Influence of graphite precursor on composition, morphology and structure of graphene materials obtained by thermal exfoliation-reduction of graphite oxide
This study aimed to determine the influence of the graphite precursor on the composition, morphology and structure of graphene materials obtained by thermal exfoliation-reduction of graphite oxide. The influence of the graphite precursor structure on the properties of the obtained graphene material is little understood in light of available literature data. Relating the composition, morphology and structure of graphene materials to the properties of the graphite precursor used is an important cognitive problem that needs to be solved. Moreover, the task set in the present research was to develop an oxidation method that would be more efficient compared to previously used modifications of the Hummers method. The descriptive table consists of results data from: * Elemental analysis * Analysis of graphite mineral matter * X-ray structural testing (XRD) * Raman spectroscopy * Thermogravimetric (TG) analysis * Structural infrared studies (FT-IR) * Scanning electron microscopy (SEM) * X-ray photoelectron spectroscopy (XPS) * Atomic force microscopy (AFM) * Porous texture analysis by N2 sorption at 77K
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Elemental analysis Carbon, hydrogen, nitrogen, sulphur and oxygen contents were determined using a Vario Macro Cube CHNS and O analyser. Analysis of graphite mineral matter The elemental composition of the mineral matter was determined by atomic emission spectroscopy (AES - ICP) using a Thermo Scientific iCAP 6500 DUO emission spectrometer with an inductively coupled argon plasma with a measuring range from 166 to 847 nm (Radial), and a charge injected semiconductor detector (CID). X-ray structural testing (XRD) Graphite studies - measurements were performed using an X`Pert PRO PW 3040/60 diffractometer from PANalytical. Monochromatic X-ray radiation of a copper lamp with the radiation length (K1) = 1.54187 Å was used. Graphite oxide and graphene materials were studied using an EMPYREAN diffractometer from PANalytical. Monochromatic X-rays of a cobalt lamp with radiation length (K1) = 1.7902 Å were used. Raman spectroscopy Spectroscopic studies of graphite, graphite oxides and reduced graphene oxides were carried out using a Raman spectrometer, N-TEGRA Spectra, from NT-MTD. The vibrations of the molecules were excited using a laser emitting a wavelength of 532 nm. Spectra were recorded with a spectral resolution of 5 to 11 cm-1 for the range studied. Thermogravimetric (TG) analysis Thermal stability studies of graphite oxides were carried out using a Netsch TG-STA209LUXX thermowell. Structural infrared studies (FT-IR) Graphite oxides and reduced graphene oxides were analysed by the FT-IR method. The absorption spectra for the obtained lozenges were recorded in the range of 4000 - 400 cm-1 with a spectral resolution of 4 cm-1. Scanning electron microscopy (SEM) Scanning electron microscopy (SEM) of graphene materials was performed using an FEI Nova NanoSEM 450 scanning electron microscope. SEM measurements were performed at an electron beam voltage of 10 - 15 kV in low vacuum mode (10 - 200 Pa). The magnification range used was 100 - 100000x. X-ray photoelectron spectroscopy (XPS) Photoelectron spectra for carbon materials were recorded at room temperature using a PHI 5000 VersaProbe photoelectron spectrometer from ULVAC (Japan)/Physical Electronics (USA). Atomic force microscopy (AFM) Measurements were performed for reduced graphene oxide samples on a N_TEGRA Prima platform (NT-MDT, Moscow, Russia), intermittent contact mode, and a High Accuracy, Noncontact (HA_NC) measurement probe. Images were acquired with a resonance frequency of 136.281 kHz. Porous texture analysis by N2 sorption at 77K The textural parameters of reduced graphene oxides were determined by measuring N2 sorption at 77 K ( 196 °C) using Micromeritics' 3FlexTM apparatus.