MOCVD生长AlN单晶薄膜的气相和表面化学反应综述

doi:10.11949/0438-1157.20230380

摘要/Abstract

摘要：

作为第三代半导体材料的代表，AlN单晶具有禁带宽度大、击穿电场强度高、电子饱和迁移率高等特点，被广泛应用于紫外和深紫外发光器件的制造。金属有机化学气相沉积(MOCVD)是生长AlN单晶薄膜最主要的技术。由于Al—N键在三种Ⅲ族氮化物(AlN、GaN和InN)中最强，导致MOCVD生长AlN过程的气相寄生反应最为严重，进而造成AlN的生长速率和效率过低、生长窗口过窄等问题。此外，较高的Al—N键能还导致含Al粒子在表面的迁移率过低，致使薄膜表面形貌变差。这些问题都与薄膜生长过程发生的化学反应密切相关。分别从气相反应路径和表面反应机理两方面，较全面地总结了前人针对MOCVD生长AlN薄膜机理开展的研究工作，并介绍了本课题组近年来在该方向取得的研究成果。最后归纳了现阶段MOCVD生长AlN研究中存在的问题与不足，并在此基础上进行了展望。

关键词: AlN, MOCVD, 化学反应, 自由基, 计算流体力学, 计算化学

Abstract:

As a representative of the third-generation semiconductor materials, AlN single crystal has the characteristics of large band gap, high breakdown electric field strength, and high electron saturation mobility, and is widely used in the manufacture of ultraviolet and deep ultraviolet light-emitting devices. Metal organic chemical vapor deposition (MOCVD) is the main technique in the manufacture of AlN thin films. Due to the highest binding energy of Al—N among the group Ⅲ-nitrides (AlN, GaN and InN), severe parasitic reactions occur in AlN MOCVD, which results in the low growth rate, low growth efficiency and very narrow growth window. Besides, the high Al—N binding energy results in the low mobility of Al-containing particles on the surface and consequently deteriorating the surface morphology. The above problems are all related with chemical reactions in AlN MOCVD. In this article, we summarize comprehensively previous research work on the MOCVD growth of AlN thin films from two aspects: gas-phase reactions and surface reactions, and introduce some research work by our team in recent years. Finally, the problems and shortcomings in the current research on MOCVD growth of AlN are summarized, and some further researches are prospected.

Key words: AlN, MOCVD, chemical reaction, radical, computational fluid dynamics, computational chemistry

中图分类号:

O 649.2

何晓崐, 刘锐, 薛园, 左然. MOCVD生长AlN单晶薄膜的气相和表面化学反应综述[J]. 化工学报, 2023, 74(7): 2800-2813.

Xiaokun HE, Rui LIU, Yuan XUE, Ran ZUO. Review of gas phase and surface reactions in AlN MOCVD[J]. CIESC Journal, 2023, 74(7): 2800-2813.

图/表 10

图1 深紫外LED的InAlGaN异质结示意图和TEM断面图[3]

Fig.1 Schematics of InAlGaN heterojunction and TEM cross section of deep UV LED[3]

图2 (a) 传统的MOCVD方法；(b) MEMOCVD方法：在传统低温形核层上生长高温AlN，TMAl和NH3交替供应，以增强表面迁移率；（c）侧向外延方法：晶体从未修饰的蓝宝石坑槽向上生长，然后横向生长，覆盖修饰区域，横向生长抑制了位错的蔓延[24]

Fig.2 (a) Conventional MOCVD; (b) Process of MEMOCVD: High-temperature AlN layer is grown on the low-temperature AlN nucleation layer with an alternative supply of TMAl and NH3 for alleviating the low surface mobility of Al atoms; (c) Process of nano-scale lateral overgrowth: Crystals grow upward from unmodified sapphire pit grooves and then laterally, covering the modified region and the spread of dislocations is suppressed[24]

表1 AlN-MOCVD气相反应机理的研究方法

Table 1 Methods for studying the gas phase reaction mechanism of AlN-MOCVD

方法	优点	缺点	文献
实验测量	可获知气相物质种类和浓度；获得生长速率及其与压力、温度、反应器结构等之间的关系	价格昂贵，无法针对各种不同的实验条件分别进行观测，无法直接观测到化学反应中间过程以及反应过渡态	[25-28,31,40-41]
CFD仿真	结合反应动力学，可模拟不同反应器内、不同操作条件下的生长过程，获得生长速率与温度、压力之间的关系；可直观显示不同反应物质的浓度分布	反应动力学数据，如速率常数、指前因子、气相物质的物化性质等需通过实验测量或量化计算获得；需要将真实环境进行适当简化	[29-30,32,37-38,42]
量化计算	可以在分子水平上预测化学反应，获得分子构型和能量，确定反应势能面和过渡态，判断反应发生的概率，获得反应动力学数据，如活化能、指前因子等	无法获知反应器各部位的温度和压强，因此无法预测实际生长中反应是否发生和反应速率大小，无法建立反应速率与温度、压强、浓度的关系	[33-36,39,43-44]

图3 MOCVD生长AlN的三条气相反应路径（从TMAl开始的三条路径）[30]

Fig.3 Schematic of reaction pathways for AlN-MOCVD[30]

图4 TMAl与NH3气相反应中主要分子的优化结构示意图[44]

Fig.4 Optimized molecular structures of major gas species in the gas phase reaction of TMAl with NH3[44]

图5 AlN-MOCVD生长的主要气相反应路径示意图[44]

Fig.5 Schematic diagram of the main gas reaction path in AlN MOCVD[44]

图6 激光散射和原位TEM观测到的衬底上方约6 mm处的纳米粒子层[31]

Fig.6 The nanoparticle layer about 6 mm above the substrate observed by laser scattering and in situ TEM[31]

图7 衬底上粒子的吸附、迁移、并入晶格、脱附示意图[58]

Fig.7 Schematic of adsorption, migration, lattice incorporation and desorption of particles on the substrate[58]

图8 AlN(0001)重构面的顶视图[67]

Fig.8 Top view of proposed models for reconstructed surface of AlN(0001)[67]

图9 DMAlNH2在理想AlN(0001)-Al面上的吸附(虚线表示与表面原子之间成键；短划线表示吸附质分子内可能断裂的键)[83]

Fig.9 Adsorption structures of DMAlNH2 on the ideal AlN(0001)-Al terminated surface (the dotted line indicates the bond with surface atom, the dashed line indicates the possible broken bond in the adsorbate)[83]

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