Authors:
Y. P. Naik Product Development Division, Radiochemistry and Isotope Group, Bhabha Atomic Research Centre, Mumbai 400085, India

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G. A. Ramarao Product Development Division, Radiochemistry and Isotope Group, Bhabha Atomic Research Centre, Mumbai 400085, India

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Ajita Banthiya Department of Chemistry, Banasthali University, Rajasthan 304022, India

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Deepika Chaudhary Department of Chemistry, Banasthali University, Rajasthan 304022, India

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Charu Arora Department of Chemistry, L.P. University, Jalandhar- Delhi G. T. Road (NH-1), Phagwara, Punjab 144402, India
Department of Chemistry, Banasthali University, Rajasthan 304022, India

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Abstract

GEL combustion technique was applied to obtain oxides of thorium and cerium from their respective nitrate solutions using citric acid as the gelating agent. The dried samples were characterized by IR and TG studies. Intermediate and final products during TG studies have been isolated and characterized by XRD studies. All the TG runs during heating of thorium and cerium nitrate with citric acid dried Gels showed a two step process. The weight loss at each step and the X-ray data of the product at each step, helped in suggesting a possible mechanism. Kinetic study was carried out independently for each step. The reaction mechanism as observed during interactive procedure was found to be diffusion controlled. The kinetic parameters (activation energy and pre-exponential factor) for each step in all reactions have been calculated. Observations from XRD studies show that with increase in cerium concentration in the oxides, the lattice parameter values have shown a decreasing trend for all the five compositions studied. It was observed that in TG studies with increase in cerium concentration, the final temperature of the reactions have shown a decreasing trend. SEM studies of the powders reveal that synthesized oxides have a tendency to form agglomerate of varying size ranging from 50 to 100 μm in case of mixed oxides but the size of thorium oxide powder so synthesized have pore size 10–100 μm. SEM images shows that GEL combustion may result in agglomeration, if the temperature is not properly controlled to the desired value. SEM studies also reveal that each agglomerate contains approximately 10–100 individual particles. Surface area of the mixed oxide powders were determined using Gas adsorption technique. The surface area was found to be in the range of 3–17 m2/g in all cases. Specific surface area of thorium oxide was found to be lesser than cerium oxide but in case of mixed oxides surface area decreases with increase in cerium content. Majority of pores, indicating the particle size are in the range of 0.01–0.04 cm3/g.

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation
1969
Volumes
per Year
1
Issues
per Year
24
Founder Akadémiai Kiadó
Founder's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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