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The present work focuses on the synthesis of a vanadium nitride (VN)/carbon nanocomposite material via the thermal decomposition of vanadyl phthalocyanine (VOPC). The morphology and chemical structure of the synthesized compounds were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), Fourier transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD), and X-ray photoemission spectroscopy (XPS). The successful syntheses of the VOPC and non-metalated phthalocyanine (H2PC) precursors were confirmed using FTIR and XRD. The VN particles present a needle-like morphology in the VN synthesized by the sol-gel method. The morphology of the VN/C composite material exhibited small clusters of VN particles. The XRD analysis of the thermally decomposed VOPC indicated a mixture of amorphous carbon and VN nanoparticles (VN(TD)) with a cubic structure in the space group FM-3M consistent with that of VN. The XPS results confirmed the presence of V(III)-N bonds in the resultant material, indicating the formation of a VN/C nanocomposite. The VN/C nanocomposite synthesized through thermal decomposition exhibited a high carbon content and a cluster-like distribution of VN particles. The VN/C nanocomposite was used as an anode material in LIBs, which delivered a specific capacity of 307 mAh g−1 after 100 cycles and an excellent Coulombic efficiency of 99.8 at the 100th cycle.more » « less
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This work focuses on the synthesis of titanium nitride–carbon (TiN–carbon) composites by the thermal decomposition of a titanyl phthalocyanine (TiN(TD)) precursor into TiN. The synthesis of TiN was also performed using the sol-gel method (TiN(SG)) of an alkoxide/urea. The structure and morphology of the TiN–carbon and its precursors were characterized by XRD, FTIR, SEM, TEM, EDS, and XPS. The FTIR results confirmed the presence of the titanium phthalocyanine (TiOPC) complex, while the XRD data corroborated the decomposition of TiOPC into TiN. The resultant TiN exhibited a cubic structure with the FM3-M lattice, aligning with the crystal system of the synthesized TiN via the alkoxide route. The XPS results indicated that the particles synthesized from the thermal decomposition of TiOPC resulted in the formation of TiN–carbon composites. The TiN particles were present as clusters of small spherical particles within the carbon matrix, displaying a porous sponge-like morphology. The proposed thermal decomposition method resulted in the formation of metal nitride composites with high carbon content, which were used as anodes for Li-ion half cells. The TiN–carbon composite anode showed a good specific capacity after 100 cycles at a current density of 100 mAg−1.more » « less
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In the present study, the removal of both As(III) and As(V) from aqueous solutions using synthesized ZnO nanomaterials was achieved. The ZnO nanomaterial was synthesized using a precipitation technique and characterized using XRD, SEM, and Raman spectroscopy. XRD confirmed the ZnO nanoparticles were present in the hexagonal wurtzite structure. SEM of the particles showed they were aggregates of triangular and spherical particles. The average nanoparticle size was determined to be 62.03 ± 4.06 nm using Scherrer’s analysis of the three largest diffraction peaks. Raman spectroscopy of the ZnO nanoparticles showed only ZnO peaks, whereas the after-reaction samples indicated that As(V) was present in both As(V)- and As(III)-reacted samples. The adsorption of the ions was determined to be pH-independent, and a binding pH of 4 was selected as the pH for reaction. Batch isotherm studies showed the highest binding capacities occurred at 4 °C with 5.83 mg/g and 14.68 mg/g for As(III) and As(V), respectively. Thermodynamic studies indicated an exothermic reaction occurred and the binding of both As(III) and As(VI) took place through chemisorption, which was determined by the ΔH values of −47.29 and −63.4 kJ/mol for As(V) and As(III), respectively. In addition, the change in Gibbs free energy, ΔG, for the reaction confirmed the exothermic nature of the reaction; the spontaneity of the reaction decreased with increasing temperature. Results from batch time dependency studies showed the reaction occurred within the first 60 min of contact time.more » « less
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