One-Stage Process of Reduction, Fluorination, and Doping with Nitrogen of Graphene Oxide Films.

The possibility of chemical modification of a graphene oxide film deposited on a Si/SiO2 substrate during a one-stage hydrothermal process in the presence of fluorine ions and reducing agents, such as ascorbic acid or hydrazine, is shown. The proposed technique makes it possible to obtain reduced fluorinated graphene nitride oxide (RGOFN) in the form of a thin film with a controlled composition of functional groups by changing the type and concentration of the reducing agent and then transferring the obtained films to any substrate. XPS and IR spectroscopy of the obtained films revealed controlled changes in the structure and composition of graphene oxide associated with the removal of oxygen groups and the incorporation of fluorine ions as well as the reduction of conjugated double bonds and the controlled incorporation of nitrogen into thin RGOFN films. The current-voltage characteristics of the fabricated RGOFN structures showed that their electrical properties are well controlled by doping with nitrogen during the proposed one-stage process.

Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers.

X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. However, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexes (Mn ∼ 6-15 mmol/l) with no visible effects of radiation damage. We also present the first L-edge absorption spectra of the oxygen evolving complex (Mn4CaO5) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions.

Reflection zone plate wavelength-dispersive spectrometer for ultra-light elements measurements.

We have developed an electron beam excitation ultra-soft X-ray add-on device for a scanning electron microscope with a reflective zone plate mulichannel spectrometer in order to analyse ultra-light elements such as Li and B. This spectrometer has high (λ/Δλ~100) resolving power in the energy range of 45 eV - 1120 eV. Metallic Li samples were examined and fluorescence spectra successfully measured. Energy resolution of 0.49 eV was measured in the ultra-low energy range using the Al L(2,3) line at 71 eV. High sensitivity of Boron detection was demonstrated on a B(4)C sample with layer thicknesses of 1-50 nm, detecting an amount of metallic Boron as small as ~0.57 fg.