doi: 10.17586/2226-1494-2015-15-5-789-795


A. E. Baranchikov, V. A. Maslov, S. V. Shcherbakov, V. A. Usachyov, N. E. Kononenko, P. P. Fedorov, K. V. Dukelskii

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For citation: Baranchikov A.E., Maslov V.A., Shcherbakov V.V., Usachyov V.A., Kononenko N.E., Fedorov P.P., Dukel’skiy K.V. Electron microscopic investigation of yttrium aluminum garnet powders Y3AL5O12, synthesized by sol–gel method. Scientific and Technical Journal of Information Technologies, Mechanics and Optics, 2015, vol. 15, no. 5, pp. 789–795.

Subject of Study. The paper presents results of characterization for neodymium doped yttrium aluminum garnet nanopowders - YAG:Nd3+ by the method of scanning electronic microscopy. Method. Synthesis of YAG:Nd3+ was carried out by sol-gel method from nitrate or acetate - nitrate solutions with addition of some organic compounds and ammonia as well. Such substances were used as the source ones: oxides of neodymium and yttrium with the content of the basic substance equal to 99.999 %; organic compounds: citric acid with the content of the basic substance not less than 99.0 %; ethylene glycol (99.5%); the ammonium lauryl sulfate (99.0 %); urea (99.0 %) of Alfa Aesar, Fluka, Aldrich companies. Oxides of yttrium and neodymium (5 at. %) were dissolved in 50% acetic acid, nitrate aluminum was added with a view to the resulting product Y2,85Nd0,15Al5,0O12, the solution was stirred and heated to 60С before reaching its transparency and uniformity. The weight of the portion corresponding to the stoichiometry YAG was 2.0 g. 50 % aqueous solutions of organic substances or 5% NH4OH in a weight ratio of 1:1 to the weight of the garnet were added in aqueous solutions, placed into glass cups. The solutions were thoroughly mixed first using a conventional stirrer, then on ultrasonic installation with simultaneous 60 С heating for 2 hours. Drying of solutions to the consistency of a powder or a thick gel was carried out at 110 С. Then the samples were placed into platinum cups and annealed in a tube furnace at 950 - 1050 С for the period from 0.5 to 2 hours. Additional annealing of the powders in the air at 950 - 1060С were carried out for the purpose of powders clarifying for residual amorphous carbon removal. Main Results. The synthesized powder precursors and powders after annealing were examined using a polarizing microscope to identify anisotropic crystalline phases. X-ray analysis of the synthesized samples was carried out on a DRON - 4 and UDR - 63 diffractometers, radiation λCu Kα. Carl Zeiss NVision 40 electron microscope was used for the study by scanning electron microscopy (SEM). The results indicate significant effects of additives in the original acetate - nitrate solutions on the size and morphology of the particles during the synthesis of powders of yttrium aluminum garnet by sol-gel method. Relatively large particles not susceptible to the mutual sintering were obtained by using ethylene glycol and ammonium lauryl sulfate as additives. Practical Relevance. Powders of yttrium aluminum garnet synthesized by the sol-gel method using ethylene glycol and ammonium lauryl sulfate as additives can be of the greatest interest for creation of YAG:Nd3+ laser ceramics.

Keywords: yttrium aluminum garnet, precursor, laser ceramics, nanopowders.

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