A novel in situ sample environment setup for combined small angle x-ray scattering (SAXS), wide-angle x-ray scattering (WAXS), and Fourier transform infrared spectrometer (FTIR) simultaneous measurement.

Developing the synchrotron radiation experiment method based on combined technology offers more information on the formation mechanism of new materials and their physical and chemical properties. In this study, a new small-angle x-ray scattering/ wide-angle x-ray scattering/ Fourier-transform infrared spectroscopy (SAXS/WAXS/FTIR) combined setup was established. Using this combined SAXS/WAXS/FTIR setup, x-ray and FTIR signals can be obtained simultaneously from the same sample. The in situ sample cell was designed to couple two FTIR optical paths for the attenuated total reflection and transmission modes, which greatly saved the time of adjusting and aligning the external infrared light path when switching between the two modes with good accuracy. A transistor-transistor logic circuit was used to trigger the synchronous acquisition from the IR and x-ray detectors. A special sample stage is designed, allowing access by the IR and x-ray with temperature and pressure control. The newly developed, combined setup can be used to observe the evolution of the microstructure during the synthesis of composite materials in real-time at both the atomic and molecular levels. The crystallization of polyvinylidene fluoride (PVDF) at different temperatures was observed. The time-dependent experimental data demonstrated the success of the in situ SAXS, WAXS, and FTIR study of the structural evolution, which is feasible to track the dynamic processes.