Abstract—
The surface morphology and composition of a NbC/C composite prepared via thermal decomposition of the products of reaction between NbCl5 and acetylene [9] have been studied by scanning electron microscopy and X-ray photoelectron spectroscopy. The results demonstrate that the NbC thus synthesized consists of nanocrystals. The surface layer of the NbC/C composite contains nine carbon atoms per Nb atom. The niobium is present in the form of the NbC carbide (33%) and the NbO2 (10%) and Nb2O5 (57%) oxides, with Nb 3d5/2 electron binding energies of 203.8, 205.0, and 207.2 eV, which are tentatively attributed to Nb2+ (NbC), Nb4+, and Nb5+ ions, respectively. The presence of NbO2 and Nb2O5 in the surface layer is due to active reaction of the NbC/C composite with atmospheric oxygen and moisture during the sample preparation process. Our results on the structure of the C1s electron spectra lead us to assume that the carbon on the surface of the composite particles has the form of a graphene-like carbon material. The composite does not become charged when exposed to an X-ray beam, which suggests that it is a weak dielectric.
Similar content being viewed by others
REFERENCES
Oshikawa, K., Nagai, M., and Omi, S., Characterization of molybdenum carbides for methane reforming by TPR, XRD, and XPS, J. Phys. Chem. B, 2001, vol. 105, pp. 9124–9131.
Schweitzer, N.M., Schaidle, J.A., Ezekoye, O.K., Pan, X., Linic, S., and Thompson, L.T., High activity carbide supported catalysts for water gas shift, J. Am. Chem. Soc., 2011, vol. 133, pp. 2378–2384.
Wan, C., Regmi, Y.N., and Leonard, B.M., Multiple phases of molybdenum carbide as electrocatalysts for the hydrogen evolution reaction, Angew. Chem., Int. Ed., 2014, vol. 53, pp. 6407–6410.
Porosoff, M.D., Yang, X., Boscoboinik, J.A., and Chen, J.G., Molybdenum carbide as alternative catalysts to precious metals for highly selective reduction of CO2 to CO, Angew. Chem., Int. Ed., 2014, vol. 53, pp. 6705–6710.
Qin Yu, Chen Ping, and Duan Jinzhao, Carbon nanofibers supported molybdenum carbide catalysts for hydrodeoxygenation of vegetable oils, RSC Adv., 2013, vol. 3, pp. 17 485–17 491.
Tolosa, A., Kruner, B., Fleischman, S., Jackel, N., Zeigel, M., Asian, M., Grobelsek, I., and Presser, V., Niobium carbide nanofibers as a versatile precursor for high power supercapacitor and high energy battery electrodes, J. Mater. Chem. A, 2016, vol. 4, pp. 16 003–16 016.
Il’in, E.G., Parshakov, A.S., Iskhakova, L.D., Buryak, A.K., and Dzhavad Ogly, A.A., Thermal stability and decomposition products of a MoCl1.9 ± 0.1(C30 ± 1H30 ± 1) composite, Inorg. Mater., 2014, vol. 51, no. 6, pp. 631–635.
Il’in, E.G., Parshakov, A.S., Buryak, A.K., Kochubei, D.I., Drobot, D.V., and Nefedov, V.I., Nanosized clusters of molybdenum chlorides—active sites in catalytic acetylene oligomerization, Dokl. Phys. Chem., 2009, vol. 427, no. 2, pp. 150–154.
Il’in, E.G., Parshakov, A.S., and Iskhakova, L.D., The studies of NbCl5 with acetylene reaction product as a new precursor for simple and economical synthesis of ceramic NbC/C nanocomposite, Advances in Synthesis and Complexing: 5th Int. Scientific Conf., Moscow, 2019, vol. 2, p. 25.
Il’in, E.G., Parshakov, A.S., Teterin, A.Yu., Maslakov, K.I., and Teterin, Yu.A., X-ray photoelectron spectroscopic characterization of the acetylene cyclotrimerization catalyst NbCl2(CnHn) (n = 10–12), Russ. J. Inorg. Chem., 2011, vol. 56, no. 11, pp. 1788–1793.
Il’in, E.G., Parshakov, A.S., Teterin, A.Yu., Maslakov, K.I., and Teterin, Yu.A., X-ray photoelectron study of the MoCl2C30H30 composite, Inorg. Mater., 2011, vol. 47, no. 4, pp. 442–448.
Il’in, E.G., Beirakhov, A.G., Teterin, Yu.A., Maslakov, K.I., and Teterin, A.Yu., Surface morphology and composition of nanocrystalline MoO2 produced via the thermal decomposition of the MoO2(i-C3H7NHO)2 complex, Inorg. Mater., 2017, vol. 53, no. 6, pp. 602–612.
Il’in, E.G., Parshakov, A.S., Teterin, Yu.A., Maslakov, K.I., and Teterin, A.Yu., surface composition and morphology of a carbon matrix/Mo2C composite material, Inorg. Mater., 2017, vol. 53, no. 5, pp. 469–476.
Marques, M.T., Ferraria, A.M., Correia, J.B., Botelho do Rego, A.M., and Vilar, R., XRD, XPS and SEM characterization of Cu–NbC nanocomposite produced by mechanical alloying, Mater. Chem. Phys., 2008, vol. 109, pp. 174–180.
Nefedov, V.N., Rentgenoelektronnaya spektroskopiya khimicheskikh soedinenii (X-ray Photoelectron Spectroscopy of Chemical Compounds), Moscow: Khimiya, 1984.
Teterin, Yu.A. and Gagarin, S.G., Inner valence molecular orbitals of compounds and the structure of X‑ray photoelectron spectra, Usp. Khim., 1996, vol. 65, no. 10, pp. 895–912.
Teterin, Yu.A. and Baev, A.S., Rentgenovskaya fotoelektronnaya spektroskopiya soedinenii lantanoidov (X-ray Photoelectron Spectroscopy of Lanthanide Compounds), Moscow: TsNIIAtominform, 1987.
Shirley, D.A., High-resolution X-ray photoemission spectrum of the valence bands of gold, Phys. Rev. B: Solid State, 1972, no. 5, pp. 4709–4714.
Nemoshkalenko, V.V. and Aleshin, A.G., Elektronnaya spektroskopiya kristallov (Electron Spectroscopy of Crystals), Kiev: Naukova Dumka, 1976.
Baev, A.S., Zelenkov, A.G., Kuakov, V.M., Odinov, B.V., Smilga, V.P., Teterin, Yu.A., Tumanov, Yu.P., and Chugunov, O.K., Radiation damage in pyrolytic graphite studied by X-ray photoelectron spectroscopy, Zh. Strukt. Khim., 1980, vol. 21, no. 5, pp. 29–33.
Ihara, H. and Watanabe, K., Electronic bond structures of the NbC–NbN alloy system from the X-ray photoelectron spectroscopic measurement, Solid State Commun., 1981, vol. 38, pp. 1211–1213.
Zhizhin, E.V., Pudikov, D.A., Rybkin, A.G., Ul’yanov, P.G., and Shikin, A.M., Synthesis and electronic structure of graphene on a nickel film adsorbed on graphite, Phys. Solid State, 2015, vol. 57, no. 9, pp. 1888–1895.
Aleshin, V.G., Kharlamov, A.I., and Prokopenko, V.M., X-ray photoelectron spectra of metal-like carbides, Izv. Akad. Nauk SSSR,Neorg. Mater., 1981, vol. 17, no. 3, pp. 550–553.
Sosulnikov, M.I. and Teterin, Yu.A., X-ray photoelectron studies of Ca, Sr, Ba and their oxides and carbonates, J. Electron Spectrosc. Relat. Phenom., 1992, vol. 59, pp. 111–126.
Funding
This work was supported by the Russian Foundation for Basic Research, project no. 18-29-11083.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Il’in, E.G., Parshakov, A.S., Teterin, Y.A. et al. Surface Morphology and Composition of a NbC/C Composite Studied by Scanning Electron Microscopy and X-Ray Photoelectron Spectroscopy. Inorg Mater 56, 443–450 (2020). https://doi.org/10.1134/S0020168520050052
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168520050052