Synthesis, characterization of Sr-Gd nanocomposites doped with zirconium possessing electrical and optical properties Vinayak Adimule, and Adarsh K. S.
Citation: AIP Conference Proceedings 1989, 030001 (2018); doi: 10.1063/1.5047719 View online: https://doi.org/10.1063/1.5047719 View Table of Contents: http://aip.scitation.org/toc/apc/1989/1 Published by the American Institute of Physics
Synthesis, Characterization of Sr-Gd Nanocomposites doped with Zirconium possessing electrical and Optical properties Vinayak Adimule1,*and Adarsh KS2 1
Department of Chemistry, Jain College of Engineering and Technology (JCET), Sainagar, Unkal, Hubli- 580031, Karnataka, India, 2 Department of Physics, Jain College of Engineering and Technology (JCET), Sainagar, Unkal, Hubli580031, Karnataka, India *
[email protected]
Abstract We report here, a set of newly synthesized perovskite oxide nanomaterials that has been prepared through co precipitation method. Primary objective is synthesis of strontium-gadolinium nanocomposites doped with appropriate different concentrations of zirconium and investigation of their various electrical and optical properties. The composite materials were prepared by co precipitation method with general composition of Sr0.5 Gd0.3 (ZrO2) x moles, thus obtained hybrid nanomaterials were calcinated, characterized by XRD, FT-IR, UV-Vis spectroscopy and SEM. Here we have doped ZrO2 to Strontium-Gadolinium perovskite hybrid nanooxide multicomponent pure isolated material with different concentrations (1-5 molar %). The dielectric constants of the pelletalized samples have been examined at room temperature. The precursor material for the synthesis is strontium carbonate and gadolinium chloride which were reduced in presence of surfactant triethanol amine (TEA) .The aqueous mixture of reddish brown coloured hybrid metal hydroxides are filtered, washed with ethanol-water mixture (1:9 volume) to remove any impurities present with the precipitate, the precipitate is dried at 50-100°C, further heat treated at 650-750°C and obtained pure nanocomposite. Scanning electron microscopic studies revealed that the doped ZrO2 grain size was 30-50nm in diameter and it’s over layer is 90% optically transparent. XRD pattern demonstrated the formation of tetragonal zirconia and dopant addition considerably does not affect the crystal structure. Higher dielectric constants were obtained with larger grain size of the hybrid nanocomposites. Keywords: Perovksite, Nanocomposite, Zirconium oxide, Co precipitation, Dielectric Constant PACS: Replace this text with PACS numbers; choose from this list: http://www.aip.org/pacs/index.html
INTRODUCTION Novel nanocomposites of strontium and gadolinium hybrid materials were reported for their dielectric, transistor, semiconductor and fluorescent characteristics [1-3]. In the present research ZrO2 is doped further to the pure isolated Sr-Gd nanocomposite mixture to enhance electrical and optical properties[4-6]. Zirconium perovskite materials shown to exhibit dielectric, magnetic, optical properties. It is envisaged that by adding different molar ratios of the zirconium to the hybrid nanomaterials enhances dielectric properties [7-9]. The perovskite oxide mixture synthesized through co- precipitation methods. Strontium carbonate and gadolinium chloride were used as starting materials ammonium hydroxide as gelation agent (P H >12) during the co precipitation high basicity is maintained to form the gel network The Sr-Gd hybrid nanocomposites were obtained by using triethanol amine as surfactant which is added to reduce the perovskite oxide materials in presence of urea and concentrated HCl under reflux condition [10-11]. The reddish brown precipitate thus obtained is further doped with zirconium (1-5%), the hybrid material was filtered, dried and calcinated and obtained pure nanocrystals. The crystals were studied for their dielectric and optical characteristics. Literature reports showed that Nanocomposites of Sr-Gd possessing various optical, electrical and electronic properties [12-13]. The material showed considerable increase in the voltage gain under the influence of magnetic field.
MATERIALS AND METHODS All the rare earth chemical, solvents and reagents were purchased from Sigma Aldrich chemicals, SD-fine and spectrochem ltd and used without purification. co-precipitation method is used to synthesize the hybrid nanomaterials. All the synthesized nanocomposites were characterized by UV-Vis, FTIR, XRD in Poornaprajna Scientific Industrial Research, Bangalore, SEM Images were recorded in IISc, Bangalore, Karnataka, India. The electrical and optical properties were recorded at Jain College of Engineering and Technology. Emerging Technologies: Micro to Nano (ETMN-2017) AIP Conf. Proc. 1989, 030001-1–030001-4; https://doi.org/10.1063/1.5047719 Published by AIP Publishing. 978-0-7354-1705-2/$30.00
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EXPERIMENTAL Synthesis of Strontium Nanocomposites Strontium carbonate (0.5 mole) is added with TEA (triethanol amine) in presence of concentrated HCl and refluxed for 8 h in an RB flask. The refluxing RM (Reaction Mixture) is added with gadolinium chloride (0.3 mole) and stirred at that temperature for 4-5h, urea (1-2 equivalents) were further added to the RM and reflux was continued for 3h. The RM was allowed to stir overnight. The reduced Sr-Gd hybrid nanocomposites were precipitated by adding concentrated solution of NH 4OH drop wise and to form the gel network and to undergo the polymerization reaction of complete gel formation in 36-48h. The entire mass was concentrated, washed with water and ethanol water and dried, calcinated at 650 0C and obtained pure Sr-Gd nanocomposites. Purification and Isolation of Sr-Gd Nanocomposites The crude hybrid nanocomposites of Sr-Gd was taken in a 25 ml RB flask added with 1:9 volume of ethanol water mixture and warmed in a water bath, the dissolved solid was cooled slowly and re precipitated by adding pet ether drop wise, the precipitate was filtered, the filtered solid was further given with THF solvent wash and calcinated at 600 0C to get the pure Sr-Gd nanocomposite. Doping of Zirconium to Sr-Gd Nanocomposites In a RB flask Zirconium oxide powder (1-5 molar %) was added with concentrated HCl under reflux condition in presence of excess of urea and TEA used as surfactant. The reaction mixture was refluxed further for 10h, cooled and the precipitated solid was added with Sr-Gd nanocomposite, which was made collapsing network with ammonium hydroxide and the precipitate was dried, the zirconium was doped with 1-4% to the mixture of Sr-Gd nanocomposites which is initially dissolved in TEA and washed with diethyl ether followed by recrystallised in ethanol water mixture processed to obtain the desired zirconium doped with strontium and gadolinium nanocomposites. Dielectric Properties Critical current density is measured with respect to the doped and undoped hybrid nanocomposites at different elevated temperatures in presence of magnetic field. The doped material shows considerable increase in the current density as compared with the undoped Sr-Gd nanocomposites. Current gain is maximum for the 5% Zr doped nanocomposite as compared with the 1-4% Zr doped Sr-Gd nanocomposite. Presence of magnetic field current increases exponentially with the doped hybrid nanocomposite. The undoped Sr-Gd nanocomposite shows differential distribution of the current as compared with the doped nanocomposites.
FIGURE 1: SEM Image of 1% Zr Doped Nanocomposites
FIGURE 2: SEM Image of 4 % Zr Doped Nanocomposites
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FIGURE 4: SEM Image of 5% Zr Doped
FIGURE 3: SEM Image of 3% Zr
Nanocomposites.
Doped Nanocomposites.
FIGURE 5: Show the variation of critical current density of the Zr doped Sr-Gd nanocomposite with undoped nanocomposite at different magnetic field.
RESULTS AND DISCUSSION In this research work we have synthesized Sr-Gd nanocomposites doped with 1-5% concentrations of zirconium and studied for their dielectric related properties. The synthesis of undoped and Zr-doped nanocomposites the composites are synthesized by co precipitation methods, isolated, purified and obtained the SEM images of doped assembly of Sr-Gd nanocomposites. Spectroscopic studies showed that ZrO2 grain size was 30-50 nm in diameter and it’s over layer is 90% optically transparent.XRD pattern demonstrated the formation of tetragonal zirconia and dopant addition does not affect the crystal structure. Current gain is maximum for the 5% Zr doped nanocomposite as compared with the 1-4% Zr doped Sr-Gd nanocomposite. Presence of magnetic field current increases exponentially with the doped hybrid nanocomposite. Higher dielectric constants were obtained with larger grain size of the nanocomposites. Further studies are in progress.
ACKNOWLEDGMENTS Authors are thankful to Jain College of Engineering and Technology for giving platform for this work to carry out. Authors are also thankful to IISc, Bangalore for providing the spectral and analytical data.
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