Empyrean x ray diffractometer

XRD was carried out on solvent cast 5FU-loaded and blank PU films, and pure 5FU powder, using a Panalytical Empyrean X-ray diffractometer (Malvern Panalytical Ltd, Malvern, Worcestershire, UK) operating at 40 mA and 40 kV with Cu Kα radiation (λ = 1.541874 Å). The analysis was conducted at a 6° take-off angle and the samples were scanned over the 2θ range of 5° to 40° with a step size and step time of 0.026° and 179.52 s, respectively. The corresponding interlayer distances or d-spacing values were calculated from the XRD experimental parameters using Bragg’s equation [41 (link),42 (link),43 (link)].

Laboratory PXRD patterns were recorded at room temperature (RT) using the monochromatic Cu Kα X-ray source (λ = 1.5406 Å) on an Empyrean X-ray diffractometer (Malvern Panalytical Ltd. Malvern, Worcestershire, UK) over a 2θ range between 10° and 80° with a scan step of 0.053°. Structure refinements against powder diffraction data were performed with the Rietveld algorithm [54 (link)] using the X’Pert High Score Plus program (Version 4.1) [55 ]. The starting magnetite phase model was based on those of M. J. Fleet [56 (link)]. A pseudo-Voigt profile function and a polynomial background with up to four coefficients were applied to the structure refinements together with instrumental parameters (i.e., sample displacement and scaling factor), peak shape parameters, and lattice parameters. The quantitative phase analysis was carried out using the Hill and Howard formalism [57 (link)]. Crystallite size information was extracted from the phase-fitting method based on the change in profile widths compared to a standard sample.

The ultrasound irradiation process was carried out using an ultrasonic processor (Model No: VCX 750, Sonics and Materials, Inc., USA (750 W, 20 kHz)) with a titanium horn. The electrospinning process for the preparation of siloxene/PVDF piezofibers was carried out on NanoNC electrospinning instrument (Model: ESR200R2, South Korea). The X-ray diffractogram of siloxene sheets was recorded using an Empyrean X-ray diffractometer (Malvern Panalytical, UK) with Cu-Kα radiation (λ = 1.54184 Å). The Fourier transform infrared spectrum (FT-IR) was measured using a Thermo Scientific Nicolet-6700 FT-IR spectrometer. The laser Raman spectra were obtained using a Lab Ram HR Evolution Raman spectrometer (Horiba Jobin-Yvon, France, at a laser excitation source of wavelength 514 nm). The chemical state of elements present in the siloxene sheets was analyzed by an X-ray photoelectron spectrometer (ESCA-2000, VG Microtech Ltd). The surface morphology of the siloxene powders and electrospun fibers was examined using field emission scanning electron microscopy (TESCAN, MIRA3) under different magnifications with energy dispersive X-ray spectroscopy (EDS) and HR-TEM (JEM-2011, JEOL) with a CCD 4k × 4k camera (Ultra Scan 400SP, Gatan).

The first investigation carried out immediately after gas boriding was the phase analysis. An EMPYREAN X-ray diffractometer (Malvern Panalytical Ltd., Malvern, UK) was used for this study. X-ray diffraction patterns (XRD) were measured using Cu K_α radiation. The samples for microstructure analysis and nanoindentation required metallographic preparation including mounting in a conductive resin, grinding, polishing and etching with Marble’s reagent. The microscopic observations and EDS microanalysis were performed using a Vega 5135 Scanning Electron Microscope (TESCAN, Brno, Czech Republic). After the nanoindentation measurements finished, the tested areas were examined in a respect of their chemical composition. The content of the main elements (nickel, chromium, iron and boron) occurring in the borided layer, were measured using an Avalon X-ray microanalyzer (Princeton Gamma Tech, Princeton, NJ, USA) equipped with an energy dispersive spectrometer (EDS).

Dome‐shaped structures were described following a traditional multiscale approach (Shapiro, 2000 ; Vennin et al., 2015 ). This was focused on the separate characterization of the megastructure (i.e., large‐scale features of microbialite bed), macrostructure (i.e., gross form of microbialite bodies with typical dimensions from decimeter to meter scale), mesostructure (i.e., internal textures of macrostructural elements visible to naked eye), and microstructure (i.e., microscopic fabrics observed under petrographic analysis).
External morphology (megastructure and macrostructure) was established using field data, whereas internal morphology (mesostructure and microstructure) was examined using a Leica DMS 100 binocular loupe and a petrographic microscope equipped with a Leica DFC 420 camera. Mineral fractions of the dome‐shape structures were analyzed using a Malvern PANalytical Empyrean x‐ray diffractometer, with X'Celerator detector and Cu tube. The scan rate was 0.5°/min, under a voltage of 40 kv and current of 30 mA. The dried and ground samples were scanned in the 2·ϴ‐diffraction angle from 5° to 70°, with a scanning step size of 0.01°, operated at 40 kV and 40 mA with a Cu X‐ray source (Cu Kα_1,2, λ = 1.54056 Å). The interpretation of the results has been done with the X'Pert Highscore Plus Software (PANalytical, 2004 ) with PDF‐2 data bank (see Faber & Fawcett, 2002 (link)).