Preparation and Electrochemical Performance of Mesoporous Niobium Nitride Powders
CUI Shuai1, 2, HU Shilei1, 2, LYU Dongfeng1, 2, CUI Yi1, 2, WEI Yingna1, 2, WEI Hengyong1, 2, BU Jinglong1, 2, CHEN Yuejun1, 2
1 College of Material Science and Engineering, North China University of Science and Technology, Tangshan 063210, China 2 Hebei Provincial Key Laboratory of Inorganic Nonmetallic Materials, Tangshan 063210, China
Abstract: Nb2O5 precursor powder was prepared by solvothermal method, NbCl5 as niobium source and P123 as the pore-forming agent, cyanamide as the structural stabilizer. The mesoporous niobium nitride powder was synthesized via nitrogen reduction of the mesoporous Nb2O5 powder at 800 ℃ in NH3.The phase and morphology were characterized by XRD, XPS, SEM, BET and TEM. The results show that the synthesized nio-bium nitride powder is cubic Nb4N5 phase, which is similar to spherical particles.It can be seen from the XPS analysis that the powder mainly contains three elements: Nb, N and O, and in the narrow spectrum of Nb elements, the binding energy is 204.6 eV, 207.2 eV and 209.8 eV, and the corresponding bonds are Nb3+-N, Nb5+-N and Nb5+-O, respectively, indicating that there are two valence states of Nb3+ and Nb5+ in the nitride powders. And the Nb5+ peak intensity is higher than Nb3+, indicating that the niobium is present in the form of Nb5+. The specific surface area of the powder is 39 m2·g-1, the pore structure in the range of 3—5 nm of powders has a high proportion, and there are also many pore structures in the range of 8—15 nm. The electrochemical properties were tested by CV, GCD and EIS. The results show that there is no obvious redox peak in CV curve, which is mainly characterized by double layer. The energy storage of niobium nitride powders is mainly controlled by the charge transfer process on the electrode surface. The specific capacitance is 90 F·g-1 when the current density is 10 mA·g-1. The internal resistance is 0.82 Ω, and the ion diffusion impedance is 0.22 Ω. When the power density is 480 kW·kg-1, the energy density is 7.2 Wh·kg-1.
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