Аннотация: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 microfocus
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 semirigidchain
polymers.