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Synthesis of nanostructured SnO and SnO2 by high-energy milling of Sn powder with stearic acid

Published online by Cambridge University Press:  08 August 2013

Lizandro Manzato
Affiliation:
Instituto Federal de Educação, Ciência e Tecnologia do Amazonas, 1672 Distrito Industrial, Manaus, Amazonas 69075-351, Brazil
Daniela Menegon Trichês*
Affiliation:
Departamento de Física, Universidade Federal do Amazonas, Setor Norte, Av. Gen. Rodrigo Otávio Ramos, 3000, Coroado, Manaus, Amazonas 69077-000, Brazil
Sérgio Michielon de Souza
Affiliation:
Departamento de Física, Universidade Federal do Amazonas, Setor Norte, Av. Gen. Rodrigo Otávio Ramos, 3000, Coroado, Manaus, Amazonas 69077-000, Brazil
Marcelo Falcão de Oliveira
Affiliation:
Universidade de São Paulo, Escola de Engenharia de São Carlos, 13.560-970 São Carlos, SP, Brazil
*
a)Address all correspondence to this author. e-mail: menegon.d@gmail.com
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Abstract

The effects of stearic acid on the high-energy ball milling of tin powder have been investigated. The mean crystallite sizes, microstrain, and phase transformations were examined using different techniques like x-ray diffraction (XRD), Rietveld refinement method, and differential scanning calorimetry (DSC). After 28 h of milling, the Rietveld analysis showed the stabilization of Sn mean crystallite sizes at around 50 nm. Due to the presence of oxygen in stearic acid, the milling process gradually produced an amorphous Sn oxide phase. The DSC thermogram of the sample milled for 28 h showed two exothermic peaks separated by an endothermic peak. Based on the DSC measurements, two samples were annealed at 240 and 350 °C for 20 min. The annealing at 240 °C confirmed the presence of an amorphous phase which crystallized in nanostructured tetragonal SnO phase. The annealing at 350 °C revealed the nucleation of nanostructured tetragonal SnO2 phase.

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Articles
Copyright
Copyright © Materials Research Society 2013 

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