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Title: Structural study and phase transition investigation in a simple synthesis of porous architected-ZnO nanopowder

In this work, zinc oxide powder with a rectangular-shaped porous architecture, made of numerous spherical nanometric particles, was obtained. A simple precipitation/decomposition procedure was used comprising a zinc oxalate intermediate, obtained from zinc sulfate and oxalic acid without any additives. Detailed studies on zinc oxalate dehydration, decomposition and zinc oxide formation, were carried out using in-situ temperature X-ray diffraction and thermogravimetric analysis. During the investigation, the temperature dependence of particle sizes, lattice parameters and crystal structures of ZnC{sub 2}O{sub 4}·2H{sub 2}O, ZnC{sub 2}O{sub 4} and ZnO nanopowders were analyzed from room temperature to 450 °C. Structural transitions were also discussed. The structure and morphology of the as-prepared ZnO nanopowder were investigated by electron microscopy and compared to the crystalline rectangular shape of ZnC{sub 2}O{sub 4}·2H{sub 2}O. The calcination temperature, counter ion and precipitate agent were found to be related to the product's shape and diameter. Spherical ZnO nanoparticles with diameters of less than 20 nm and a maximum specific surface of 53 m{sup 2}/g were obtained using this method. Highlights: • ZnO nanopowders with porous architecture were synthesized by a simple method. • Spherical ZnO nanoparticles confined in submicronic rectangular shape are obtained. • Crystal structures are determined temperature in-situmore » XRD up to 450 °C. • Structural transitions were analyzed.« less
Authors:
;
Publication Date:
OSTI Identifier:
22288704
Resource Type:
Journal Article
Resource Relation:
Journal Name: Materials Characterization; Journal Volume: 86; Other Information: Copyright (c) 2013 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; CALCINATION; CRYSTAL STRUCTURE; LATTICE PARAMETERS; NANOSTRUCTURES; PARTICLE SIZE; PHASE DIAGRAMS; PHASE TRANSFORMATIONS; POROUS MATERIALS; POWDERS; PRECIPITATION; SYNTHESIS; TEMPERATURE DEPENDENCE; THERMAL GRAVIMETRIC ANALYSIS; X-RAY DIFFRACTION; ZINC; ZINC OXIDES; ZINC SULFATES