Leo 912 ab omega

TEM images and small area electron diffraction (SAED) patterns were obtained on a transmission electron microscope LEO912 AB OMEGA (Carl Zeiss, Germany) operating at 100 kV. Samples were prepared by drying the sol droplets placed on copper grids coated by Formvar™ film. SAED patterns were obtained at accelerated voltage of 100 kV and drawtube length of 290 mm. Both SAED patterns and dark field images were used to confirm the crystallinity of Au nanoparticles. The length and diameter distributions of the nanorods and nanospheres were measured by ImageJ 1.50b open source software (Wayne Rasband, NIH, USA). SEM images were obtained on a scanning electron microscope JSM 7401F (JEOL, Japan).

Metal NPs were obtained in a plasma electric arc discharge as published previously [14 (link),28 (link)] using ethanol as a solvent. They were characterized by size using a transmission electron microscope LEO 912 AB OMEGA (Carl Zeiss, Oberkochen, Germany) with energy filter and Keller system; by size distribution and ζ-potential using dynamic light scattering on a Zetasizer Nano ZS (Malvern Instruments, Worcestershire, UK); by qualitative elemental composition using an atomic-emission spectrometer iCAP 6300 Radial View (Thermo Fisher Scientific Inc., Waltham, MA, USA) with inductively coupled plasma.

TEM images were performed with a transmission electron microscope LEO 912AB OMEGA, Zeiss (Oberkochen, Germany) at an acceleration voltage of 100 kV. Cu-carrying chitosan composites for measurements were previously suspended in deionized water (resisting 18 MΩ) and sonicated in an ultrasonic bath for 15 min at RT. Then, a small drop of the suspension was dripped onto a copper grid (200 mesh) previously coated with formvar film. Then, the samples were dried at RT for 15 min and placed under the microscope.

The phase composition and morphology of the nanopowders obtained were investigated by X-ray diffraction methods (XRD, DRON-3M (Russia) and XRD-6000 Shimadzu (Japan)), transmission electron microscopy (TEM, LEO 912 AB Omega Carl Zeiss and Philips EM-301) and diffusion aerosol spectrometry (DAS, model 2702, Aeronanotech). The specific surface area was determined using the BET method on a NOVA 2200 instrument. Elemental analysis for the presence of residual carbon and nitrogen was carried out using an inductively coupled plasma atomic emission spectrometer (ICP-MS, Optima-5300). It was shown that the content of residual carbon and nitrogen in the powders did not exceed 0.08 and 0.07 wt %, respectively. The NiO nanopowder was characterized by X-ray photoelectron spectroscopy (XPS, PHI5500 Versa Probe II) with a monochromatic Al Kα X-ray source (hν = 1486.6 eV, 50 W).

Structural investigations of SiNW-based samples were carried out by using a field emission scanning electron microscope (FE-SEM, Carl Zeiss ULTRA 55, Carl Zeiss, Jena, Germany) and a transmission electron microscope (TEM, LEO912 AB OMEGA, Carl Zeiss, Jena, Germany). A Malvern Zetasizer Nano ZS instrument (Malvern Instruments Ltd., Malvern, England, UK) was used to determine the size and zeta potential (ζ) of SiNPs obtained from data of dynamic light scattering (DLS). The surface composition of nanoparticles was studied by using a Fourier-transform infrared (FTIR) spectrometer Bruker IFS 66v/S, (Bruker, Karlsruhe, Germany) with a germanium prism for attenuated total reflection. Before recording FTIR spectra, the suspensions were dried in air on the prism surface. The FTIR measurements were done at room temperature in vacuum at a residual pressure of 10⁻³ Torr.
Additionally, the suspensions of SiNPs were characterised by using PL spectroscopy by excitation with an Ar-ion laser (wavelength 364 nm, power 10 mW, spot diameter 1 mm, Spectra-Physics, Stahnsdorf, Germany). The PL signal was detected using a grating monochromator (MS750, SOLAR TII, Moscow, Russia) equipped with a CCD array. The measurements were carried out at room temperature in air.

Structural analysis of the samples was carried out by Carl Zeiss ULTRA 55 scanning electron microscopy (SEM) for SiNW layers and by LEO912 AB OMEGA transmission electron microscopy (TEM) for SiNPs. The samples of NPs for TEM studies were prepared by deposition of the nanoparticle powder on the standard carbon-coated gold TEM-grids. TEM images were processed with ImageJ Software to obtain the silicon nanocrystals (nc-Si) size distribution. To determine the hydrodynamic size of the nanoparticles a Malvern Instruments Mastersizer 200 have been used. The specific surface area of the SiNPs as well as their pore sizes and pore volumes were determined with N₂ adsorption/desorption (Micromeritics Tristar 3000). The pore area from the adsorption branch using BET theory (Brunauer, Emmett, and Teller), and the pore size was calculated from the desorption branch using BJH theory (Barrett, Joyner, and Halenda). Before measurements, the samples were dried by lyophilization. Fourier transform infrared (FTIR) spectra were measured by using Bruker spectrometer and attenuated total reflectance (ATR) addon.