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Title: On the evolution of morphology of zirconium sponge during reduction and distillation

Abstract

High purity zirconium metal is produced by magnesio-thermic reduction of zirconium tetrachloride followed by vacuum distillation. The reduction process is carried out in a batch giving metal sponge and magnesium chloride in the reduced mass. The sponge is purified to using by vacuum distillation. The morphology of the sponge formed during the reduction and its influence on further processing has significant importance. In the present study, a detailed investigation involving evolution of the morphology of sponge particles and its implication during the vacuum distillation was carried out. The study of the microstructure was done using scanning electron microscopy and X-ray diffraction. It is observed that the nascent sponge formed is highly unstable which transforms to a needle-like morphology almost immediately, which further transforms to rounded and finally to a bulk shape. Faceting of the surface and needle-shape formation were observed in these particles, this is probably due to anisotropy in the surface energy. The morphology of the sponge formed during the reduction influences the distillation process. The fine needle-like shape sponge morphology leads to particle ejection, which is explained to be due to curvature effect. This is responsible for the formation of unwanted mass during distillation. XRD line broadening analysismore » indicates that the individual sponge particles are free from structural defects (dislocation) and are nearly single crystalline in nature.« less

Authors:
 [1]; ;  [2]
  1. Nuclear Fuel Complex, Hyderabad, 500 062 (India), E-mail: kapoork@nfc.ernet.in
  2. Nuclear Fuel Complex, Hyderabad, 500 062 (India)
Publication Date:
OSTI Identifier:
21062198
Resource Type:
Journal Article
Resource Relation:
Journal Name: Materials Characterization; Journal Volume: 59; Journal Issue: 3; Other Information: DOI: 10.1016/j.matchar.2006.12.015; PII: S1044-5803(07)00026-5; Copyright (c) 2007 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; ANISOTROPY; DISLOCATIONS; MAGNESIUM CHLORIDES; MICROSTRUCTURE; MONOCRYSTALS; MORPHOLOGY; REDUCTION; SCANNING ELECTRON MICROSCOPY; SURFACE ENERGY; VACUUM DISTILLATION; X-RAY DIFFRACTION; ZIRCONIUM; ZIRCONIUM CHLORIDES

Citation Formats

Kapoor, K., Padmaprabu, C., and Nandi, D. On the evolution of morphology of zirconium sponge during reduction and distillation. United States: N. p., 2008. Web. doi:10.1016/j.matchar.2006.12.015.
Kapoor, K., Padmaprabu, C., & Nandi, D. On the evolution of morphology of zirconium sponge during reduction and distillation. United States. doi:10.1016/j.matchar.2006.12.015.
Kapoor, K., Padmaprabu, C., and Nandi, D. Sat . "On the evolution of morphology of zirconium sponge during reduction and distillation". United States. doi:10.1016/j.matchar.2006.12.015.
@article{osti_21062198,
title = {On the evolution of morphology of zirconium sponge during reduction and distillation},
author = {Kapoor, K. and Padmaprabu, C. and Nandi, D.},
abstractNote = {High purity zirconium metal is produced by magnesio-thermic reduction of zirconium tetrachloride followed by vacuum distillation. The reduction process is carried out in a batch giving metal sponge and magnesium chloride in the reduced mass. The sponge is purified to using by vacuum distillation. The morphology of the sponge formed during the reduction and its influence on further processing has significant importance. In the present study, a detailed investigation involving evolution of the morphology of sponge particles and its implication during the vacuum distillation was carried out. The study of the microstructure was done using scanning electron microscopy and X-ray diffraction. It is observed that the nascent sponge formed is highly unstable which transforms to a needle-like morphology almost immediately, which further transforms to rounded and finally to a bulk shape. Faceting of the surface and needle-shape formation were observed in these particles, this is probably due to anisotropy in the surface energy. The morphology of the sponge formed during the reduction influences the distillation process. The fine needle-like shape sponge morphology leads to particle ejection, which is explained to be due to curvature effect. This is responsible for the formation of unwanted mass during distillation. XRD line broadening analysis indicates that the individual sponge particles are free from structural defects (dislocation) and are nearly single crystalline in nature.},
doi = {10.1016/j.matchar.2006.12.015},
journal = {Materials Characterization},
number = 3,
volume = 59,
place = {United States},
year = {Sat Mar 15 00:00:00 EDT 2008},
month = {Sat Mar 15 00:00:00 EDT 2008}
}