Integrated control of a nanoindenter and X-ray nanodiffraction for automated in situ nanomechanical studies

X-ray diffraction (XRD) combined with in situ mechanical testing is a powerful, non-destructive technique that provides valuable information on structural evolution and defect formation during deformation. Unlike many other characterization methods, XRD does not impose constraints on sample dimensions, does not require a vacuum environment, and can be applied to a wide range of materials with periodic structures. However, such experiments present significant challenges due to the need for precise synchronization between independently controlled systems: one managing mechanical loading and the other handling X-ray measurements. In this work, we report on the successful software-level integration of a nanoindenter control system directly into the beamline control system. This integration enables full control of both mechanical and diffraction measurements from a single user interface, allowing real-time synchronization and automation of complex in situ experiments. We demonstrate the capabilities of this setup through uniaxial compression tests on α-Ti micropillars. Mechanical data from the nanoindenter and XRD patterns were collected simultaneously in an automated mode. Raster scans were performed on the micropillar in its pristine state, at two intermediate deformation stages, and post-mortem. This approach enabled detailed analysis of mechanical behavior and structural evolution under load, illustrating the effectiveness of the integrated system for advanced in situ studies.