Nanowire
heterostructures of the oxide (shell)–semiconducting
(core) type are of interest for various applications in energy harvesting,
such as electrodes for photocatalysis and in sensors. Their complete
synthesis often requires the deposition of the shell and the core
in two separate reactors, with the risk of exposing the core to oxidation
from atmospheric conditions during transfer. Here, we study the desorption
mechanisms and protection efficiency of an arsenic shell, which was
purposely deposited on the GaAs core for protection against undesirable
oxidation. Using in situ heating in transmission
electron microscopy and synchrotron radiation scanning photoelectron
microscopy, we explore the morphology, structure, and surface chemistry
of GaAs nanowires capped with an arsenic shell, from room temperature
to 500 °C. A phase transformation from amorphous to polycrystalline
arsenic is evidenced at a temperature of about 300 °C, alongside
the disappearance of the surface oxidation observed at room temperature.
At higher temperatures, the arsenic shell desorbs with an activation
energy of 2.32 eV, leading to clean facets. These results are helpful
to determine pathways toward improving the efficiency of oxidation-protective
layers on III–V semiconducting nanostructures.