Abstract
This paper presents a study regarding the obtaining of NiCr2O4 by two new unconventional synthesis methods: (i) the first method is based on the formation of Cr(III) and Ni(II) carboxylate-type precursors in the redox reaction between the nitrate ion and 1,3-propanediol. The thermal decomposition of these complex combinations, at ~300 °C, leads to an oxide mixture of Cr2O3+x and NiO, with advanced homogeneity, small particles and high reactivity. On heating this mixture at 500 °C, Cr2O3 reacts with NiO to form NiCr2O4, which was evidenced by FT-IR and X-ray diffractometry (XRD) analysis; (ii) the second method starts from a mechanical mixture of (NH4)2Cr2O7 and Ni(NO3)2·6H2O. On heating this mixture, a violent decomposition at 240 °C with formation of an oxides mixture (Cr2O3 + CrO3) and NiO takes place. On thermal treatment up to 500 °C, an intermediary phase NiCrO4 is formed, which by decomposition at ~700 °C leads to NiCr2O4, evidenced by FT-IR and XRD analysis. NiCr2O4 is formed, in both cases, starting with a temperature higher than 400 °C, when the non-stoichiometric chromium oxide (Cr2O3+x ) loses the oxygen excess and turns to stoichiometric chromium oxide (Cr2O3), which further reacts with NiO.
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Abbreviations
- 1, 3PG:
-
1, 3-Propanediol
References
Jebarathinam NJ, Eswaramoorthy M, Krishnasamy V. Dehydrogenation of ethylbenzene over spinel oxides. Bull Chem Soc Japan. 1994;67:3334–8.
Sloczynski J, Ziolkowski J, Grzybowska B, Grabowski R, Jachewicz D, Wcislo K, Gengembre L. Oxidative dehydrogenation of propane on Ni x Mg1−x Al2O4 and NiCr2O4 spinels. J Catal. 1999;187:410–8.
Honeybourne CL, Rasheed RK. Nitrogen dioxide and volatile sulfide sensing properties of copper, zinc and nickel chromite. J Mat Chem. 1996;6:277–83.
Strawbridge A, Stott FH, Wood GC. The formation and incorporation into the scale of internal oxides developed during the high-temperature oxidation of dilute nickel-base alloys. Corros Sci. 1993;35:852–5.
Mančić L, Marinković ZV, Vulić P, Milošević O. The synthesis–structure relationship in the ZnO–Cr2O3 system. Sci Sinter. 2004;36:189–96.
Szczygiel I, Winiarska K. Low-temperature synthesis and characterization of the Mn–Zn ferrite. J Therm Anal Calorim. 2011;104:577–83.
Souaya ER, Ismail EH, Mohamed AA, Milad NE. Preparation, characterization and thermal studies of some transition metal ternary complexes. J Therm Anal Calorim. 2009;95:253–8.
Stefanescu M, Stefanescu O, Stoia M, Lazau C. Thermal decomposition of some metal-organic precursors: Fe2O3 nanoparticles. J Therm Anal Calorim. 2007;88(1):27–32.
Suryanarayana C, Grant Norton M. X-ray diffraction: a practical approach. New York: Plenum Press; 1998.
Stefanescu M, Barbu M, Vlase T, Barvinschi P, Barbu-Tudoran L, Stoia M. Novel low temperature synthesis method for nanocrystalline zinc and magnesium chromites. Thermochim Acta. 2011. doi:10.1016/j.tca.2011.09.005.
Stefanescu M, Sasca V, Birzescu M. Thermal behaviour of the homopolynuclear glyoxylate complex combinations with Cu(II) and Cr(III). J Therm Anal Calorim. 2003;72(2):515–24.
Stefanescu M, Sasca V, Birzescu M. Studies on the thermal decompositions of heteropolynuclear glyoxylates of Cr(III) and Cu(II). J Therm Anal Calorim. 1999;56(2):569–78.
Pocol V, Patron L, Carp O, Brezeanu M, Segal E, Stanica N. Some polynuclear coordination compounds precursor of chromites synthesis, physicochemical characterization and thermal stability. J Therm Anal Calorim. 1999;55:143–54.
Terada M, Maekawa T. The infrared absorption spectra of several chromites. Trans JIM. 1964;5:205–6.
Joint Committee on powder diffraction standards-International Center for Diffraction Data, Swarthmore; 1993;23-0432.
Holman HYN, Perry DL, Martin MC, Lamble GM, McKinney WR, Hunter-Cevera JC. Real-time characterization on biogeochemical reduction of Cr(VI) on basalt surfaces by SR-FTIR imaging. Geomicrobiol J. 1999;16:307–24.
Acknowledgements
This work was partially supported by the strategic grant POSDRU/88/1.5/S/50783, Project ID50783 (2009), co-financed by the European Social Fund–Investing in People, within the Sectoral Operational Programme Human Resources Development 2007–2013.
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Ştefănescu, M., Barbu, M., Barvinschi, P. et al. The obtaining of NiCr2O4 nanoparticles by unconventional synthesis methods. J Therm Anal Calorim 111, 1121–1127 (2013). https://doi.org/10.1007/s10973-011-2177-2
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DOI: https://doi.org/10.1007/s10973-011-2177-2