Nanostar system

Scanning electron microscopy (SEM) was performed using FEI FEG250 with resolution of 1.2 nm equipped with SE and BSE detector. The surface morphology of the diamond and MoS₂ films was probed by atomic force microscopy (AFM) in a tapping mode (Bruker, Dimension Edge), using an etched silicon probe (Bruker, RTESPA - 300).
The crystallographic structure and orientation of the films were examined by X-ray diffraction (XRD) (CuKα) in the classical Bragg–Brentano and in the grazing-incidence configuration using BRUKER AXS D8 DISCOVER diffractometer with a rotating Cu anode.
The grazing-incidence wide-angle X-ray scattering (GIWAXS) measurements were performed using Nanostar system (Bruker AXS, Germany) equipped with IμS microfocus Cu X-ray source (λ = 0.154 nm). The parallel X-ray beam after Montel optics was further collimated using evacuated pinhole collimator equipped with two 550 µm pinholes separated by 1 m. The grazing-angle of incidence of X-ray beam on the sample was set to 0.8°. Reciprocal space maps were measured using an image plate detector at a sample-to-detector distance of 80 mm. All GIWAXS measurements were performed in fully evacuated chamber.

Small angle X-ray scattering (SAXS) data were collected using a NanoSTAR system (Bruker AXS GmbH, Karlsruhe, Germany) with pinhole collimation and a two-dimensional Hi STAR detector with resolution of 1,024 × 1,024 pixels, mounted on an X-ray tube with a copper anode and equipped with crossed Göbel focusing mirrors. Samples were mounted between two mica windows in sample holders with thickness of 1 or 2 mm. The sample-to-detector distance was 650 mm, and the exposure time for a single frame was 10,000 s. Each sample was measured three times, and the obtained data were averaged. The SAXS data were recorded within the scattering vector range of 0.15 nm⁻¹ < s < 3.5 nm⁻¹ (where s = 4πsinθ/λ, 2θ is the scattering angle, and λ is the X-ray wavelength). The recorded images were integrated using the spherical averaging method. The SAXS data were corrected for the detector response and normalized to the intensity of the incident beam, and the background scattering (empty holder) was subtracted using the SAXS_NT v4.1 program package (Bruker AXS GmbH, Karlsruhe, Germany).

The small-angle X-ray diffraction
(SAXRD) measurements were performed with a Bruker Nanostar system
(Cu Kα radiation, parallel beam formed by cross-coupled Goebel
mirrors and 3-pinhole collimation system, area detector VANTEC 2000).
The temperature of the sample was controlled with a precision of 0.1
°C. Samples were prepared as a thin film on a Kapton tape substrate.
For all samples temperature-dependent measurements were performed
in the same manner—data were collected every 5 °C for
60 s. A quasi-monodomain sample was prepared by a mechanical shearing
at elevated temperatures (10 °C below the phase transition point)
on a heating table.
Fitting of the experimental diffractograms
and simulation of the patterns were done using Topas 3 software (Bruker).
Each procedure started with choosing the most probable symmetry of
the lattice. Then, the unit cell parameters, intensities of the (Pseudo-Voigt)
signals, and (1/x) background intensity were considered
as independently adjustable parameters.