Understanding the Correlation between Ga Speciation and Propane Dehydrogenation Activity on Ga/H-ZSM-5 Catalysts

Yuan, Yong; Brady, Casper; Lobo, Raul F.; Xu, Bingjun

doi:10.1021/acscatal.1c01497

Focused Ga + ion milling of lightly Si-doped, n-type Ga 2 O 3 was performed with 2–30 kV ions at normal incidence and beam currents that were a function of beam voltage, 65 nA for 30 kV, 26 nA for 10 kV, 13 nA for 5 kV, and 7.1 nA for 2 kV, to keep the milling depth constant at 100 nm. Approximate milling rates were 15, 6, 2.75, and 1.5 μm 3 /s for 30, 10, 5, and 2 kV, respectively. The electrical effects of the ion damage were characterized by Schottky barrier height and diode ideality factor on vertical rectifier structures comprising 10 μm epitaxial n-Ga 2 O 3 on n + Ga 2 O 3 substrates, while the structural damage was imaged by transmission electron microscopy. The reverse bias leakage was largely unaffected even by milling at 30 kV beam energy, while the forward current-voltage characteristics showed significant deterioration at 5 kV, with an increase in the ideality factor from 1.25 to 2.25. The I–V characteristics no longer showed rectification for the 30 kV condition. Subsequent annealing up to 400 °C produced substantial recovery of the I–V characteristics for all beam energies and was sufficient to restore the initial ideality factor completely for beam energies up to 5 kV. Even the 30 kV-exposed rectifiers showed a recovery of the ideality factor to 1.8. The surface morphology of the ion-milled Ga 2 O 3 was smooth even at 30 kV ion energy, with no evidence for preferential sputtering of the oxygen. The surface region was not amorphized by extended ion milling (35 min) at 5 kV with the samples held at 25 °C, as determined by electron diffraction patterns, and significant recovery of the lattice order was observed after annealing at 400 °C.

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