Instrumentation developments on PAINEIRA beamline for <i>in situ/operando</i> synchrotron radiation powder X-ray diffraction

Abstract Structural characterization under in situ/operando conditions using synchrotron radiation powder X-ray diffraction (SR-PXRD) facilities is a powerful technique for investigating technological materials and devices. The high resolution and rapid data acquisition provide valuable insights into the structure-property relationship in functional materials. However, such experiments require complex and specific instrumentation. In this context, we describe the development and capabilities of instrumentation based on a capillary flow cell supplied by an automated control module and real-time acquisition software for conducting in situ and operando SR-PXRD experiments at the PAINEIRA beamline at Sirius, the Brazilian Synchrotron Light Laboratory (LNLS). This system comprises a compact, multifunctional capillary cell within a controlled module that regulates the flow of gases, vapors, or liquids and allows for pressure variations, simulating realistic operating conditions such as catalytic reactions involving oxidation, reduction, or hydrocarbon dry and steam reforming. The beamline has a user-friendly interface for monitoring and controlling dynamic experiments. Additionally, custom software enables real-time visualization of XRD patterns, providing crucial information on the evolution of critical structural properties during kinetic studies. The IGUAPE software continuously fits peak positions, integrated areas, and full width at half maximum (FWHM).