Characterization of ZrB2(0 0 0 1) surface prepared by ex situ HF solution treatment toward applications as a substrate for GaN growth

ZrB₂(0 0 0 1) crystals grown by the rf-floating zone technique were characterized by X-ray photoelectron spectroscopy, reflection high-energy electron diffraction, and atomic force microscopy. These characteristics were investigated as a function of thermal cleaning temperature up to 1000 °C in vacuum for as-received substrates as well as substrates treated ex situ in HF aqueous solution. The HF treatment process removed the ZrO₂ native oxide layer present on as-received substrates and resulted in ZrB₂(0 0 0 1) surfaces exhibiting long-range order. Upon annealing the HF-treated surface in high vacuum, two types of reconstructions were observed: an incommensurate reconstruction from 650 to 900 °C related to residual H₂ gas, and n × n reconstructions at 1000 °C, possibly related to oxygen.