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Title: Influence of starting precursors and synthesis methods on the physiochemical properties of zirconia

Graphical abstract: Crystallite size of tetragonal phase of the zirconia samples prepared using different synthesis parameters and precursors as a function of calcination temperature. Surface area values of the zirconia samples calcined at 500 and 700 °C are in given brackets. - Highlights: • Zirconia prepared with modified sol–gel method is less stable compared with zirconia prepared by precipitation method. • Optimized synthesis conditions shifted the glow exotherm to higher temperature range indicating better thermal stability. • Tetragonal-zirconia could be synthesized in cost-effective manner using zirconium oxy-nitrate. • In our studies no co-relation between the surface area and crystallite size was observed. - Abstract: Under identical and judiciously pre-optimized synthesis conditions, the influence of different combinations of zirconium sources and/or post treatment conditions on structural properties, thermal stability, phase composition and morphology of zirconia has been investigated. High surface area tetragonal zirconia could be synthesized in a cost-effective manner from 1 M solution of zirconium oxy-nitrate at pH 11 using aqueous ammonia solution as a precipitant when calcined at 400 °C for 3 h. Irrespective of the preparation method, pH and starting precursor, zirconia samples prepared without digestion contained dominant monoclinic phase with some traces of tetragonal phase when calcinedmore » at 700 °C. Even though there is linear decrease in surface area with increase in the crystallite size for each sample as a function of calcination temperature, no co-relation between the surface area and crystallite size could be achieved. SEM images show agglomerated and irregular shape particles between 10 to 20 μm.« less
Authors:
 [1] ;  [1] ;  [2] ;  [1]
  1. Catalysis Division, National Chemical Laboratory, Pune 411008 (India)
  2. Department of Chemistry, University of Pune, Pune 411 007 (India)
Publication Date:
OSTI Identifier:
22348665
Resource Type:
Journal Article
Resource Relation:
Journal Name: Materials Research Bulletin; Journal Volume: 55; Other Information: Copyright (c) 2014 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; AMMONIA; CALCINATION; MONOCLINIC LATTICES; NITRATES; PARTICLES; PRECIPITATION; SCANNING ELECTRON MICROSCOPY; SOL-GEL PROCESS; SOLUTIONS; SURFACE AREA; SYNTHESIS; THERMAL GRAVIMETRIC ANALYSIS; ZIRCONIUM; ZIRCONIUM OXIDES