Environmental chambers for thin film characterization by grazing incidence x-ray scattering and broadband dielectric spectroscopy

While x-ray scattering and broadband dielectric spectroscopy (BDS) experiments are routinely performed in vacuum and under controlled humidity on bulk samples, in situ measurements of thin films in non-aqueous solvent vapor environments introduce additional requirements. Two controlled environmental chambers for performing grazing incidence x-ray scattering and BDS address this critical need for studying thin films in either aqueous or organic atmospheres. Both chambers enable temperature-controlled measurements under ambient conditions, flowing gas or solvent vapor, or partial pressures generated by solvent reservoirs. In situ control of temperature is achieved by attaching to an external temperature controller. To facilitate grazing incidence small- and wide-angle x-ray scattering and x-ray reflectivity, the environmental chamber for grazing incidence x-ray scattering has exit angles of 2θ = 38° and 51° in the horizontal and vertical directions, respectively. Low x-ray attenuation (∼ 10%) is achieved by using Kapton windows, and the chamber is sealed to enable use in evacuated x-ray scattering systems such as the Xenocs Xeuss 2.0. The broadband dielectric spectroscopy environmental chamber measures dipole dynamics and ionic conductivities of materials on interdigitated electrodes. Cord grip feedthroughs eliminate additional capacitance from the sample chamber and make the environmental chamber broadly compatible with electrochemical impedance spectrometers. The utility of these chambers is demonstrated on three polymeric systems with various film thicknesses, morphologies, and solvents.