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Effect of Calcination Condition on Phase Formation Characteristics of NdBa2Cu3Oy Powder Prepared by Solidstate Reaction


Paper Type 
Contributed Paper
Title 
Effect of Calcination Condition on Phase Formation Characteristics of NdBa2Cu3Oy Powder Prepared by Solidstate Reaction
Author 
Paitoon Boonsong, Pimpilai Wannasut and Anucha Watcharapasorn*
Email 
anucha@stanfordalumni.org
Abstract:
The article details the solid-state synthesis of Nd-123 powder under a normal air atmosphere
using a stoichiometric ratio (i.e. Nd:Ba:Cu = 1:2:3) of high-purity Nd2O3, BaCO3 and CuO starting
powders. The as-calcined powder was analyzed using thermo-analytical (DSC/TGA) techniques. The
exotherm was related to the formation of Nd-123 which occurred around 850-920°C and, thereafter,
the sample melted. The calcination process of Nd-123 compound was carried out by heating the starting
precursors at 800-950°C for 12 h. Phase identification was determined using an X-ray diffractometer
(XRD) and the quantitative phase analysis was performed by fitting the XRD pattern using the
GSAS-II program. The morphology was observed by scanning electron microscopy (SEM) with
chemical composition identification from EDS mode. The result of XRD showed that NdBa2Cu3Oy
(Nd-123) was identified as the main crystalline phase along with other minor secondary phases when
the calcination temperature was 900°C. The approximated stoichiometry of the powder was Nd:Ba:Cu
= 1:2.09:3.16, which was very close to the expected nominal composition. Therefore, the calcination
temperature at 900°C was selected for further synthesis study by varying the calcination time (12,
18, 24 and 30 h). Particle size analysis indicated that the powders were consisted of irregular-shaped
particles linked together to form agglomerates. The particle size tended to increase with increasing
time of calcination process with a size range from 1.16±0.33 μm to 31.72 ±9.27 μm. The result of
fitting the XRD pattern showed that the sample re-calcined at 900°C for 24 h exhibited increased
weight fraction of Nd-123 with minimized concentration of secondary phases.
Start & End Page 
654 - 664
Received Date 
2019-07-26
Revised Date 
2019-10-10
Accepted Date 
2019-12-09
Full Text 
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Keyword 
NdBa2Cu3Oy, layered perovskite, thermo analytical method, solid-state synthesis, quantitative phase analysis
Volume 
Vol.47 No.4 (Special Issue II : July 2020)
DOI 
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Chiang Mai Journal of Science

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