A quantitative method is proposed to determine Stone–Wales defects for 1D and 2D carbon nanostructures. The technique is based on the diene synthesis reaction (Diels–Alder reaction). The proposed method was used to determine Stone–Wales defects in the few-layer graphene (FLG) nanostructures synthesized by the self-propagating high-temperature synthesis (SHS) process in reduced graphene oxide (rGO) synthesized based on the method of Hammers and in the single-walled carbon nanotubes (SWCNT) TUBAL trademark, Russia. Our research has shown that the structure of FLG is free of Stone–Wales defects, while the surface concentration of Stone–Wales defects in TUBAL carbon nanotubes is 1.1 × 10−5 mol/m2 and 3.6 × 10−5 mol/m2 for rGO.
The method of self-propagating high-temperature synthesis has been employed to prepare 2D graphene structures (SHS-graphSHS procedure for carbonizing cyclic organic structures is a simple accessible method for making 2D graphene structures in practically needed amounts. The material obtained is designated as SHS-graphene. The study on starch carbonization product by combined complementary methods has shown the structure of SHS-graphene particles is similar to 2-3-layered graphene particles. The addition of graphene to NBR matrix results in the significant (to twice) enhancement of strength and thermal characteristics of composition material obtained, as compared to unfilled rubber.ene). A set of complementary methods (scanning electron microscopy, Raman microscopy, X-ray diffraction analysis) evidenced 2-3-layer graphene structure of the substance obtained. SHS-graphene has been utilized to modify NBR and thereby markedly strengthen the polymer matrix.
For the first time, few-layer graphene (FLG) nanosheets were synthesized by the method of self-propagating high-temperature synthesis (SHS) from biopolymers (glucose, starch, and cellulose). We suggest that biopolymers and polysaccharides, particularly starch, could be an acceptable source of native cycles for the SHS process. The carbonization of biopolymers under the conditions of the SHS process was chosen as the basic method of synthesis. Under the conditions of the SHS process, chemical reactions proceed according to a specific mechanism of nonisothermal branched-chain processes, which are characterized by the joint action of two fundamentally different process-accelerating factors—avalanche reproduction of active intermediate particles and self-heating. The method of obtaining FLG nanosheets included the thermal destruction of hydrocarbons in a mixture with an oxidizing agent. We used biopolymers as hydrocarbons and ammonium nitrate as an oxidizing agent. Thermal destruction was carried out in SHS mode, heating the mixture in a vessel up to 150–200 °C at a heating speed of 20–30 °C/min and keeping at this temperature for 15–20 min with the discharge of excess gases into the atmosphere. A combination of spectrometric research methods, supplemented by electron microscopy data, has shown that the particles of the carbonated product powder in their morphometric and physical parameters correspond to FLG nanosheets. An X-ray diffraction analysis of the indicated FLG nanosheets was carried out, which showed the absence of formations with a graphite crystal structure in the final material. The surface morphology was also studied, and the IR absorption features of FLG nanosheets were analyzed. It is shown that the developed SHS method makes it possible to obtain FLG nanosheets with linear dimensions of tens of microns and a thickness of not more than 1–5 graphene layers (several graphene layers).
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