度为10nm-100nm,所述包含三元氮化物层的超晶格结构的厚度为10nm-200nm。In one embodiment, the thickness of the ternary nitride layer is 10 nm-100 nm, and the thickness of the superlattice structure including the ternary nitride layer is 10 nm-200 nm.

在一个实施例中,当所述预置应力为张应力时,所述二元氮化物层中第一III族元素的含量为5at.%~10at.%,所述包含三元氮化物层的超晶格结构中第一III族元素的含量为5at.%~20at.%。In one embodiment, when the preset stress is tensile stress, the content of the first group III element in the binary nitride layer is 5 at.% to 10 at.%, and the content of the first group III element in the superlattice structure including the ternary nitride layer is 5 at.% to 20 at.%.

具体地,所述二元氮化物层为InN材料时,所述三元氮化物层为InGaN材料,且InGaN材料中In元素的含量为5at.%~10at.%,三元氮化物层的厚度为10~50nm,同时所述三元氮化物层中的组分可不变也可以是组分渐变。Specifically, when the binary nitride layer is InN material, the ternary nitride layer is InGaN material, and the content of In element in the InGaN material is 5at.% to 10at.%, the thickness of the ternary nitride layer is 10 to 50nm, and the components in the ternary nitride layer can be constant or gradually changed.

具体地,所述二元氮化物层为InN材料时,所述包含三元氮化物层的超晶格结构为InGaN/GaN超晶格结构,且InGaN材料中In元素的含量为5at.%~20at.%,包含三元氮化物层的超晶格结构的厚度为10~200nm。Specifically, when the binary nitride layer is InN material, the superlattice structure including the ternary nitride layer is an InGaN/GaN superlattice structure, and the content of In element in the InGaN material is 5at.% to 20at.%, and the thickness of the superlattice structure including the ternary nitride layer is 10 to 200nm.

在一个实施例中,当所述预置应力为压应力时,所述三元氮化物层中第一III族元素的含量为5at.%~20at.%,所述包含三元氮化物层的超晶格结构中第一III族元素的含量为5at.%~100at.%。In one embodiment, when the preset stress is compressive stress, the content of the first group III element in the ternary nitride layer is 5 at.% to 20 at.%, and the content of the first group III element in the superlattice structure including the ternary nitride layer is 5 at.% to 100 at.%.

具体地,所述二元氮化物层为AlN材料时,所述三元氮化物层为AlGaN单层材料,AlGaN中Al元素的含量为5at.%~20at.%,三元氮化物层的厚度为10~100nm,同时所述三元氮化物层中的组分可不变也可以是组分渐变。Specifically, when the binary nitride layer is AlN material, the ternary nitride layer is AlGaN single layer material, the Al content in AlGaN is 5at.% to 20at.%, the thickness of the ternary nitride layer is 10 to 100nm, and the components in the ternary nitride layer can be constant or gradually changed.

具体地,所述二元氮化物层为AlN材料时,所述包含三元氮化物层的超晶格结构为AlGaN/GaN超晶格结构,AlGaN中Al元素的含量为5at.%~100at.%,包含三元氮化物层的超晶格结构的厚度为10~200nm。Specifically, when the binary nitride layer is AlN material, the superlattice structure including the ternary nitride layer is an AlGaN/GaN superlattice structure, the content of Al element in AlGaN is 5at.% to 100at.%, and the thickness of the superlattice structure including the ternary nitride layer is 10 to 200nm.

进一步地,所述超晶格结构包括InGaN/GaN超晶格结构、AlGaN/GaN超晶格结构等,且不限于此。Furthermore, the superlattice structure includes an InGaN/GaN superlattice structure, an AlGaN/GaN superlattice structure, etc., but is not limited thereto.

本申请中,GaN的晶格常数介于InN和AlN之间,而三者的热失配小于晶格失配,故可以灵活实现张应力和压应力之间的转变。比如,InN的晶格常数大于GaN,此时在GaN单晶衬底上生长In(Ga)N时,就会引入张应力,使后续生长的外延层往凹的方向弯曲。而AlN的晶格常数小于GaN,此时在衬底上生长Al(Ga)N时,就会引入压应力,使后续生长的外延层往凸的方向弯曲。而由于生长的是异质层材料,其晶格是不匹配的,需要单晶衬底这样晶体质量很好的材料为基底。从而实现了本申请中氮化物单晶衬底的同质外延结构的均匀性调控方法。In the present application, the lattice constant of GaN is between InN and AlN, and the thermal mismatch of the three is smaller than the lattice mismatch, so the transition between tensile stress and compressive stress can be flexibly realized. For example, the lattice constant of InN is greater than that of GaN. At this time, when In(Ga)N is grown on a GaN single crystal substrate, tensile stress will be introduced, causing the subsequently grown epitaxial layer to bend in a concave direction. The lattice constant of AlN is smaller than that of GaN. At this time, when Al(Ga)N is grown on a substrate, compressive stress will be introduced, causing the subsequently grown epitaxial layer to bend in a convex direction. However, since a heterogeneous layer material is grown, its lattice is not matched, and a single crystal substrate with very good crystal quality is required as a substrate. Thereby realizing the uniformity control method of the homoepitaxial structure of a nitride single crystal substrate in the present application.

在一个实施例中,所述基于氮化物单晶衬底的同质外延结构的均匀性调控方法具体包括:In one embodiment, the method for controlling the uniformity of the homoepitaxial structure based on a nitride single crystal substrate specifically includes:

S1、将所述衬底置入生长腔室,并在所述生长腔室内形成保护性气氛,之后将所述衬底温度设置为所述二元氮化物层的生长温度,再向所述生长腔室内输入第一III族源,以在所述衬底表面沉积一层第一III族元素的原子,形成界面浸润层;S1, placing the substrate into a growth chamber, and forming a protective atmosphere in the growth chamber, then setting the substrate temperature to the growth temperature of the binary nitride layer, and then inputting a first group III source into the growth chamber to deposit a layer of atoms of the first group III element on the surface of the substrate to form an interface wetting layer;

S2、向所述生长腔室内输入第一III族源和氮源,在所述界面浸润层上生长二元氮化物层,从而形成界面弛豫层;S2, inputting a first Group III source and a nitrogen source into the growth chamber to grow a binary nitride layer on the interface wetting layer, thereby forming an interface relaxation layer;

S3、向所述生长腔室内输入第一III族源、第二III族源及氮源,在所述界面弛豫层上生长三元氮化物层或包含三元氮化物层的超晶格结构,从而形成翘曲调控层。S3. Inputting a first Group III source, a second Group III source and a nitrogen source into the growth chamber, growing a ternary nitride layer or a superlattice structure including the ternary nitride layer on the interface relaxation layer, thereby forming a warp regulation layer.

进一步地,所述第一III族源可以是In、Al、Ga、B源等,且不限于此。Furthermore, the first Group III source may be an In, Al, Ga, B source, etc., but is not limited thereto.

具体地,所述第一III族源可以是TMIn或者TMAl。Specifically, the first Group III source may be TMIn or TMAl.

进一步地,所述第二III族源可以是Al、Ga、源等,且不限于此。Further, the second Group III source may be Al, Ga, source, etc., but is not limited thereto.

在一个实施例中,所述氮化物单晶衬底包括GaN单晶衬底或AlN单晶衬底。In one embodiment, the nitride single crystal substrate includes a GaN single crystal substrate or an AlN single crystal substrate.

在一个实施例中,步骤S3具体包括:将所述第一III族源、第二III族源及氮源交替输入所述生长腔室,在所述界面弛豫层上生长超晶格结构,从而形成所述翘曲调控层。In one embodiment, step S3 specifically includes: alternately inputting the first group III source, the second group III source and the nitrogen source into the growth chamber, growing a superlattice structure on the interface relaxation layer, thereby forming the warp regulation layer.

在一个实施例中,步骤S3具体包括:向所述生长腔室内输入第一III族源、第二III族源及氮源,并将所述第一III族源、第二III族源及氮源的流量控制在200sccm以下,以及将所述生长腔室内的气压设置为30-70torr,在所述界面弛豫层上生长超晶格结构,从而形成所述翘曲调控层。In one embodiment, step S3 specifically includes: inputting a first Group III source, a second Group III source and a nitrogen source into the growth chamber, and controlling the flow rates of the first Group III source, the second Group III source and the nitrogen source to be below 200 sccm, and setting the gas pressure in the growth chamber to 30-70 torr, growing a superlattice structure on the interface relaxation layer, thereby forming the warp regulation layer.

例如,对于AlGaN/GaN的超晶格层,可以通过交替通入所需的Al源、Ga源和N源,交替在衬底表面淀积成膜,降低生长速率,提高晶格排布的致密性;此外,还可以在AlGaN/GaN的超晶格层的生长时,降低气流流量,200sccm;降低压强,30-70torr,以提高晶格排布的致密性。For example, for the AlGaN/GaN superlattice layer, the required Al source, Ga source and N source can be alternately introduced to alternately deposit films on the substrate surface to reduce the growth rate and improve the density of the lattice arrangement; in addition, when growing the AlGaN/GaN superlattice layer, the gas flow rate can be reduced to 200sccm and the pressure can be reduced to 30-70torr to improve the density of the lattice arrangement.

在一个实施例中,在制备界面弛豫层和翘曲调控层时,所述第一III族源、第二III族源及氮源通入装置示意图如图4所示。In one embodiment, when preparing the interface relaxation layer and the warpage regulation layer, the schematic diagram of the first Group III source, the second Group III source and the nitrogen source introduction device is shown in FIG4 .

在一个实施例中,当所述氮化物单晶衬底为GaN单晶衬底时,所述二元氮化物层为AlN层,所述三元氮化物层为AlxGa1-xN层,所述包含三元氮化物层的超晶格结构为AlxGa1-xN/GaN超晶格结构,0<x<1;In one embodiment, when the nitride single crystal substrate is a GaN single crystal substrate, the binary nitride layer is an AlN layer, the ternary nitride layer is an AlxGa1 -xN layer, the superlattice structure including the ternary nitride layer is an AlxGa1 -xN /GaN superlattice structure, 0<x<1;

或者,当所述氮化物单晶衬底为GaN单晶衬底时,所述二元氮化物层为InN层,所述三元氮化物层为InyGa1-yN层,所述包含三元氮化物层的超晶格结构为InyGa1-yN/GaN超晶格结构,0<y<1;Alternatively, when the nitride single crystal substrate is a GaN single crystal substrate, the binary nitride layer is an InN layer, the ternary nitride layer is an In y Ga 1-y N layer, the superlattice structure including the ternary nitride layer is an In y Ga 1-y N/GaN superlattice structure, 0<y<1;

或者,当所述氮化物单晶衬底为AlN单晶衬底时,所述二元氮化物层为GaN层,所述三元氮化物层为AlxGa1-xN层,所述包含三元氮化物层的超晶格结构为AlxGa1-xN/AlN超晶格结构,0<x<1;Alternatively, when the nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a GaN layer, the ternary nitride layer is an AlxGa1 -xN layer, the superlattice structure including the ternary nitride layer is an AlxGa1 -xN /AlN superlattice structure, 0<x<1;

或者,当所述氮化物单晶衬底为AlN单晶衬底时,所述二元氮化物层为BN层,所述三元氮化物层为BxAl1-xN层,所述包含三元氮化物层的超晶格结构为BxAl1-xN/AlN超晶格结构,0<x<1。Alternatively, when the nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a BN layer, the ternary nitride layer is a BxAl1 -xN layer, the superlattice structure including the ternary nitride layer is a BxAl1-xN /AlN superlattice structure, and 0<x<1.

在一个实施例中,所述均匀性调控方法还包括:在所述翘曲调控层上生长半导体功能层。In one embodiment, the uniformity control method further comprises: growing a semiconductor functional layer on the warp control layer.

在一个较为具体的实施方案中,所述基于氮化物单晶衬底的同质外延结构的均匀性调控方法可以包括:In a more specific embodiment, the method for controlling the uniformity of the homoepitaxial structure based on a nitride single crystal substrate may include:

首先,在氨气的保护GaN单晶衬底的情况下升温到InN基或者AlN基材料的生长温度后,进行界面弛豫层的生长。需要断开氨气的同时,通入有机金属源TMIn或者TMAl,时间控制在几秒,目的是为了在GaN单晶衬底上铺一层金属In原子或者金属Al原子,作用是浸润衬底二次外延的界面层。然后切入氨气,进行生长InN或者AlN材料,为后续失配材料进行晶格弛豫,从而生长界面弛豫层,厚度控制在1-10nm。界面弛豫层为生长翘曲调控层进行前期的弛豫和界面处理,来保证后续较厚的材料的晶体质量和有效调控。First, under the protection of ammonia, the temperature of the GaN single crystal substrate is raised to the growth temperature of the InN-based or AlN-based material, and then the interface relaxation layer is grown. It is necessary to disconnect the ammonia and introduce the organic metal source TMIn or TMAl at the same time, and the time is controlled to be a few seconds. The purpose is to lay a layer of metal In atoms or metal Al atoms on the GaN single crystal substrate, which serves to wet the interface layer of the secondary epitaxial growth of the substrate. Then cut in the ammonia to grow InN or AlN materials, and perform lattice relaxation for subsequent mismatch materials, so as to grow an interface relaxation layer with a thickness controlled at 1-10nm. The interface relaxation layer performs early relaxation and interface treatment for the growth of the warp control layer to ensure the crystal quality and effective regulation of subsequent thicker materials.

接着,对应InN基材料的界面弛豫层,则生长翘曲调控层为InGaN材料或者InGaN/GaN超晶格结构来进行外延片凹方向的弯曲调整;InGaN材料的In元素的含量为5%~10%,组分可不变也可以是组分渐变,厚度范围10-50nm,如果是InGaN/GaN超晶格结构,InGaN的In元素的含量为5%~20%,则厚度范围10-200nm。对应AlN基材料的界面弛豫层,则生长翘曲调控层为AlGaN单层材料或者AlGaN超晶格结构来进行外延片凸方向的弯曲调整;AlGaN材料的Al元素的含量为5%~20%,组分可不变也可以是组分渐变,厚度范围10-100nm。如果是AlGaN/GaN超晶格结构,AlGaN的Al元素的含量为5%~100%,厚度范围10-200nm。以上完成翘曲调控层的生长。Next, corresponding to the interface relaxation layer of the InN-based material, the warpage control layer is grown as InGaN material or InGaN/GaN superlattice structure to adjust the curvature of the epitaxial wafer in the concave direction; the content of the In element in the InGaN material is 5% to 10%, the composition can be unchanged or the composition can be gradually changed, and the thickness range is 10-50nm. If it is an InGaN/GaN superlattice structure, the content of the In element in InGaN is 5% to 20%, and the thickness range is 10-200nm. Corresponding to the interface relaxation layer of the AlN-based material, the warpage control layer is grown as AlGaN single layer material or AlGaN superlattice structure to adjust the curvature of the epitaxial wafer in the convex direction; the content of the Al element in the AlGaN material is 5% to 20%, the composition can be unchanged or the composition can be gradually changed, and the thickness range is 10-100nm. If it is an AlGaN/GaN superlattice structure, the content of the Al element in AlGaN is 5% to 100%, and the thickness range is 10-200nm. The above completes the growth of the warpage control layer.

本申请提出在GaN单晶衬底上,首先沉积界面弛豫层,为后续翘曲调控层做准备,该层的材料为金属In/InN材料或金属Al/AlN材料,后续再以Al(In)GaN材料或者超晶格材料为翘曲调控层,然后再生长外延结构,如光电器件的LED或者电子器件的HEMT结构。本申请通过翘曲调控层中In(Ga)N或Al(Ga)N的组分和厚度调整,来实现整个外延片的凹凸性调节,从而实现对翘曲的可控以及高均匀性外延片的生长。The present application proposes to first deposit an interface relaxation layer on a GaN single crystal substrate to prepare for a subsequent warpage control layer, wherein the material of the layer is a metal In/InN material or a metal Al/AlN material, and then an Al(In)GaN material or a superlattice material is used as a warpage control layer, and then an epitaxial structure is grown, such as an LED of an optoelectronic device or a HEMT structure of an electronic device. The present application adjusts the concavity and convexity of the entire epitaxial wafer by adjusting the composition and thickness of In(Ga)N or Al(Ga)N in the warpage control layer, thereby achieving controllable warpage and growth of highly uniform epitaxial wafers.

本申请中为了平衡氮化物单晶衬底的翘曲问题,先生长与氮化物单晶衬底晶格失配大的界面弛豫层来平衡衬底的翘曲,同时也可以作为后续翘曲调控层的过渡层,提高晶体质量;其次后续生长的翘曲调控层是为了将平衡翘曲后的结构逐渐长平,可以通过减缓生长速率,使得晶格排布更加致密,拉应力或压应力更加均匀,实现更好的平整度。In order to balance the warping problem of the nitride single crystal substrate in the present application, an interface relaxation layer with a large lattice mismatch with the nitride single crystal substrate is first grown to balance the warping of the substrate. It can also serve as a transition layer for the subsequent warping control layer to improve the crystal quality. Secondly, the subsequently grown warping control layer is to gradually flatten the structure after the balanced warping. The growth rate can be slowed down to make the lattice arrangement denser, the tensile stress or compressive stress more uniform, and better flatness can be achieved.

本申请的一些实施例提供了一种基于氮化物单晶衬底的同质外延结构,其包括:Some embodiments of the present application provide a homoepitaxial structure based on a nitride single crystal substrate, comprising:

氮化物单晶衬底;Nitride single crystal substrate;

界面弛豫层,其生长在所述衬底上,所述界面弛豫层包括二元氮化层,所述二元氮化层的组成材料与所述衬底的组成材料晶格失配,以产生压应力或张应力,从而平衡所述衬底的翘曲;An interface relaxation layer grown on the substrate, the interface relaxation layer comprising a binary nitride layer, the constituent material of the binary nitride layer being lattice mismatched with the constituent material of the substrate to generate compressive stress or tensile stress, thereby balancing the warping of the substrate;

翘曲调控层,其生长在所述界面弛豫层上,所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构。A warp regulation layer is grown on the interface relaxation layer, the surface of the warp regulation layer is flat, and the warp regulation layer includes a ternary nitride layer or a superlattice structure including the ternary nitride layer.

在一个实施例中,所述基于氮化物单晶衬底的同质外延结构还包括半导体功能层,所述半导体功能层生长在所述翘曲调控层上。In one embodiment, the homoepitaxial structure based on a nitride single crystal substrate further includes a semiconductor functional layer, and the semiconductor functional layer is grown on the warp regulating layer.

在一个实施例中,所述二元氮化层第一III族氮化层的组成材料的晶格常数大于所述衬底的组成材料的晶格常数,以产生张应力;或者,所述第一III族氮化层的组成材料的晶格常数小于所述衬底的组成材料的晶格常数,以产生压应力。In one embodiment, the lattice constant of the constituent material of the first Group III nitride layer of the binary nitride layer is greater than the lattice constant of the constituent material of the substrate to generate tensile stress; or, the lattice constant of the constituent material of the first Group III nitride layer is less than the lattice constant of the constituent material of the substrate to generate compressive stress.

在一个实施例中,所述氮化物单晶衬底的厚度在1μm以上。In one embodiment, the thickness of the nitride single crystal substrate is greater than 1 μm.

进一步地,所述氮化物单晶衬底的厚度为1-2.5μm。Furthermore, the thickness of the nitride single crystal substrate is 1-2.5 μm.

在一个实施例中,所述界面弛豫层的厚度为1-10nm。In one embodiment, the thickness of the interface relaxation layer is 1-10 nm.

在一个实施例中,所述三元氮化物层的厚度为10nm-100nm,所述包含所述三元氮化物层组成的超晶格结构的厚度为10nm-200nm。In one embodiment, the thickness of the ternary nitride layer is 10 nm-100 nm, and the thickness of the superlattice structure composed of the ternary nitride layer is 10 nm-200 nm.

在一个实施例中,当所述氮化物单晶衬底为GaN单晶衬底时,所述二元氮化物层为AlN层,所述三元氮化物层为AlxGa1-xN层,所述包含三元氮化物层的超晶格结构为AlxGa1-xN/GaN超晶格结构,0<x<1;In one embodiment, when the nitride single crystal substrate is a GaN single crystal substrate, the binary nitride layer is an AlN layer, the ternary nitride layer is an AlxGa1 -xN layer, the superlattice structure including the ternary nitride layer is an AlxGa1 -xN /GaN superlattice structure, 0<x<1;

或者,当所述氮化物单晶衬底为GaN单晶衬底时,所述二元氮化物层为InN层,所述三元氮化物层为InyGa1-yN层,所述包含三元氮化物层的超晶格结构为InyGa1-yN/GaN超晶格结构,0<y<1;Alternatively, when the nitride single crystal substrate is a GaN single crystal substrate, the binary nitride layer is an InN layer, the ternary nitride layer is an In y Ga 1-y N layer, the superlattice structure including the ternary nitride layer is an In y Ga 1-y N/GaN superlattice structure, 0<y<1;

或者,当所述氮化物单晶衬底为AlN单晶衬底时,所述二元氮化物层为GaN层,所述三元氮化物层为AlxGa1-xN层,所述包含三元氮化物层的超晶格结构为AlxGa1-xN/AlN超晶格结构,0<x<1;Alternatively, when the nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a GaN layer, the ternary nitride layer is an AlxGa1 -xN layer, the superlattice structure including the ternary nitride layer is an AlxGa1 -xN /AlN superlattice structure, 0<x<1;

或者,当所述氮化物单晶衬底为AlN单晶衬底时,所述二元氮化物层为BN层,所述三元氮化物层为BxAl1-xN层,所述包含三元氮化物层的超晶格结构为BxAl1-xN/AlN超晶格结构,0<x<1。Alternatively, when the nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a BN layer, the ternary nitride layer is a BxAl1 -xN layer, the superlattice structure including the ternary nitride layer is a BxAl1 -xN /AlN superlattice structure, and 0<x<1.

在一个实施例中,所述均匀性调控方法还包括:在所述翘曲调控层上生长半导体功能层。In one embodiment, the uniformity control method further comprises: growing a semiconductor functional layer on the warp control layer.

在一个实施例中,当所述预置应力为张应力时,所述二元氮化物层中第一III族元素的含量为5at.%~10at.%,所述包含三元氮化物层的超晶格结构中第一III族元素的含量为5at.%~20at.%。In one embodiment, when the preset stress is tensile stress, the content of the first group III element in the binary nitride layer is 5 at.% to 10 at.%, and the content of the first group III element in the superlattice structure including the ternary nitride layer is 5 at.% to 20 at.%.

具体地,所述二元氮化物层为InN材料时,所述三元氮化物层为InGaN材料,且InGaN材料中In元素的含量为5at.%~10at.%,三元氮化物层的厚度为10~50nm,同时所述三元氮化物层中的组分可不变也可以是组分渐变。Specifically, when the binary nitride layer is InN material, the ternary nitride layer is InGaN material, and the content of In element in the InGaN material is 5at.% to 10at.%, the thickness of the ternary nitride layer is 10 to 50nm, and the components in the ternary nitride layer can be constant or gradually changed.

具体地,所述二元氮化物层为InN材料时,所述包含三元氮化物层的超晶格结构为InGaN/GaN超晶格结构,且InGaN材料中In元素的含量为5at.%~20at.%,包含三元氮化物层的超晶格结构的厚度为10~200nm。Specifically, when the binary nitride layer is InN material, the superlattice structure including the ternary nitride layer is an InGaN/GaN superlattice structure, and the content of In element in the InGaN material is 5at.% to 20at.%, and the thickness of the superlattice structure including the ternary nitride layer is 10 to 200nm.

在一个实施例中,当所述预置应力为压应力时,所述三元氮化物层中第一III族元素的含量为5at.%~20at.%,所述包含三元氮化物层的超晶格结构中第一III族元素的含量为5at.%~100at.%。In one embodiment, when the preset stress is compressive stress, the content of the first group III element in the ternary nitride layer is 5 at.% to 20 at.%, and the content of the first group III element in the superlattice structure including the ternary nitride layer is 5 at.% to 100 at.%.

具体地,所述二元氮化物层为AlN材料时,所述三元氮化物层为AlGaN单层材料,AlGaN中Al元素的含量为5at.%~20at.%,三元氮化物层的厚度为10~100nm,同时所述三元氮化物层中的组分可不变也可以是组分渐变。Specifically, when the binary nitride layer is AlN material, the ternary nitride layer is AlGaN single layer material, the Al content in AlGaN is 5at.% to 20at.%, the thickness of the ternary nitride layer is 10 to 100nm, and the components in the ternary nitride layer can be constant or gradually changed.

具体地,所述二元氮化物层为AlN材料时,所述包含三元氮化物层的超晶格结构为AlGaN/GaN超晶格结构,AlGaN中Al元素的含量为5at.%~100at.%,包含三元氮化物层的超晶格结构的厚度为10~200nm。Specifically, when the binary nitride layer is AlN material, the superlattice structure including the ternary nitride layer is an AlGaN/GaN superlattice structure, the content of Al element in AlGaN is 5at.% to 100at.%, and the thickness of the superlattice structure including the ternary nitride layer is 10 to 200nm.

在一个实施例中,所述氮化物单晶衬底包括GaN单晶衬底或AlN单晶衬底,且不限于此。In one embodiment, the nitride single crystal substrate includes a GaN single crystal substrate or an AlN single crystal substrate, but is not limited thereto.

在一个实施例中,所述同质外延结构为半导体发光器件结构,其中所述半导体功能层包括第一导电类型的半导体层、多量子阱发光层和第二导电类型的半导体层。In one embodiment, the homoepitaxial structure is a semiconductor light-emitting device structure, wherein the semiconductor functional layer comprises a semiconductor layer of a first conductivity type, a multi-quantum well light-emitting layer and a semiconductor layer of a second conductivity type.

在一个实施例中,所述同质外延结构为电子器件结构,其中所述半导体功能层包括高阻层、插入层、沟道层、势垒层、帽层等。In one embodiment, the homoepitaxial structure is an electronic device structure, wherein the semiconductor functional layer includes a high resistance layer, an insertion layer, a channel layer, a barrier layer, a cap layer, and the like.

在一个较为具体的实施方案中,一种基于氮化物单晶衬底的同质外延结构如图1a所示,包括GaN单晶衬底(前述的氮化物半导体单晶衬底),依次生长在所述衬底上的界面弛豫层和翘曲调控层,以及形成于翘曲调控层上的N型GaN区域层、MQWs发光层、p型GaN区域层(前述的半导体功能层)。其中通过界面弛豫层和翘曲调控层实现对N型GaN区域层、MQWs发光层、p型GaN区域层的均匀性调控。In a more specific embodiment, a homoepitaxial structure based on a nitride single crystal substrate is shown in Figure 1a, comprising a GaN single crystal substrate (the aforementioned nitride semiconductor single crystal substrate), an interface relaxation layer and a warpage regulation layer sequentially grown on the substrate, and an N-type GaN regional layer, an MQWs light-emitting layer, and a p-type GaN regional layer (the aforementioned semiconductor functional layer) formed on the warpage regulation layer. The uniformity of the N-type GaN regional layer, the MQWs light-emitting layer, and the p-type GaN regional layer is regulated by the interface relaxation layer and the warpage regulation layer.

在一个较为具体的实施方案中,一种基于氮化物单晶衬底的同质外延结构如图1b所示,包括GaN单晶衬底(前述的氮化物半导体单晶衬底),依次生长在所述衬底上的界面弛豫层和翘曲调控层,以及形成于翘曲调控层上的高阻层、插入层、沟道层、势垒层、帽层(前述的半导体功能层)。In a more specific embodiment, a homoepitaxial structure based on a nitride single crystal substrate is shown in Figure 1b, including a GaN single crystal substrate (the aforementioned nitride semiconductor single crystal substrate), an interface relaxation layer and a warp regulation layer sequentially grown on the substrate, and a high resistance layer, an insertion layer, a channel layer, a barrier layer, and a cap layer (the aforementioned semiconductor functional layer) formed on the warp regulation layer.

以下将结合附图及若干实施例对本申请的技术方案进行更详细的描述,但应当理解,如下实施例仅仅是为了解释和说明该技术方案,但不限制本申请的范围。又及,若非特别说明,如下实施例中所采用的各种原料、反应设备、检测设备及方法等均是本领域已知的。The technical solution of the present application will be described in more detail below in conjunction with the accompanying drawings and several embodiments, but it should be understood that the following embodiments are only for the purpose of explaining and illustrating the technical solution, but do not limit the scope of the present application. In addition, unless otherwise specified, the various raw materials, reaction equipment, detection equipment and methods used in the following embodiments are all known in the art.

常规的GaN单晶衬底在同质外延中易出现凹的现象,因此,实施例以解决衬底GaN单晶衬底凹的现象而采用的均匀性调控方法为例。Conventional GaN single crystal substrates are prone to concavity during homoepitaxial growth. Therefore, the embodiment takes the uniformity control method adopted to solve the concavity phenomenon of the GaN single crystal substrate as an example.

实施例1Example 1

将GaN单晶衬底放入MOCVD外延系统生长GaN同质LED外延片,记为样品A。The GaN single crystal substrate was placed in a MOCVD epitaxial system to grow a GaN homogeneous LED epitaxial wafer, which was recorded as sample A.

首先压强设为70torr,开启氨气,在N2载气的气氛下升温到1100℃,达到平衡后,关闭氨气的同时切入TMAl流量300sccm,持续时间5s,在单晶衬底表面铺约一层金属Al原子。然后重新打开氨气,生长AlN约1min,厚度约2nm。至此完成界面弛豫层的生长。然后在同样条件下,同时通入Al源、Ga源及氮源,进行AlGaN/GaN的超晶格材料生长,其中AlGaN的厚度为3nm,AlGaN中Al元素的含量为50%,GaN的厚度为2nm,周期30个。First, the pressure is set to 70torr, ammonia is turned on, and the temperature is raised to 1100°C in an atmosphere of N2 carrier gas. After reaching equilibrium, the ammonia is turned off and the TMAl flow rate is cut in at 300sccm for 5s, so that a layer of metal Al atoms is laid on the surface of the single crystal substrate. Then the ammonia is turned on again, and AlN is grown for about 1min with a thickness of about 2nm. The growth of the interface relaxation layer is completed. Then, under the same conditions, Al source, Ga source and nitrogen source are introduced at the same time to grow AlGaN/GaN superlattice materials, where the thickness of AlGaN is 3nm, the content of Al element in AlGaN is 50%, the thickness of GaN is 2nm, and there are 30 periods.

完成翘曲调控层后,生长LED外延结构,2μm厚度n型GaN,接着5个周期的InGaN/GaN量子阱,其中InGaN的In元素的含量为15%,厚度3nm,GaN的厚度12nm,然后是200nm厚度的p型GaN。After the warp control layer is completed, the LED epitaxial structure is grown, with 2μm thick n-type GaN, followed by 5 periods of InGaN/GaN quantum wells, where the InGaN has an In element content of 15% and a thickness of 3nm, the GaN has a thickness of 12nm, and then a p-type GaN with a thickness of 200nm.

对比例1Comparative Example 1

方法同实施例1,不同之处在于:GaN单晶衬底不生长界面弛豫层及翘曲调控层,制备的同质GaN外延片记为样品B。The method is the same as Example 1, except that: the GaN single crystal substrate does not grow an interface relaxation layer and a warp regulation layer, and the prepared homogeneous GaN epitaxial wafer is recorded as sample B.

对实施例1和对比例1中的样品A和样品B进行测试,图2-图3为样品A和样品B的光致发光PL测试图谱。可见,常规生长方法(即对比例1中的方案),由于GaN单晶衬底的生长工艺和后续切磨抛的原因,容易晶格弯曲而生长LED时容易出现如样品B波长中间短、整体中心凹陷的情况,在主波长450nm的情况,波长均匀性在4.4nm。而通过本申请实施例1中插入界面弛豫层和翘曲调控层后,GaN同质外延片样品A,在相同的主波长情况下,波长均匀性提高到1.2nm。这是外延片的弯曲变凸的结果,验证了本申请提供的调控方法的有效性。Samples A and B in Example 1 and Comparative Example 1 were tested, and Figures 2-3 are the photoluminescence PL test spectra of Sample A and Sample B. It can be seen that the conventional growth method (i.e., the scheme in Comparative Example 1) is prone to lattice bending due to the growth process and subsequent cutting, grinding and polishing of the GaN single crystal substrate, and when growing LEDs, it is easy to have a situation such as sample B with a short wavelength in the middle and a concave center as a whole. In the case of a main wavelength of 450nm, the wavelength uniformity is 4.4nm. After inserting the interface relaxation layer and the warping control layer in Example 1 of the present application, the wavelength uniformity of GaN homogeneous epitaxial wafer sample A is improved to 1.2nm under the same main wavelength. This is the result of the bending of the epitaxial wafer becoming convex, which verifies the effectiveness of the control method provided in the present application.

对比例2Comparative Example 2

方法同实施例1,不同之处在于:GaN单晶衬底不生长界面弛豫层(即:直接在GaN单晶衬底上依次生长AlGaN/GaN的超晶格材料和LED外延结构),制备的同质GaN外延片记为样品C。The method is the same as Example 1, except that: the GaN single crystal substrate does not grow an interface relaxation layer (ie, the AlGaN/GaN superlattice material and the LED epitaxial structure are grown directly on the GaN single crystal substrate in sequence), and the prepared homogeneous GaN epitaxial wafer is recorded as sample C.

对比例3Comparative Example 3

方法同实施例1,不同之处在于:GaN单晶衬底不生长翘曲调控层(即:直接在GaN单晶衬底上依次生长界面弛豫层和LED外延结构),制备的同质GaN外延片记为样品D。The method is the same as Example 1, except that: the warpage regulation layer is not grown on the GaN single crystal substrate (ie, the interface relaxation layer and the LED epitaxial structure are grown sequentially directly on the GaN single crystal substrate), and the prepared homogeneous GaN epitaxial wafer is recorded as sample D.

实施例2Example 2

方法同实施例1,不同之处在于:在进行翘曲调控层生长时,将Al源、Ga源及氮源交替输入生长腔室,在AlN界面弛豫层上生长AlGaN/GaN的超晶格结构,从而形成翘曲调控层。The method is the same as that in Example 1, except that when the warp control layer is grown, the Al source, Ga source and nitrogen source are alternately input into the growth chamber to grow an AlGaN/GaN superlattice structure on the AlN interface relaxation layer, thereby forming the warp control layer.

具体地将Al源、Ga源及氮源的流量控制降低在200sccm以下,以及将生长腔室内的气压设置为30-70torr,在AlN界面弛豫层上生长AlGaN/GaN的超晶格结构,从而形成翘曲调控层。Specifically, the flow rates of the Al source, Ga source and nitrogen source are controlled to be lower than 200 sccm, and the gas pressure in the growth chamber is set to 30-70 torr, and an AlGaN/GaN superlattice structure is grown on the AlN interface relaxation layer, thereby forming a warp regulation layer.

制备的同质GaN外延片记为样品E。The prepared homogeneous GaN epitaxial wafer is recorded as sample E.

实施例3Example 3

将GaN单晶衬底放入MOCVD外延系统生长GaN同质LED外延片,记为样品F。The GaN single crystal substrate is placed in a MOCVD epitaxial system to grow a GaN homogeneous LED epitaxial wafer, which is recorded as sample F.

首先压强设为50torr,开启氨气,在N2载气的气氛下升温到1100℃,达到平衡后,关闭氨气的同时切入TMAl流量300ccm,持续时间5s,在单晶衬底表面铺约一层金属Al原子。然后重新打开氨气,生长AlN约1min,厚度约2nm。至此完成界面弛豫层的生长。然后在同样条件下,进行AlGaN单层材料生长,其中AlGaN的厚度为3nm,AlGaN中Al元素的含量为10%,GaN的厚度为2nm,周期30个。完成翘曲调控层后,生长LED外延结构,2μm厚度n型GaN,接着5个周期的InGaN/GaN量子阱,其中InGaN的In元素的含量为15%,厚度3nm,GaN的厚度12nm,然后是200nm厚度的p型GaN。First, the pressure is set to 50torr, ammonia is turned on, and the temperature is raised to 1100℃ in an atmosphere of N2 carrier gas. After reaching equilibrium, the ammonia is turned off and the TMAl flow rate is cut in at 300ccm for 5s, and a layer of metal Al atoms is laid on the surface of the single crystal substrate. Then the ammonia is turned on again, and AlN is grown for about 1min with a thickness of about 2nm. The growth of the interface relaxation layer is completed. Then under the same conditions, AlGaN single layer material is grown, where the thickness of AlGaN is 3nm, the content of Al element in AlGaN is 10%, the thickness of GaN is 2nm, and the period is 30. After completing the warp control layer, the LED epitaxial structure is grown, 2μm thick n-type GaN, followed by 5 cycles of InGaN/GaN quantum wells, where the content of InGaN is 15%, the thickness is 3nm, the thickness of GaN is 12nm, and then 200nm thick p-type GaN.

实施例4Example 4

将AlN单晶衬底放入MOCVD外延系统生长AlN同质UV-LED外延片,记为样品G。The AlN single crystal substrate was placed in a MOCVD epitaxial system to grow an AlN homogeneous UV-LED epitaxial wafer, which was recorded as sample G.

首先压强设为30torr,开启氨气,在N2载气的气氛下升温到1100℃,达到平衡后,关闭氨气的同时切入B源流量200ccm,持续时间5s,在单晶衬底表面铺约一层B原子。然后重新打开氨气,生长BN约1min,厚度约2nm。至此完成界面弛豫层的生长。然后在同样条件下,进行BN/AlN的超晶格材料生长,其中BN的厚度为3nm,AlN的厚度为2nm,周期25个。完成翘曲调控层后,生长UV-LED外延结构,2μm厚度n型AlGaN,接着5个周期的AlGaN/GaN量子阱,其中AlGaN的Al元素的含量为50%,厚度3nm,GaN的厚度12nm,然后是200nm厚度的p型AlGaN。First, the pressure is set to 30torr, ammonia is turned on, and the temperature is raised to 1100°C in an atmosphere of N2 carrier gas. After reaching equilibrium, the ammonia is turned off and the B source flow rate is cut in at 200ccm for 5 seconds to spread about a layer of B atoms on the surface of the single crystal substrate. Then the ammonia is turned on again, and BN is grown for about 1 minute with a thickness of about 2nm. The growth of the interface relaxation layer is completed. Then, under the same conditions, the superlattice material of BN/AlN is grown, where the thickness of BN is 3nm, the thickness of AlN is 2nm, and the period is 25. After completing the warp control layer, the UV-LED epitaxial structure is grown, 2μm thick n-type AlGaN, followed by 5 cycles of AlGaN/GaN quantum wells, where the Al content of AlGaN is 50%, the thickness is 3nm, the thickness of GaN is 12nm, and then 200nm thick p-type AlGaN.

利用本领域习知的方式,分别利用实施例1-4以及对比例1-3中的同质外延结构制作LED器件,再对这些器件进行测试如表1所示。LED devices were fabricated using the homoepitaxial structures in Examples 1-4 and Comparative Examples 1-3 in a manner known in the art, and then these devices were tested as shown in Table 1.

表1实施例1-4以及对比例1-3中的同质外延结构制作LED器件的测试结果Table 1 Test results of LED devices made of homoepitaxial structures in Examples 1-4 and Comparative Examples 1-3

最后应说明的是:以上所述仅为本申请的优选实施例而已,并不用于限制本申请,尽管参照前述实施例对本申请进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。Finally, it should be noted that the above is only a preferred embodiment of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims (7)

1.一种基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其特征在于,包括:1. A method for controlling the uniformity of a homoepitaxial structure based on a nitride single crystal substrate, comprising: S1、将氮化物单晶衬底置入生长腔室,并在所述生长腔室内形成保护性气氛,之后将所述衬底温度设置为二元氮化物层的生长温度,再向所述生长腔室内输入第一III族源,以在所述衬底表面沉积一层第一III族元素的原子,形成界面浸润层;其中,所述衬底包括第二III族元素;所述氮化物单晶衬底的厚度在1μm以上;S1, placing a nitride single crystal substrate into a growth chamber, and forming a protective atmosphere in the growth chamber, then setting the substrate temperature to the growth temperature of the binary nitride layer, and then inputting a first group III source into the growth chamber to deposit a layer of atoms of the first group III element on the surface of the substrate to form an interface wetting layer; wherein the substrate includes a second group III element; and the thickness of the nitride single crystal substrate is greater than 1 μm; S2、向所述生长腔室内输入第一III族源和氮源,在所述界面浸润层上生长二元氮化物层,从而形成界面弛豫层;所述界面弛豫层包括二元氮化物层,所述二元氮化物层包括第一III族元素,所述第一III族元素与所述第二III族元素不同,以产生压应力或张应力,从而平衡所述衬底的翘曲;所述界面弛豫层的厚度为1-10nm;S2, inputting a first group III source and a nitrogen source into the growth chamber, growing a binary nitride layer on the interface wetting layer, thereby forming an interface relaxation layer; the interface relaxation layer comprises a binary nitride layer, the binary nitride layer comprises a first group III element, the first group III element is different from the second group III element, so as to generate compressive stress or tensile stress, thereby balancing the warping of the substrate; the thickness of the interface relaxation layer is 1-10nm; S3、向所述生长腔室内输入第一III族源、第二III族源及氮源,在所述界面弛豫层上生长三元氮化物层或包含三元氮化物层的超晶格结构,从而形成翘曲调控层;所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构,所述三元氮化物层包括第一III族元素和第二III族元素;所述三元氮化物层的厚度为10nm-100nm,所述包含所述三元氮化物层组成的超晶格结构的厚度为10nm-200nm;S3, inputting a first group III source, a second group III source and a nitrogen source into the growth chamber, growing a ternary nitride layer or a superlattice structure including the ternary nitride layer on the interface relaxation layer, thereby forming a warp regulation layer; the surface of the warp regulation layer is flat, the warp regulation layer includes a ternary nitride layer or a superlattice structure including the ternary nitride layer, the ternary nitride layer includes a first group III element and a second group III element; the thickness of the ternary nitride layer is 10nm-100nm, and the thickness of the superlattice structure including the ternary nitride layer is 10nm-200nm; S4、在所述翘曲调控层上生长半导体功能层;S4, growing a semiconductor functional layer on the warpage regulating layer; 其中,所述氮化物单晶衬底为AlN单晶衬底,所述二元氮化物层为BN层,所述三元氮化物层为BxAl1-xN层,所述包含三元氮化物层的超晶格结构为BxAl1-xN/AlN超晶格结构,0<x<1。The nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a BN layer, the ternary nitride layer is a BxAl1 -xN layer, the superlattice structure including the ternary nitride layer is a BxAl1 -xN /AlN superlattice structure, and 0<x<1. 2.根据权利要求1所述的基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其特征在于:所述二元氮化物层的组成材料的晶格常数大于所述氮化物单晶衬底的组成材料的晶格常数,以产生张应力;或者,所述二元氮化物层的组成材料的晶格常数小于所述氮化物单晶衬底的组成材料的晶格常数,以产生压应力。2. The uniformity control method of the homoepitaxial structure based on the nitride single crystal substrate according to claim 1 is characterized in that: the lattice constant of the constituent material of the binary nitride layer is greater than the lattice constant of the constituent material of the nitride single crystal substrate to generate tensile stress; or, the lattice constant of the constituent material of the binary nitride layer is less than the lattice constant of the constituent material of the nitride single crystal substrate to generate compressive stress. 3.根据权利要求1所述的基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其特征在于:所述氮化物单晶衬底的厚度为1-2.5μm。3. The method for controlling the uniformity of a homoepitaxial structure based on a nitride single crystal substrate according to claim 1, wherein the thickness of the nitride single crystal substrate is 1-2.5 μm. 4.根据权利要求1所述的基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其特征在于,步骤S3具体包括:将所述第一III族源、第二III族源及氮源交替输入所述生长腔室,在所述界面弛豫层上生长超晶格结构,从而形成所述翘曲调控层。4. The uniformity control method of the homoepitaxial structure based on the nitride single crystal substrate according to claim 1 is characterized in that step S3 specifically comprises: alternately inputting the first Group III source, the second Group III source and the nitrogen source into the growth chamber, growing a superlattice structure on the interface relaxation layer, thereby forming the warp control layer. 5.根据权利要求1所述的基于氮化物单晶衬底的同质外延结构的均匀性调控方法,其特征在于,步骤S3具体包括:向所述生长腔室内输入第一III族源、第二III族源及氮源,并将所述第一III族源、第二III族源及氮源的流量控制在200sccm以下,以及将所述生长腔室内的气压设置为30-70torr,在所述界面弛豫层上生长超晶格结构,从而形成所述翘曲调控层。5. The uniformity control method of the homoepitaxial structure based on the nitride single crystal substrate according to claim 1 is characterized in that step S3 specifically includes: inputting a first Group III source, a second Group III source and a nitrogen source into the growth chamber, and controlling the flow rates of the first Group III source, the second Group III source and the nitrogen source to be below 200 sccm, and setting the gas pressure in the growth chamber to 30-70 torr, growing a superlattice structure on the interface relaxation layer, thereby forming the warp control layer. 6.一种基于氮化物单晶衬底的同质外延结构,其特征在于,包括:6. A homoepitaxial structure based on a nitride single crystal substrate, characterized by comprising: 氮化物单晶衬底,所述氮化物单晶衬底的厚度在1μm以上;A nitride single crystal substrate, wherein the thickness of the nitride single crystal substrate is greater than 1 μm; 界面弛豫层,其生长在所述衬底上,所述界面弛豫层包括二元氮化物层,所述二元氮化物层的组成材料与所述衬底的组成材料晶格失配,以产生压应力或张应力,从而平衡所述衬底的翘曲;所述界面弛豫层的厚度为1-10nm;An interface relaxation layer grown on the substrate, the interface relaxation layer comprising a binary nitride layer, the constituent material of the binary nitride layer being lattice mismatched with the constituent material of the substrate to generate compressive stress or tensile stress, thereby balancing the warping of the substrate; the thickness of the interface relaxation layer is 1-10 nm; 翘曲调控层,其生长在所述界面弛豫层上,所述翘曲调控层表面平整,所述翘曲调控层包括三元氮化物层或包含三元氮化物层的超晶格结构;所述三元氮化物层的厚度为10nm-100nm,所述包含所述三元氮化物层组成的超晶格结构的厚度为10nm-200nm;A warp regulation layer, which is grown on the interface relaxation layer, the surface of the warp regulation layer is flat, the warp regulation layer comprises a ternary nitride layer or a superlattice structure comprising the ternary nitride layer; the thickness of the ternary nitride layer is 10nm-100nm, and the thickness of the superlattice structure comprising the ternary nitride layer is 10nm-200nm; 半导体功能层,其生长在所述翘曲调控层上;A semiconductor functional layer grown on the warp regulation layer; 其中,所述氮化物单晶衬底为AlN单晶衬底,所述二元氮化物层为BN层,所述三元氮化物层为BxAl1-xN层,所述包含三元氮化物层的超晶格结构为BxAl1-xN/AlN超晶格结构,0<x<1。The nitride single crystal substrate is an AlN single crystal substrate, the binary nitride layer is a BN layer, the ternary nitride layer is a BxAl1 -xN layer, the superlattice structure including the ternary nitride layer is a BxAl1 -xN /AlN superlattice structure, and 0<x<1. 7.根据权利要求6所述的基于氮化物单晶衬底的同质外延结构,其特征在于,所述二元氮化物层的组成材料的晶格常数大于所述衬底的组成材料的晶格常数,以产生张应力;或者,所述二元氮化物层的组成材料的晶格常数小于所述衬底的组成材料的晶格常数,以产生压应力。7. The homoepitaxial structure based on a nitride single crystal substrate according to claim 6 is characterized in that the lattice constant of the constituent material of the binary nitride layer is greater than the lattice constant of the constituent material of the substrate to generate tensile stress; or, the lattice constant of the constituent material of the binary nitride layer is smaller than the lattice constant of the constituent material of the substrate to generate compressive stress.
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