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Correlative and in situ microscopy investigation of phase transformation, crystal growth and degradation of antimony sulfide thin films
Mingjian Wu, Maïssa K. S. Barr, Vanessa M. Koch, Martin Dierner, Tobias Dierke, Penghan Lu, Johannes Will, Rafal Dunin-Borkowski, Janina Maultzsch, Julien Bachmann, Erdmann Spiecker
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Antimony sulfide (Sb₂S₃), a compound of earth-abundant elements with highly anisotropic, quasi-layered crystal structure, triggered growing interest as a solar absorber in photovoltaics and as a phase change material in memory devices, yet challenges remain in achieving high-quality thin films with controlled nucleation and growth for optimal performance. Here, we investigate the phase transformation, crystal structure and properties, growth and degradation of atomic layer deposited Sb₂S₃ thin films using in situ TEM and correlative ex situ analysis. The as-deposited amorphous films crystallized at 243{\deg}C, forming grains with an [100] out-of-plane texture and developed into tens to hundreds of micrometer, leaves-shaped grains. Introducing an ultra-thin ZnS interfacial layer increased nucleation density, and resulted in a few micrometer-sized, more uniform grains while retaining the overall [100] texture. In situ observations and subsequent crystal orientation analysis with cutting-edge 4D-STEM and EBSD revealed that the grains grew faster along the [010] ribbon direction and that the bare films underwent early-stage degradation, forming holes in amorphous regions during annealing. The ZnS interlayer mitigated degradation, stabilizing the films and improving their uniformity. These findings offer valuable insights for optimizing Sb₂S₃ thin films for applications both as solar cell materials and phase change materials.
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