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Synthesis and crystallographic study of cation substituted NZP materials: Na1+xZr2−xMxP3O12 (M = Sb, Al, Cr and x = 0.1)

  • Rashmi Chourasia (a1) and O. P. Shrivastava (a1)


A novel concept of immobilization of light water nuclear reactor fuel reprocessing waste effluent through interaction with sodium zirconium phosphate (NZP) has been established. It was found that a large number of hazardous cations could be loaded in the NZP-based matrix without significant change of three-dimensional framework structure. Starting from the raw powder diffraction data of polycrystalline solid phases, crystal structure of substituted NZP phases has been investigated using the General Structure Analysis System (GSAS) package. Cation(s) substituted NZP phases crystallize in rhombohedral symmetry (space group R-3c and Z = 6). Powder diffraction data have been subjected to Rietveld refinement to reach satisfactory structural convergence of R-factors. Unit cell parameters, inter atomic distances, bond angles, reflecting planes (h, k, l), structure factors, polyhedral (ZrO6 and PO4) distortion, and particle size have been reported. PO4 stretching and bending vibrations in the Infra red (IR) region have been assigned. SEM and EDAX analysis provide analytical evidence of fixation of cations in the matrix.


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Bhuvneshwari, G. and Varadaraju, U. V. (1999). “Synthesis of new network phosphates with NZP structure,” J. Solid State Chem. 145, 227.
Bois, L., Guitter, M. J., Carrot, F., Trocellier, P., and Guatier-Soyer, M. (2001). “Preliminary results on the leaching process of phosphate ceramics, potential hosts for actinide immobilization,” J. Nucl. Mater. 297, 129137.
Breval, E., McKinstry, H. A., and Agrawal, D. K. (1998). “Synthesis and thermal expansion properties of the Ca(1+x)/2Sr(1+x)/2Zr4P6−2xSi2xO24 system,” J. Am. Ceram. Soc. 81, 9621032.
Carla, V., Garrido, F. M., Alves, O. L., Calle, P., Martinez Juarez, A., Iglesias, J. E., and Rojo, J. M. (1997). “Ionic conductivity and structural characterization of Na1.5Nb0.3Zr1.5(PO4)3 with NASICON-type structure,” Solid State Ion. 100, 127134.
Chakir, M., El Jazouli, A., and de Waal, D. (2006). “Synthesis, crystal structure and spectroscopy properties of Na3AZr(PO4)3 (A: Mg, Ni) and Li2.6Na0.4NiZr(PO4)3 phosphates,” J. Solid State Chem. 179, 18831891.
Govindan Kutty, K. V., Asuvathraman, R., and Sridharan, R. (1998). “Thermal expansion studies on the sodium zirconium phosphate family of compounds A1/2M2(PO4)3: effect of interstitial and framework cations,” J. Mater. Sci. 33, 40074013.
JCPDS Powder Diffraction Data File No. 71-0959. (2000). Compiled by International Center for Diffraction Data U.S.A.
Larson, A. C. and Von Dreele, R. B. (2000). General Structure Analysis System Technical Manual LANSCE, MS-H805, Los Alamos National University LAUR, 86748.
Petkov, V. I. and Orlova, A. I. (2003). “Crystal-chemical approach to predicting the thermal expansion of compounds in the NZP family,” Inorg. Mater. 39, 10131023.
Petkov, V. I., Orlova, A. I., Kazantsev, G. N., Samoilov, S. G., and Spiridonova, M. L. (2001). “Thermal expansion in the Zr and 1-, 2-valent complex phosphates of NaZr2(PO4)3 (NZP),” J. Thermal Anal. Calor. 66, 623632.
Rega, D. A., Agrawal, D. K., Huang, C. Y., and McKinstry, H. A. (1992). “Microstructure and microcracking behavior of barium zirconium phosphate (BaZr4P6O24) ceramics,” J. Mater. Sci. 27, 24062412.
Roger, H. M., Ruslan, P., and Liferovich, A. (2004). “Structural study of the perovskite series Ca1−xNaxTi1−xTaxO3,” J. Solid State Chem. 177, 44204427.
Shannon, R. D. (1976). “Effective ionic radii in oxides and fluorides,” Acta Crystallogr. A 32, 751.
Shrivastava, O. P. and Chourasia, R. (2008). “Crystal chemistry of sodium zirconium phosphate based simulated ceramic waste forms of effluent cations (Ba2+, Sn4+, Fe3+, Cr3+, Ni2+ and Si4+) from light water reactor fuel reprocessing plants,” J. Hazard. Mater. 153, 285292.
Tantri, S., Ushadevi, S., and Ramasesha, S. K. (2002). “High temperature X-ray studies on barium and strontium zirconium phosphate based low thermal expansion materials,” Mater. Res. Bull. 37, 11411147.
Terki, R., Bertrand, G., and Aourag, H. (2005). “The proceedings of the 2nd international symposium on nano and giga-challenges in microelectronics,” Microelectron. Eng. 81, 514523.
Varadaraju, M., Sugantha, U. V., and Subba Rao, G. V. (1994). “Synthesis and characterization of NZP phases, AM‘3+M“4+P3O12,” J. Solid State Chem. 111, 3340.
West, A. R. (2003). Solid State Chemistry and its Application (John Willey and Sons, Singapore), chapter A9, pp. 710.
Yoon, C. S., Kim, J. H., Kim, C. K., and Hong, K. S. (2001). “Synthesis of low thermal expansion ceramics based on CaZr4(PO4)6–Li2O system,” Mater. Sci. Eng. B 79, 610.



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