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The examination of anisotropic nanostructures, such as wires, platelets or spikes, inside a transmission electron microscope is normally performed only in plan view. However, intrinsic defects such as growth twin interfaces could occasionally be concealed from direct observation for geometric reasons, leading to superposition. This article presents the shadow-focused ion-beam technique to prepare multiple electron-beam-transparent cross-section specimens of ZnO nanospikes, via a procedure which could be readily extended to other anisotropic structures. In contrast with plan-view data of the same nanospikes, here the viewing direction allows the examination of defects without superposition. By this method, the coexistence of two twin configurations inside the wurtzite-type structure is observed, namely [2 {\overline 1} {\overline 1} 0]^{\rm W}/(0 1 {\overline 1} 1) and [2 {\overline 1} {\overline 1} 0]^{\rm W}/(0 1 {\overline 1} 3), which were not identified during the plan-view observations owing to superposition of the domains. The defect arrangement could be the result of coalescence twinning of crystalline nuclei formed on the partially molten Zn substrate during the flame-transport synthesis. Three-dimensional defect models of the twin interface structures have been derived and are correlated with the plan-view investigations by simulation. 

Many topological semimetals are known to exhibit exceptional electronic properties, which are the fundamental basis for design of novel devices and further applications. Materials containing the structural motif of a square net are known to frequently be topological semimetals. In this work, the synthesis and structural characterization of the square‐net‐based magnetic topological semimetal candidates GdSb_xTe_2−x−δ(0,δindicating the vacancy level) are reported. The structural evolution of the series with Sb substitution is studied, finding a transition between a simple tetragonal square‐net structure to complex superstructure formations due to the presence of charge density waves. The structural modulations coincide with a significant modification of the magnetic order. This work thus establishes GdSb_xTe_2−x−δas a platform to study the interplay between crystal symmetry, band filling, charge density wave, and magnetism in a topological semimetal candidate.