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Phase and microstructural evolution of gallium oxide (Ga2O3) films grown on vicinal (0001) sapphire substrates was investigated using a suite of analytical tools. High-resolution transmission electron microscopy and scanning transmission electron microscopy of a film grown at 530 °C revealed the initial pseudomorphic growth of three to four monolayers of α-Ga2O3, a 20–60 nm transition layer that contained both β- and γ-Ga2O3, and a top ∼700 nm-thick layer of phase-pure κ-Ga2O3. Explanations for the occurrence of these phases and their sequence of formation are presented. Additional growths of Ga2O3 films in tandem with x-ray diffraction and scanning electron microscopy investigations revealed that the top layer varied in phase composition between ∼100% κ-Ga2O3 and ∼100% β-Ga2O3; the surface microstructure ranged from poorly coalesced to completely coalesced grains as a function of growth temperature, growth rate, or diluent gas flow rate. In general, it was found that the κ-phase is favored at lower growth temperatures and higher triethylgallium flow rates (low VI/III ratios). The growth of nominally single-phase κ-Ga2O3 within the top layer was observed in a temperature range between 500 and 530 °C. Below 470 °C, only amorphous Ga2O3 was obtained; above 570 °C, only the β-phase was deposited. [ABSTRACT FROM AUTHOR]

Atomic resolution scanning/transmission electron microscopy (S/TEM) and energy-dispersive x-ray (EDX) analysis were used to determine the effects of annealing at 800–1000 °C in air on Ga2O3 films grown on (100) MgAl2O4 at 650 °C via metal-organic chemical vapor deposition. Annealing resulted in the diffusion of Mg and Al into the films concomitantly with the transformation of β-Ga2O3 to γ-Ga2O3 solid solutions. The minimum atomic percent of Al + Mg that corresponded with the transformation was ∼4.6 at. %. Analyses of atomic-scale STEM images and EDX profiles revealed that the Al and Mg atoms in the γ-Ga2O3 solid solutions occupied octahedral sites; whereas the Ga atoms occupied tetrahedral sites. These site preferences may account for the stabilization of the γ-Ga2O3 solid solutions. [ABSTRACT FROM AUTHOR]

Ga2O3 films were deposited on (100) MgAl2O4 spinel substrates at 550, 650, 750, and 850 ° C using metal-organic chemical vapor deposition and investigated using x-ray diffraction and transmission electron microscopy. A phase-pure γ-Ga2O3-based material having an inverse spinel structure was formed at 850 °C; a mixture of the γ-phase and β-Ga2O3 was detected in films grown at 750 ° C. Only β-Ga2O3 was determined in the films deposited at 650 and 550 ° C. A β- to γ-phase transition occurred from the substrate/film interface during growth at 750 ° C. The growth and stabilization of the γ-phase at the outset of film growth at 850 ° C was affected by the substantial Mg and Al chemical interdiffusion from the MgAl2O4 substrate observed in the energy-dispersive x-ray spectrum. Atomic-scale investigations via scanning transmission electron microscopy of the films grown at 750 and 850 ° C revealed a strong tetrahedral site preference for Ga and an octahedral site preference for Mg and Al. It is postulated that the occupation of these atoms in these particular sites drives the β-Ga2O3 to γ-phase transition and markedly enhances the thermal stability of the latter phase at elevated temperatures. [ABSTRACT FROM AUTHOR]