Structural characterization of gel-grown neodymium copper oxalate single crystals
Sparingly soluble neodymium copper oxalate (NCO) single crystals were grown by gel method, by the diffusion of a mixture of neodymium nitrate and cupric nitrate into the set gel containing oxalic acid. Tabular crystal, revealing well-defined dissolution figures has been recorded. X-ray diffraction studies of the powdered sample reveal that NCO is crystalline. Infrared absorption spectrum confirmed the formation of oxalato complex with water of crystallization, while energy dispersive X-ray analysis established the presence of neodymium dominant over copper in the sample. X-ray photoelectron spectroscopic studies established the presence of Nd and Cu in oxide states besides (C2O4)2− oxalate group. The intensities of Nd (3d5/2) and Cu (2p3/2) peaks measured in terms of maximum photoelectron count rates also revealed the presence of Nd in predominance. The inductively coupled plasma analysis supports the EDAX and XPS data by the estimation of neodymium percentage by weight to that of copper present in the NCO sample. On the basis of these findings, an empirical structure for NCO has been proposed. The implications are discussed.
KeywordsNeodymium copper oxalate gel growth characterization XRD IR EDAX XPS
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- Beille J, Cabanel R, Chaillout C, Chevallier B, Demazeau G, Deslandes F, Etourneau J, Lejay P, Michel C, Provost J, Raveau B, Sulpice A, Tholence J L and Tournier R 1987C. R. Acad. Sci. Ser. 2 304 1097Google Scholar
- George V, Ittyachen M A and Jayakumari Issac 1990Cryst. Res. Technol. 25 k-153Google Scholar
- Henisch H K 1970Crystal growth in gels (University Park and London: Pennsylvania State University Press)Google Scholar
- Huheey J E 1983Inorganic chemistry—Principles of structure and reactivity (New York: Harper International) 3rd edn pp. 314–315Google Scholar
- Nakamoto K 1978Infrared and Raman spectra of inorganic and coordination compounds (New York: John Wiley and Sons) 3rd edn p. 234Google Scholar
- Raju K S 1983bBull. Mater. Sci. 5 67Google Scholar
- Raju K S 1986VIII International Conference on crystal growth, University of York, York, UK Google Scholar
- Riggs W M and Parker M J 1975 inMethods of surface analysis (ed.) (A W Czanderna) (Amsterdam: Elsevier Scientific Pub. Co.) Chap. 4 p. 108Google Scholar
- Wagner C D, Riggs W M, Davis L E, Moulder J F and Mullenberg G E 1978Handbook of X-ray photoelectron spectroscopy (Minnesota: Perkin Elmer Corporation)Google Scholar
- Weast R C and Lide D R 1990CRC Handbook of chemistry and physics (Boca Raton, Florida: CRC Press Inc.) B-109Google Scholar