Digital micro-photogrammetry in analysis and modeling habit and sectoral structure of real high-pressure high-temperature single-crystal diamonds.

We demonstrate the potential of using digital stereo micro-photogrammetry for the analysis and modeling of the habit and sectoral structure of real high-pressure high-temperature single-crystal diamonds. A prototype scanning system with a resolution of 5 µm has been implemented based on a digital single-lens reflex camera, making it possible to create highly accurate reproductions of crystal shapes with a minimum size of 4 mm. This method makes it possible to monitor the effect of actual conditions on the physical processes of crystal growth, which is a useful advance for the development of active device elements based on semiconductor diamonds.

Mechanochemical synthesis of carbon-stabilized Cu/C, Co/C and Ni/C nanocomposites with prolonged resistance to oxidation.

Metal-carbon nanocomposites possess attractive physical-chemical properties compared to their macroscopic counterparts. They are important and unique nanosystems with applications including in the future development of nanomaterial enabled sensors, polymer fillers for electromagnetic radiation shields, and catalysts for various chemical reactions. However, synthesis of these nanocomposites typically employs toxic solvents and hazardous precursors, leading to environmental and health concerns. Together with the complexity of the synthetic processes involved, it is clear that a new synthesis route is required. Herein, Cu/C, Ni/C and Co/C nanocomposites were synthesized using a two-step method including mechanochemical treatment of polyethylene glycol and acetates of copper, nickel and cobalt, followed by pyrolysis of the mixtures in an argon flow at 700 °C. Morphological and structural analysis of the synthesized nanocomposites show their core-shell nature with average crystallite sizes of 50 (Cu/C), 18 (Co/C) and 20 nm (Ni/C) respectively. The carbon shell originates from disordered sp2 carbon (5.2-17.2 wt.%) with a low graphitization degree. The stability and prolonged resistance of composites to oxidation in air arise from the complete embedding of the metal core into the carbon shell together with the presence of surface oxide layer of metal nanoparticles. This approach demonstrates an environmentally friendly method of mechanochemistry for controllable synthesis of metal-carbon nanocomposites.

Low-Temperature Reduction of Graphene Oxide: Electrical Conductance and Scanning Kelvin Probe Force Microscopy.

Graphene oxide (GO) films were formed by drop-casting method and were studied by FTIR spectroscopy, micro-Raman spectroscopy (mRS), X-ray photoelectron spectroscopy (XPS), four-points probe method, atomic force microscopy (AFM), and scanning Kelvin probe force (SKPFM) microscopy after low-temperature annealing at ambient conditions. It was shown that in temperature range from 50 to 250 °C the electrical resistivity of the GO films decreases by seven orders of magnitude and is governed by two processes with activation energies of 6.22 and 1.65 eV, respectively. It was shown that the first process is mainly associated with water and OH groups desorption reducing the thickness of the film by 35% and causing the resistivity decrease by five orders of magnitude. The corresponding activation energy is the effective value determined by desorption and electrical connection of GO flakes from different layers. The second process is mainly associated with desorption of oxygen epoxy and alkoxy groups connected with carbon located in the basal plane of GO. AFM and SKPFM methods showed that during the second process, first, the surface of GO plane is destroyed forming nanostructured surface with low work function and then at higher temperature a flat carbon plane is formed that results in an increase of the work function of reduced GO.

Infrared Reflectance Analysis of Epitaxial n-Type Doped GaN Layers Grown on Sapphire.

Infrared (IR) reflectance spectroscopy is applied to study Si-doped multilayer n+/n0/n+-GaN structure grown on GaN buffer with GaN-template/sapphire substrate. Analysis of the investigated structure by photo-etching, SEM, and SIMS methods showed the existence of the additional layer with the drastic difference in Si and O doping levels and located between the epitaxial GaN buffer and template. Simulation of the experimental reflectivity spectra was performed in a wide frequency range. It is shown that the modeling of IR reflectance spectrum using 2 × 2 transfer matrix method and including into analysis the additional layer make it possible to obtain the best fitting of the experimental spectrum, which follows in the evaluation of GaN layer thicknesses which are in good agreement with the SEM and SIMS data. Spectral dependence of plasmon-LO-phonon coupled modes for each GaN layer is obtained from the spectral dependence of dielectric of Si doping impurity, which is attributed to compensation effects by the acceptor states.

Structural Modification of Single-Layer Graphene Under Laser Irradiation Featured by Micro-Raman Spectroscopy.

Confocal micro-Raman spectroscopy is used as a sensitive tool to study the nature of laser-induced defects in single-layer graphene. Appearance and drastic intensity increase of D- and D' modes in the Raman spectra at high power of laser irradiation is related to generation of structural defects. Time- and power-dependent evolution of Raman spectra is studied. The dependence of relative intensity of defective D- and D' bands is analyzed to relate the certain types of structural defects. The surface density of structural defects is estimated from the intensity ratio of D- and G bands using the D-band activation model. Unusual broadening of the D band and splitting of the G band into G- and G+ components with redistribution of their intensities is observed at high laser power and exposition. Position of the G+ band is discussed in relation with nonuniform doping of graphene with charge impurities. Simultaneous presence in the Raman spectra of heavily irradiated graphene of rather narrow G band and broaden D band is explained by coexistence within the Raman probe of more and less damaged graphene areas. This assumption is additionally confirmed by confocal Raman mapping of the heavily irradiated area.

Structure and Optical Features of Micro/Nanosized Carbon Forms Prepared by Electrochemical Exfoliation.

Micro/nanosized carbon materials were prepared by electrochemical exfoliation method in the forms of the colloids and thin films. Scanning electronic microscopy, optical and luminescent microscopy, and Raman scattering and luminescent spectroscopy were applied for characterization of materials. The wide photoluminescence band in the visible spectral region was observed for each of the samples. The shape of the photoluminescence band depends on excitation wavelength and on the size of the particles. At least two components with maxima at ~580 and ~710 nm can be distinguished in the photoluminescence spectra. The relations between the photoluminescence properties and morphology of the samples have been described and discussed.

Silicon Substrate Strained and Structured via Cavitation Effect for Photovoltaic and Biomedical Application.

A hybrid structure, which integrates the nanostructured silicon with a bio-active silicate, is fabricated using the method of MHz sonication in the cryogenic environment. Optical, atomic force, and scanning electron microscopy techniques as well as energy dispersive X-ray spectroscopy were used for the investigation of the morphology and chemical compound of the structured surface. Micro-Raman as well as X-ray diffraction, ellipsometry, and photovoltage spectroscopy was used for the obtained structures characterization. Ellipsometer measurements demonstrated the formation of the layer with the thicknesses ~700 nm and optical parameters closed to SiO2 compound with an additional top layer of the thicknesses ~15 nm and the refractive index ~1. Micro-Raman investigation detects an appearance of Ca-O local vibrational mode, and the stretching vibration of SiO4 chains characterized the wollastonite form of CaSiO3. A significant rise in the value and an expansion of the spectral range of the surface photovoltage for silicon structured via the megasonic processing was found. The concept of biocompatible photovoltaic cell on the base of Si\CaSiO3 structure for the application in bioelectronics was proposed.

Manifestation of Structure of Electron Bands in Double-Resonant Raman Spectra of Single-Walled Carbon Nanotubes.

Micro-Raman spectra of single-walled carbon nanotubes in the range of two-phonon 2D bands are investigated in detail. The fine structure of two-phonon 2D bands in the low-temperature Raman spectra of the mixture and individual single-walled carbon nanotubes is considered as the reflection of structure of their π-electron zones. The dispersion behavior of 2D band fine structure components in the resonant Raman spectra of single-walled carbon nanotube mixture is studied depending on the energy of excitating photons. The role of incoming and outgoing electron-phonon resonances in the formation of 2D band fine structure in Raman spectra of single-walled carbon nanotubes is analyzed. The similarity of dispersion behavior of 2D phonon bands in single-walled carbon nanotubes, one-layer graphene, and bulk graphite is discussed.

Possibility of graphene growth by close space sublimation.

Carbon films on the Si/SiO2 substrate are fabricated using modified method of close space sublimation at atmospheric pressure. The film properties have been characterized by micro-Raman and X-ray photoelectron spectroscopy and monochromatic ellipsometry methods. Ellipsometrical measurements demonstrated an increase of the silicon oxide film thickness in the course of manufacturing process. The XPS survey spectra of the as-prepared samples indicate that the main elements in the near-surface region are carbon, silicon, and oxygen. The narrow-scan spectra of C1s, Si2p, O1s regions indicate that silicon and oxygen are mainly in the SiOx (x ≈ 2) oxide form, whereas the main component of C1s spectrum at 284.4 eV comes from the sp2-hybridized carbon phase. Micro-Raman spectra confirmed the formation of graphene films with the number of layers that depended on the distance between the graphite source and substrate.