Journal
RSC ADVANCES
Volume 8, Issue 11, Pages 5882-5890Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c8ra00157j
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- Science and Engineering Research Board (SERB), the Department of Science and Technology (DST), New Delhi
- Madhya Pradesh Council of Science and Technology (MPCST), Bhopal
- Ministry of Science and Technology of Taiwan [MOST-103-2112-M-259-008-MY3]
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A thermal decomposition route with different sintering temperatures was employed to prepare non-stoichiometric nickel oxide (Ni1-delta O) from Ni(NO3)(2)center dot 6H(2)O as a precursor. The non-stoichiometry of samples was then studied chemically by iodometric titration, wherein the concentration of Ni3+ determined by chemical analysis, which is increasing with increasing excess of oxygen or reducing the sintering temperature from the stoichiometric NiO; it decreases as sintering temperature increases. These results were corroborated by the excess oxygen obtained from the thermo-gravimetric analysis (TGA). X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) techniques indicate the crystalline nature, Ni-O bond vibrations and cubic structural phase of Ni1-delta O. The change in oxidation state of nickel from Ni3+ to Ni2+ were seen in the X-ray photoelectron spectroscopy (XPS) analysis and found to be completely saturated in Ni2+ as the sintering temperature reaches 700 degrees C. This analysis accounts for the implication of non-stoichiometric on the magnetization data, which indicate a shift in antiferromagnetic ordering temperature (T-N) due to associated increased magnetic disorder. A sharp transition in the specific heat capacity at T-N and a shift towards lower temperature are also evidenced with respect to the non-stoichiometry of the system.
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