Empyrean diffractometer

The in-situ XRD measurements were carried out on a PANalytical Empyrean diffractometer using Cu-K_α radiation. This technique was used to determine in-situ structural changes during heating and cooling cycles performing in the 25–120 °C range. The diffraction data were acquired using a step size of 0.013° 2θ and the count time of 1 S per step.

An X-ray diffraction analysis of nanomaterial powders was performed with a Panalytical Empyrean diffractometer (step size 0.02, time per step 1 s) at room temperature. For all analyses made, Cu Ka radiations with l = 1.541874 Å were used. Samples were scanned at a Bragg 2u angle between 10–80.

X-ray powder diffraction (XRPD) analysis was performed using an Empyrean diffractometer (PANalytical, 2012, Malvern, UK) in reflection–transmission mode. X-ray tubes equipped with Cu anodes were utilized as radiation sources (X-ray wavelength (1.5418 Å)). The PIXcel3D detector was used in linear (1D) scanning mode. The incident beam path consisted of W/Si, and a stepped X-ray mirror with an elliptical shape. Scans were made over a 2θ range of 10–90° with a total exposure time of 2 h. The SAXS measurements were performed by the same device at the SAXS/WAXS sample stage with capillary mode. The device was operated with a generator setting of 40 kV and 40 mA. The incident beam path consisted of W/Si, with a stepped X-ray mirror with an elliptical shape. The SAXS measurements were performed at −0.1–4 degrees 2θ with a step size of 0.005. The primary beam was measured with a Cu 0.2 mm beam attenuator and a PIXcel3D detector. The length of the scattering vector (or scattering vector) q is defined as q = (4πsinθ)/λ, where 2θ is the scattering angle and λ is the X-ray wavelength (1.5418 Å). Background scattering was evaluated by an air scattering measurement using an empty sample holder with foil. The Dv(R) calculations were performed using the indirect Fourier transform technique applied in the EasySAXS software (PANalytical, Malvern, United Kingdom, version 1.2).