Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China.
University of Chinese Academy of Sciences, Beijing 100049, China.
Rev Sci Instrum. 2023 Mar 1;94(3):033103. doi: 10.1063/5.0128211.
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.
基于组合技术开发同步辐射实验方法为新材料的形成机制及其物理化学性质提供了更多信息。本研究建立了一种新的小角 X 射线散射/广角 X 射线散射/傅里叶变换红外光谱（SAXS/WAXS/FTIR）组合装置。使用这种组合的 SAXS/WAXS/FTIR 装置，可以从同一样品中同时获得 X 射线和 FTIR 信号。设计了原位样品池，以将两个 FTIR 光路耦合到衰减全反射和透射模式，当在两种模式之间切换时，这极大地节省了调整和对准外部红外光路的时间，并且具有很好的精度。采用晶体管-晶体管逻辑电路来触发从 IR 和 X 射线探测器的同步采集。设计了一个特殊的样品台，允许进行具有温度和压力控制的 IR 和 X 射线访问。新开发的组合装置可用于在原子和分子水平上实时观察复合材料合成过程中微观结构的演变。观察了不同温度下聚偏二氟乙烯（PVDF）的结晶过程。时变实验数据表明，对结构演变的原位 SAXS、WAXS 和 FTIR 研究是成功的，这是一种可行的跟踪动态过程的方法。
