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III-V族氮化物半导体通常采用金属有机气相外延（MOCVD）方法进行生长，但其复杂的生长动力学及缺陷控制问题仍是制备高质量材料所面临的核心挑战。尤其对于GaN基材料，系统揭示其晶体结构演化规律及外延生长机制，对提升材料质量和器件性能具有重要的科学意义和应用价值。近年来，原位X射线表征技术的快速发展，使研究人员能够实现对外延生长过程的实时监测，深入解析氮化物材料表界面结构的演化过程，从而为材料结构与性能的精准调控提供了可能。借助具有高时空分辨率的同步辐射光源，原位X射线技术已成为研究氮化物生长动力学的重要手段。本文系统回顾了近年来国际上在氮化物半导体原位X射线研究方面的最新进展，重点介绍了原位MOCVD生长系统的构建、原位X射线表征方法的发展与应用，以及外延过程中表界面结构演化的实时观测与动力学分析。最后，结合当前研究热点与挑战，对该领域未来的发展方向进行了展望。Metal-organic chemical vapor deposition (MOCVD) remains the dominant technique for the growth of III-nitride semiconductors; however, the complex growth kinetics and defect formation mechanisms continue to limit the achievable material quality and device performance. In recent years, the rapid advancement of in situ X-ray characterization techniques—particularly those enabled by high-brightness synchrotron radiation—has provided unprecedented opportunities for probing real-time structural evolution during nitride epitaxy. This review summarizes the latest international progress in in situ X-ray studies of III-nitride MOCVD growth, with emphasis on the development of in situ MOCVD growth platforms, emerging X-ray methodologies, and their applications in monitoring surface and interfacial dynamics.
We present the principles and implementation of in situ X-ray reflectivity (XRR), crystal truncation rods (CTR), grazing-incidence diffraction, and microbeam/coherent scattering techniques（XPCS） in nitride epitaxy. Using representative case studies from GaN and InGaN, we discuss how these tools reveal key dynamical processes—including early-stage nucleation, strain relaxation, step-flow behavior, alloy segregation, and interface roughening—under realistic growth conditions. Special attention is given to transient non-equilibrium phenomena such as compositional fluctuations and interface reconstruction in high-In content alloys, which remain inaccessible to conventional in situ probes.
Furthermore, we highlight emerging trends enabled by next-generation synchrotron sources, including millisecond- to microsecond-resolved measurements, nanoscale spatial mapping, and in situ coherent X-ray diffraction imaging (CXDI/XPCS). These capabilities are expected to provide direct atomic-to-mesoscale insights into island nucleation, step dynamics, defect evolution, and strain-composition coupling in complex heterostructures. Finally, we outline future research directions, such as integrating data-driven structure inversion, multi-scale modeling, and closed-loop “growth-measurement-feedback” control to accelerate the understanding and optimization of nitride epitaxy.
This review demonstrates that in situ X-ray techniques have become a powerful and indispensable bridge between microscopic structural evolution and macroscopic device performance, and will play a key role in enabling precise, controllable epitaxy of next-generation wide-bandgap semiconductor materials.-
Keywords:
- Epitaxial growth by MOCVD /
- In situ X-ray characterization /
- growth kinetics of Surface and interface /
- Synchrotron radiation X-rays
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