DOI: 10.17586/2226-1494-2015-15-4-578-586


J. A. Rozhnova, S. V. Kuznetsov, P. P. Fedorov, V. V. Voronov, V. A. Usachyov, N. E. Kononenko, D. . Khegai, K. V. Dukelskiy

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For citation: Rozhnova J.A., Kuznetsov S.V., Fedorov P.P., Voronov V.V., Usachyov V.A., Kononenko N.E., Khegai D.K., Dukel’skiy K.V. Preparation and characterization of strontium fluoride powders activated by neodymium fluoride. Scientific and Technical Journal of Information Technologies, Mechanics and Optics, 2015, vol.15, no. 4, pp. 578–586.

Subject of Study. The paper deals with preparation processes of ultradisperse, homogeneous powder Sr1-хNdхF2+х (х= 0.003-0.2), with use of ammonium fluoride as the fluorinating agent taken over 114-120 % from stoichiometry. Method. Nitrate of strontium, neodymium nitrate hexahydrate, with the content equal to 99. 99 % of the basic substance and ammonium fluoride were used as the source of substances. Activated powders of strontium fluoride were obtained by the method of deposition from aqueous solutions by washing the precipitate with a solution of ammonium fluoride, taken over 114 - 120% from stoichiometry. The washed precipitate was centrifuged for 5-7 min, dried in the air at 30-350 C. Heat treatment of the dried precipitate was carried out in two stages: the first stage at the temperature of 200- 2500 C for 0.5-1 hour, the second one at 550- 6000 C for 2-3 hours. X-ray analysis of the synthesized samples was carried out on a Bruker D8 Advance diffractometer, radiation Cu K. The size and shape measuring of the particles of activated strontium fluoride was carried out by means of electron microscope Carl Zeiss NVision 40. The content of neodymium in activated powders of strontium fluoride was determined by the method of spectral emission analysis on the device LEA - S500. Chemical analysis for determination of ammonium ion (NH4+) content in the obtained samples was performed by the method of Kjeldahl. Calculations of lattice parameters, size of coherent scattering regions and the values of micro-deformations were carried out by TOPAS program. Main Results. Preparation processes of ultradisperse, homogeneous powder Sr1-хNdхF2+х (х= 0.003-0.2), with use of ammonium fluoride as the fluorinating agent taken over 114-120 % from stoichiometry, provides obtaining the firm solution Sr1-x-yNdx(NH4)yF2+x-y of the cubic fluorite structure. It has been found out that the morphology and size of the resulting product depend on the quantity of excess ammonium fluoride. The changes in the morphology of the particles from nano – and microcubes to a plate shape were made clear by varying the quantity of excess ammonium fluoride from 114% to 120%. The particle size significantly decreased with increasing excess of ammonium fluoride from 114% to 120%. After heat treatment of the obtained powders agglomeration of cubic morphology particles to a size equal to 50-350 nm without changing their shape occurred. The plate-like particles have got a rounded shape after heat treatment with size between 50 and 200 nm. Practical Relevance. Obtained mixtures with ammonium fluoride excess over 114 % and 120 % are promising for use in the technology of ceramics by hot pressing.

Keywords: laser ceramics, powders.

Acknowledgements. The authors are grateful to A.E. Baranchikov (Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences), to V.K. Ivanov (Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences) for characterization of samples by the method of scanning electronic microscopy and to A. A. Luginina for d iscussion of results.

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