Design of an in situ setup combining nanocalorimetry and nano- or micro-focus x-ray scattering to address fast structure formation processes

Abstract

In the present chapter, we describe an original experimental setup combining micro- or nano-focus X-ray scattering and chip calorimetry (nanocalorimetry), which is designed for simultaneous in situ measurements. Some technical aspects of the setup design regarding its adaptation to the sample environment specific to the nano- and micro-focus synchrotron beamlines are discussed in the first part. In the following, we provide examples of applications of the setup for thermal studies of inorganic and nanostructured hybrid systems with nano-focus X-ray diffraction. In the last part, we report for the first time on the in situ nanocalorimetry/fast micro-focus X-ray scattering experiments on a semicrystalline polymer using heating ramps of 2000 °C/s at the X-ray detector acquisition rate of 4 ms/frame. For such real-time combination, one has to employ fast X-ray detectors with a high photon efficiency. In addition, one would absolutely need intense sources of X-rays such as the ones provided at the ID beamlines of the ESRF. We show that the setup capable of simultaneously probing the microstructural and thermodynamic properties can be useful for studies of materials having complex thermal behavior. In particular, the microstructural evolution during fast heating of a typical aromatic polyester, poly(trimethylene terephthalate), can be analyzed in much detail, which sheds light on the long-standing issue of multiple melting behavior in semirigid-chain polymers.