CN105489723B - 氮化物底层及其制作方法 - Google Patents
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- 239000000463 material Substances 0.000 description 7
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Abstract
本发明提供了一种氮化物底层的制作方法，采用PVD溅射AlN层时同时掺少量非Al物质以形成分解温度低于AlN的氮化物，然后进行高温下退火，经过退火后的AlN层不再是平整表面，而是在微观上呈现高低起伏，在这种表面上继续采用MOCVD生长AlGaN能通过三维到二维之间的模式转换释放应力，从而改善AlN裂纹。
Description
技术领域
本发明涉及半导体制备领域，具体为一种可以改善表面裂纹的氮化物底层结构及其制作方法。
背景技术
深紫外AlGaN发光二极管在杀菌消毒、医疗、生化检测、高密度信息存储、白光照明和保密通信等领域具有巨大的潜在应用价值和前景，受到越来越多研究人员和机构的重视。然而AlGaN与常用衬底之间失配很大，导致当前深紫外LED的发光效率普遍较低，使用AlN作为缓冲层，获得高晶体质量无裂纹的AlN薄膜，成为提高深紫外LED的发光效率关键技术。
越来越多的试验结果证实，在蓝宝石衬底上使用溅射式(Sputter) AlN 材料作为进一步生长氮化物薄膜的缓冲层，可以得到高品质的底层材料，并且对于发光二极管的光输出功率有较大的提升。例如，在蓝宝石衬底上溅射AlN层作为缓冲层，再采用MOCVD生长AlN薄膜于该溅射式AlN缓冲层上，可以大幅降低XRD (102) 衍射半波宽。然而，溅射式 AlN缓冲层表面非常平整，不会形成不连续的薄膜表面，无法提供应力释放的路径，导致表面裂纹严重。
发明内容
为了解决氮化物薄膜生长在溅射式AlN缓冲层上会出现表面裂纹严重的问题，本发明提供了一种氮化物底层的制作方法，采用PVD溅射AlN层时同时掺少量Ga、In等非Al物质，以形成分解温度低于AlN的氮化物，镀完AlN后进行高温下退火，经过退火后的AlN层不再是平整表面，而是在微观上呈现高低起伏，在这种表面上继续采用MOCVD生长AlGaN能通过三维到二维之间的模式转换释放应力，从而改善AlN裂纹。
本发明的技术方案为：氮化物底层的制作方法，包括步骤：1）提供衬底；2）在所述衬底的表面上溅射AlN层：在溅射过程中加入Al源的同时掺入非Al物质，从而形成分解温度低于AlN的氮化物；3）对所述AlN层进行退火处理，形成粗糙的表面；4）采用MOCVD 法在所述AlN 层表面沉积AlxGa1-xN层（0 ≤x≤1）。
进一步地，所述非Al物质在退火过程中脱附，形成粗糙的表面。
优选地，所述步骤2）中的非Al物质为In、Ga或其组合。
优选地，所述掺入的非Al物质的不超过Al源的10%。
优选地，所述步骤3）的预设温度为600~2000℃。
优选地，所述步骤4）中采用MOCVD生长的AlxGa1-xN层在所述粗糙表面上通过三维到二维之间的模式转换释放应力。
本发明同时提供了一种发光二极管制作方法，包括步骤：1）提供衬底；2）在所述衬底的表面上溅射AlN层：在溅射过程中加入Al源的同时掺入非Al物质，从而形成分解温度低于AlN的氮化物；3）对所述AlN层进行退火处理，形成粗糙的表面；4）采用MOCVD 法在所述AlN 层表面沉积AlxGa1-xN层（0 ≤x≤1）；5）在所述AlxGa1-xN层上沉积n型氮化物层、有源层和p型氮化物层。
优选地，所述有源层的发光波长为365nm~210nm。
前述方法制备获得的氮化物底层结构可应用于发光二极管，特别是深紫外发光二极管。采用前述制作方法可以获得高晶格质量且无裂纹的AlN底层，然后再进行各外延材料层的生长，从而获得高发光效率的发光二极管。
本发明的其它特征和优点将在随后的说明书中阐述，并且，部分地从说明书中变得显而易见，或者通过实施本发明而了解。本发明的目的和其他优点可通过在说明书、权利要求书以及附图中所特别指出的结构来实现和获得。
附图说明
附图用来提供对本发明的进一步理解，并且构成说明书的一部分，与本发明的实施例一起用于解释本发明，并不构成对本发明的限制。此外，附图数据是描述概要，不是按比例绘制。
图1为根据本发明实施的一种氮化物底层的制作方法流程图。
图2为根据本发明实施的一种氮化物底层结构示意图。
图3为根据本发明实施的一种氮化物发光二极管示意图。
具体实施方式
以下将结合附图及实施例来详细说明本发明的实施方式，借此对本发明如何应用技术手段来解决技术问题，并达成技术效果的实现过程能充分理解并据以实施。需要说明的是，只要不构成冲突，本发明中的各个实施例以及各实施例中的各个特征可以相互结合，所形成的技术方案均在本发明的保护范围之内。
实施例1
参看图1，根据本发明实施的一种氮化物底层的制作方法，包括步骤S11~14，下面进行详细说明。
首先，提供衬底110，衬底的选取包括但不限于蓝宝石、氮化铝、氮化镓、硅、碳化硅，其表面结构可为平面结构或图案化图结构。在本实施例中，采用蓝宝石平片衬底。
接着，将衬底110置入PVD腔室，调节腔室温度为300～600℃，压力为2～10mtorr，利用PVD 法沉积厚度为10～350nm的AlN膜层120，在沉积过程中掺入少量的Ga金属，其量少于Al金属的10%，从而在AlN膜层中夹杂形成少量的GaN。
沉积结束后将镀有AlN 膜层120 的衬底进行高温退火处理，其退火温度为1100~2000℃。由于Ga组分在温度高于1077℃时会发生严重的脱附现象，因此通过退火处理的AlN膜层120不再是平整表面，而是在微观上呈现高低起伏，即为粗糙表面。在本实施例中，优选退火温度为1080~1200℃。
接着，将镀有AlN 膜层2 的衬底转入CVD 腔室，并调节腔室温度为400～ 600℃，通入金属源、NH3、H2 外延生长AlxGa1-xN层3（0 ≤ x≤1），该层厚度为1～100nm，覆盖于衬底表面，图2显示了生长AlxGa1-xN层3后结构示意图。在此过程中，利用Al原子表面迁移能力不强，MOCVD生长AlxGa1-xN时, Al原子会优先在高低起伏形成的小岛聚集，小岛会逐渐变成大岛，当岛面积变大，相邻两个岛或多个岛会相遇并相互合并，合并过程包含岛变大、相互挤压、逐渐变厚等过程，挤压形成的压应力会抵消部分薄膜与衬底之间由于失配导致的张应力，使张应力变小，从而改善AlN层的裂纹。
在上述方法中，保留了PVD镀AlN膜提升MOCVD生长AlN晶体质量的优点，同时通过引入微观粗化的方法达到改善薄膜应力，解决裂纹的问题。
图3显示了一种生长于上述氮化物底层结构100上的LED结构，至少还包括n型半导体层200、有源层300和p型半导体层400。一般，AlN材料层可允许实现低至约200 纳米波长的光发射，特别适用于进行深紫外LED生长。在该实施例中，氮化物底层结构100的AlxIn1-x- yGayN层140选用AlN材料，n型半导体层200、有源层300和p型半导体层400形成于AlN底层100上，采用AlGaN材料，可实现波长为210~365nm的高品质紫外LED。
实施例2
区别于实施例1，在本实施例在PVD溅射AlN膜层120时同时溅射少量In金属，从而在AlN膜层中夹杂形成少量InN材料，将PVD溅射的AlN膜层120在高温下退火形成微粗的表面。由于InN材料在800℃左右即可分解，因此本实施例中控制温度为800~1000℃进行退火。
很明显地，本发明的说明不应理解为仅仅限制在上述实施例，而是包括利用本发明构思的所有可能的实施方式。
Claims (11)
1.氮化物底层的制作方法，包括步骤：
1）提供衬底；
2）在所述衬底的表面上溅射AlN层：在溅射过程中加入Al源的同时掺入非Al物质，以形成分解温度低于AlN的氮化物；
3）对所述AlN层进行退火处理，其退火温度高于形成的氮化物的分解温度使得该氮化物分解，形成粗糙的表面；
4）采用MOCVD 法在所述AlN 层表面沉积AlxGa1-xN层，其中0 ≤x≤1。
2.根据权利要求1所述的氮化物底层的制作方法，其特征在于：所述非Al物质在退火过程中脱附，形成粗糙的表面。
3.根据权利要求1所述的氮化物底层的制作方法，其特征在于：所述步骤2）中的非Al物质为In、Ga或其组合。
4.根据权利要求1所述的氮化物底层的制作方法，其特征在于：所述掺入的非Al物质的摩尔量不超过Al源的10%。
5.根据权利要求1所述的氮化物底层的制作方法，其特征在于：所述步骤3）的退火温度为600~2000℃。
6.根据权利要求1所述的氮化物底层的制作方法，其特征在于：所述步骤4）中采用MOCVD生长的AlxGa1-xN层在所述粗糙表面上通过三维到二维之间的模式转换释放应力。
7.氮化物底层结构，采用上述权利要求1~6中的任一项氮化物底层的制作方法制得。
8.发光二极管制作方法，包括步骤：
1）提供衬底；
2）在所述衬底的表面上溅射AlN层：在溅射过程中加入Al源的同时掺入非Al物质，从而形成分解温度低于AlN的氮化物；
3）对所述AlN层进行退火处理，其退火温度高于形成的氮化物的分解温度使得该氮化物分解，形成粗糙的表面；
4）采用MOCVD 法在所述AlN 层表面沉积AlxGa1-xN层，其中0 ≤ x<1；
5）在所述AlxGa1-xN层上沉积n型氮化物层、有源层和p型氮化物层。
9.根据权利要求8所述的发光二极管的制作方法，其特征在于：所述有源层的发光波长为365nm~210nm。
10.根据权利要求8所述的发光二极管的制作方法，其特征在于：所述步骤2）中的非Al物质为In、Ga或其组合。
11.根据权利要求8所述的发光二极管的制作方法，其特征在于：所述步骤4）中采用MOCVD生长的AlxGa1-xN层在所述粗糙表面上通过三维到二维之间的模式转换释放应力。
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