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We report the detailed mechanism behind the β to γ phase transformation in Sn-doped and Si-implanted Ga2O3 that we determined based on the direct observation of the atomic scale structure using scanning transmission electron microscopy (STEM). Quantitative analysis of the STEM images revealed that the high concentration of impurity atoms favored the formation of interstitial–divacancy complexes, which then leads to the secondary relaxation that creates additional interstitial atoms and cation vacancies, resulting in a local structure that closely resembles γ-Ga2O3. We explain the mechanism of how the impurity atoms facilitate the transformation, as well as the detailed sequence of the local γ phase transformation. The findings here offer an insight on how the lattice respond to the external stimuli, such as doping and strain, and transform into different structures, which is important for advancing Ga2O3 but also a variety of low symmetry crystals and oxides with multiple polymorphs. 

Growths of monoclinic (Al_xGa_1−x)₂O₃thin films up to 99% Al contents are demonstrated via metalorganic chemical vapor deposition (MOCVD) using trimethylgallium (TMGa) as the Ga precursor. The utilization of TMGa, rather than triethylgallium, enables a significant improvement of the growth rates (>2.5 μm h⁻¹) of β‐(Al_xGa_1−x)₂O₃thin films on (010), (100), and (01) β‐Ga₂O₃substrates. By systematically tuning the precursor molar flow rates, growth of coherently strained phase pure β‐(Al_xGa_1−x)₂O₃films is demonstrated by comprehensive material characterizations via high‐resolution X‐ray diffraction (XRD) and atomic‐resolution scanning transmission electron microscopy (STEM) imaging. Monoclinic (Al_xGa_1−x)₂O₃films with Al contents up to 99, 29, and 16% are achieved on (100), (010), and (01) β‐Ga₂O₃substrates, respectively. Beyond 29% of Al incorporation, the (010) (Al_xGa_1−x)₂O₃films exhibit β‐ to γ‐phase segregation. β‐(Al_xGa_1−x)₂O₃films grown on (01) β‐Ga₂O₃show local segregation of Al along (100) plane. Record‐high Al incorporations up to 99% in monoclinic (Al_xGa_1−x)₂O₃grown on (100) Ga₂O₃are confirmed from XRD, STEM, electron nanodiffraction, and X‐ray photoelectron spectroscopy measurements. These results indicate great promises of MOCVD development of β‐(Al_xGa_1−x)₂O₃films and heterostructures with high Al content and growth rates using TMGa for next‐generation high‐power and high‐frequency electronic devices.