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Nanoprobe X‐ray diffraction (nXRD) using focused synchrotron radiation is a powerful technique to study the structural properties of individual semiconductor nanowires. However, when performing the experiment under ambient conditions, the required high X‐ray dose and prolonged exposure times can lead to radiation damage. To unveil the origin of radiation damage, a comparison is made of nXRD experiments carried out on individual semiconductor nanowires in their as‐grown geometry both under ambient conditions and under He atmosphere at the microfocus station of the P08 beamline at the third‐generation source PETRA III. Using an incident X‐ray beam energy of 9 keV and photon flux of 10 10  s −1 , the axial lattice parameter and tilt of individual GaAs/In 0.2 Ga 0.8 As/GaAs core–shell nanowires were monitored by continuously recording reciprocal‐space maps of the 111 Bragg reflection at a fixed spatial position over several hours. In addition, the emission properties of the (In,Ga)As quantum well, the atomic composition of the exposed nanowires and the nanowire morphology were studied by cathodoluminescence spectroscopy, energy‐dispersive X‐ray spectroscopy and scanning electron microscopy, respectively, both prior to and after nXRD exposure. Nanowires exposed under ambient conditions show severe optical and morphological damage, which was reduced for nanowires exposed under He atmosphere. The observed damage can be largely attributed to an oxidation process from X‐ray‐induced ozone reactions in air. Due to the lower heat‐transfer coefficient compared with GaAs, this oxide shell limits the heat transfer through the nanowire side facets, which is considered as the main channel of heat dissipation for nanowires in the as‐grown geometry.

Beam damage of single semiconductor nanowires during X‐ray nanobeam diffraction experiments