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Nitrogen-doped carbon nanomaterial (NDCNM) was synthesized by grinding a mixture of graphene oxide and melamine in a planetary mill with both balls and milling chamber of zirconium dioxide. In the electron spin resonance spectrum of NDCNM, a broad signal with g = 2.08 was observed in addition to a narrow signal at g = 2.0034. In the study using a vibrating-sample magnetometer, the synthesized material is presumably a ferromagnet with a coercive force of 100 Oe. The specific magnetization at 10,000 Oe is approximately 0.020 and 0.055 emu/g at room temperature and liquid nitrogen temperature, respectively.
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Cellulose HogC was produced by the modified traditional method with 35% yield from the stem of Sosnovsky hogweed and was characterized by elemental analysis, infrared (IR) spectroscopy, powder X-ray diffractometry, differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). For HogC, the degree of crystallinity (approximately 70%) and the glass transition temperature (105-108 °C) were determined. It was found that the whiteness characteristic in the case of HogC was 92% and this significate was obtained without a bleaching procedure using chlorine-containing reagents. In this paper, the possibility of hydrophobization of HogC films by treatment with radiation-synthesized telomers of tetrafluoroethylene is shown. It was found that the contact angle of the telomer-treated cellulose film surface depended on the properties of the telomers (the chemical nature of the solvent, and the initial concentration of tetrafluoroethylene) and could reach 140 degrees.
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Celulosa , Cloro , Celulosa/química , Fluorocarburos , Polvos , SolventesRESUMEN
An improved procedure for the preparation of aerogel granules of polytetrafluoroethylene-graphene oxide (PTFE-GO) with a composition of 50:50 (in wt %) and a specific density of 35 ± 2 mg/cm3 is described. The technique practically excludes the granule cracking. The specific density of the pellets after reduction using hydrazine vapor and annealing at 370 °C decreased to 29 ± 2 mg/cm3. The PTFE-reduced GO (rGO) pellets obtained were tested as a recyclable sorbent for isopropyl alcohol (IPA) in sorption/combustion cycles. It has been shown that the aerogel sorption capacity for IPA increases from 35.6 to 39.3 g/g as a result of alcohol burning off. During the combustion of IPA, the temperature of an individual pellet can exceed 300 °C. When several contingent pellets are burned, the temperature of their heating increases. The fine-pored structure of the near-surface layer of the granule is destroyed during the alcohol burning, the internal structure with larger pores is exposed, and the relative proportion of PTFE on the surface of the granules decreases. It was also shown that the specific surface area of PTFE-rGO increases from 26 to 49 m2/g during cycling.
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A mixture of water suspensions of graphene oxide (GO) and polytetrafluoroethylene (PTFE) was used to make the films GO-PTFE (50:50). They became conductive (2.0-2.8 S/cm) while maintaining flexibility after reduction with hydrazine and subsequent annealing at 370 °C. The structure and morphology of the reduced films (rGO-PTFE) are examined in detail by means of a number of techniques such as scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Raman, and contact angle wetting. The results of the films tested as current collectors in a metal-free supercapacitor with electrodes from microwave exfoliated GO and an acid (1 M H2SO4) electrolyte are presented.
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Sodium alginate (NaAlg) is widely used as a food additive. To study the effect of irradiation with X-ray quanta with energies of 1253.6 eV and 1486.6 eV on the composition of NaAlg, thick films with a smooth surface were prepared, which did not differ in IR spectra from the original powders. The films were irradiated in a high vacuum (3 × 10-10 mbar) in the chamber of a Specs PHOIBOS 150 MCD9 XPS spectrometer with an X-ray source power of 150 W and an irradiation duration of up to 300 min, which significantly exceeded the time required to obtain an XPS spectrum. This made it possible to use XPS to monitor changes in the composition of the NaAlg surface directly during irradiation. As a result of the research, it has been established that NaAlg degrades with prolonged irradiation, which is accompanied by a significant decrease in the O/C ratio. When analyzing the dependence of the intensities of individual peaks in the C1s spectrum on the irradiation time, it was found that after 100 min of irradiation, a peak due to the carbonate group appears in the spectrum. The decomposition was also accompanied by a change in the color of NaAlg from white to yellow-brown. In the IR spectrum of the NaAlg film irradiated for 300 min, an absorption band was detected at 1910 cm-1, which is usually associated with the presence of allene groups.
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The chemical structure of the surface of glass fibers, including silanized fibers, was studied. Highly efficient heat-resistant composites were obtained by impregnating silanized glass fiber with a polysulfone solution, and the effect of modification of the surface of glass fibers on the physical, mechanical and thermophysical properties of the composite materials was studied. As a result of the study, it was found that the fiber-to-polymer ratio of 70/30 wt.% showed the best mechanical properties for composites reinforced with pre-heat-treated and silanized glass fibers. It has been established that the chemical treatment of the glass fibers with silanes makes it possible to increase the mechanical properties by 1.5 times compared to composites reinforced with initial fibers. It was found that the use of silane coupling agents made it possible to increase the thermal stability of the composites. Mechanisms that improve the interfacial interaction between the glass fibers and the polymer matrix have been identified. It has been shown that an increase in adhesion occurs both due to the uniform distribution of the polymer on the surface of the glass fibers and due to the improved wettability of the fibers by the polymer. An interpenetrating network was formed in the interfacial region, providing a chemical bond between the functional groups on the surface of the glass fiber and the polymer matrix, which was formed as a result of treating the glass fiber surface with silanes, It has been shown that when treated with aminopropyltriethoxysilane, significant functional unprotonated amino groups NH+/NH2+ are formed on the surface of the fibers; such free amino groups, oriented in the direction from the fiber surface, form strong bonds with the matrix polymer. Based on experimental data, the chemical structure of the polymer/glass fiber interface was identified.
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A special technique has been developed for producing a composite aerogel which consists of graphene oxide and soy wax (GO/wax). The reduction of graphene oxide was carried out by the stepwise heating of this aerogel to 250 °C. The aerogel obtained in the process of the stepwise thermal treatment of rGO/wax was studied by IR and Raman spectroscopy, scanning electron microscopy, and thermogravimetry. The heat treatment led to an increase in the wax fraction accompanied by an increase in the contact angle of the rGO/wax aerogel surface from 136.2 °C to 142.4 °C. The SEM analysis has shown that the spatial structure of the aerogel was formed by sheets of graphene oxide, while the wax formed rather large (200-1000 nm) clumps in the folds of graphene oxide sheets and small (several nm) deposits on the flat surface of the sheets. The sorption properties of the rGO/wax aerogel were studied with respect to eight solvent, oil, and petroleum products, and it was found that dichlorobenzene (85.8 g/g) and hexane (41.9 g/g) had the maximum and minimum sorption capacities, respectively. In the case of oil and petroleum products, the indicators were in the range of 52-63 g/g. The rGO/wax aerogel was found to be highly resistant to sorption-desorption cycles. The cyclic tests also revealed a swelling effect that occurred differently for different parts of the aerogel.
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Thermally stable films were obtained from a water-based polyurethane (PU) dispersion with small (0.1-1.5 wt.%) additions of graphene oxide (GO). The films were studied through elemental analysis, X-ray photoelectron spectroscopy, differential thermogravimetry, and Raman spectroscopy. It was found that the introduction of GO into a PU matrix was accompanied by a partial reduction in graphene oxide nanosheet and an increase in the concentration of defects in GO structure. It has been also established that the [C/N]at ratio in the near-surface layer of PU/GO composite films grows with an increase in the content of graphene oxide in the composite films.
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The electrochemical properties of the highly porous reduced graphene oxide/titanium dioxide (rGO/TiO2) nanocomposite were studied to estimate the possibility of using it as a supercapacitor electrode. Granular aerogel rGO/TiO2 was used as an initial material for the first time of manufacturing the electrode. For the aerogel synthesis, industrial TiO2 Hombikat UV100 with a high specific surface area and anatase structure was used, and the aerogel was carried out with hydrazine vapor. Porous structure and hydrophilic-hydrophobic properties of the nanocomposite were studied with a method of standard contact porosimetry. This is important for a supercapacitor containing an aqueous electrolyte. It was found that the hydrophilic specific surface area of the nanocomposite was approximately half of the total surface area. As a result of electrochemical hydrogenation in the region of zero potential according to the scale of a standard hydrogen electrode, a reversible Faraday reaction with high recharge rate (exchange currents) was observed. The characteristic charging time of the indicated Faraday reaction does not exceed several tens of seconds, which makes it possible to consider the use of this pseudocapacitance in the systems of fast energy storage such as hybrid supercapacitors. Sufficiently high limiting pseudo-capacitance (about 1200 C/g TiO2) of the reaction was obtained.
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A simple method for the mechanochemical synthesis of an effective metal-free electrocatalyst for the oxygen reduction reaction was demonstrated. A nitrogen-doped carbon material was obtained by grinding a mixture of graphene oxide and melamine in a planetary ball mill. The resulting material was characterized by XPS, EPR, and Raman and IR spectroscopy. The nitrogen concentration on the N-bmGO surface was 5.5 at.%. The nitrogen-enriched graphene material (NbmGO has half-wave potential of -0.175/-0.09 V and was shown to possess high activity as an electrocatalyst for oxygen reduction reaction. The electrocatalytic activity of NbmGO can be associated with a high concentration of active sites for the adsorption of oxygen molecules on its surface. The high current retention (93% for 12 h) after continuous polarization demonstrates the excellent long-term stability of NbmGO.
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The alkaline activation of a carbonized graphene oxide/dextrin mixture yielded a carbon-based nanoscale material (AC-TR) with a unique highly porous structure. The BET-estimated specific surface area of the material is 3167 m2/g, which is higher than the specific surface area of a graphene layer. The material has a density of 0.34 g/cm3 and electrical resistivity of 0.25 Ω·cm and its properties were studied using the elemental analysis, transmission electron microscopy (TEM), electron diffraction (ED), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray induced Auger electron spectroscopy (XAES), and electron energy loss spectroscopy (EELS) in the plasmon excitation range. From these data, we derive an integral understanding of the structure of this material. The concentration of sp3 carbon atoms was found to be relatively low with an absolute value that depends on the measurement method. It was shown that there is no graphite-like (002) peak in the electron and X-ray diffraction pattern. The characteristic size of a sp2-domain in the basal plane estimated from the Raman spectra was 7 nm. It was also found that plasmon peaks in the EELS spectrum of AC-TR are downshifted compared to those of graphite.
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Polytetrafluoroethylene-based aerogel was synthesized for the first time. Graphene oxide was used as a binder. After reduction with hydrazine and annealing at 370 °C, the aerogel with a density of 29 ± 2 mg/cm3 became superhydrophobic. The aerogel was characterized by IR spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. The sorption capacity of the aerogel for seven solvents and its sorption recyclability for hexane were measured.