Metal organic chemical vapor deposition (MOCVD) and molecular beam epitaxy (MBE) are two versatile growth techniques that can readily produce multilayer structures with atomic-level precision control, which have found broad applications in technology. However, compared to MBE, MOCVD growth involves the surface reaction of metal-organic precursor compounds, which changes during film deposition. Consequently, a thorough investigation on the chemical profile layer-by-layer is critical for optimizing MOCVD film performance. Here, we examine Sb segregation in an MOCVD-grown InAs/InAs1−xSbx superlattice by analyzing composition and lattice strain at atomic resolution using scanning transmission electron microscopy and compare with the previously reported MBE growth results. Our findings show a different Sb profile along the growth direction in MOCVD, with the segregation coefficient being higher at the InAsSb-on-InAs interface (0.807 ± 0.021) than at the InAs-on-InAsSb interface (0.695 ± 0.009), giving rise to asymmetric composition and lattice strain profiles unlike those obtained with MBE. Furthermore, we obtain direct evidence of Sb clusters with size of ∼1–3 nm and Sb ordering within the InAs1−xSbx layer, which is largely absent in the reported MBE growth. These findings demonstrate the concurrent interplay between surface segregation, surface reconstruction, and surface reaction that is unique to MOCVD growth with broad implications on preparing Sb-containing quantum materials.

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