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.Electronic supplementary materialThe online version of this article (10.1186/s11671-018-2536-z) contains supplementary material, which is available to authorized users.

Atomic force microscopy in different operation modes (topography, derivative topography, and phase contrast) was used to obtain 3D images of Vickers indents on the surface of diamond and cBN single crystals with high spatial resolution. Confocal Raman spectroscopy and Kelvin probe force microscopy were used to study the structure of the material in the indents. It was found that Vickers indents in diamond has no sharp and clear borders. However, the phase contrast operation mode of the AFM reveals a new viscoelastic phase in the indent in diamond. Raman spectroscopy and Kelvin probe force microscopy revealed that the new phase in the indent is disordered graphite, which was formed due to the pressure-induced phase transformation in the diamond during the hardness test. The projected contact area of the graphite layer in the indent allows us to measure the Vickers hardness of type-Ib synthetic diamond. In contrast to diamond, very high plasticity was observed for 0.5 N load indents on the (001) cBN single crystal face. Radial and ring cracks were absent, the shape of the indents was close to a square, and there were linear details in the indent, which looked like slip lines. The Vickers hardness of the (111) synthetic diamond and (111) and (001) cBN single crystals were determined using the AFM images and with account for the elastic deformation of the diamond Vickers indenter during the tests.

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.

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.