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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).

New Way of Synthesis of Few-Layer Graphene Nanosheets by the Self Propagating High-Temperature Synthesis Method from Biopolymers