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KMID : 1059520170610010029
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Journal of the Korean Chemical Society
2017 Volume.61 No. 1 p.29 ~ p.33
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Formation of Au Particles in Cu2?xICu2IIO3?δ (x ? 0.20; δ ? 0.10) Oxide Matrix by Sol-Gel Growth
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Das Bidhu Bhusan
Palanisamy Kuppan
Venugopal Potu
Sandeep Eesam
Kumar Karrothu Varun
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Abstract
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Formation of Au particles in nonstoichiometric Cu2?x ICu2 IIO3?δ (x ? 0.20; δ ? 0.10) oxide from aniline + hydrochloric acid mixtures and chloroauric acid in the ratios 30 : 1; 60 : 1; 90 : 1 (S1-S3) by volume and 0.01 mol of copper acetate, Cu(OCOCH3)2.H2O, in each case is performed by sol-gel growth. Powder x-ray diffraction (XRD) results show Au particles are dispersed in tetragonal nonstoichiometric dicopper (I) dicopper (II) oxides, Cu2?x ICu2 IIO3?δ (x ? 0.20; δ ? 0.10). Average crystallite sizes of Au particles determined using Scherrer equation are found to be in the approximate ranges ~85?140 A, ~85?150 A and ~80?150 A in S1-S3, respectively which indicate the formation of Au nano-micro size particles in Cu2?x ICu2 IIO3?δ (x ? 0.20; δ ? 0.10) oxides. Hysteresis behaviour at 300 K having low loop areas and magnetic susceptibility values ~ 5.835×10?6 ?9.889×10?6 emu/gG in S1-S3 show weakly ferromagnetic nature of the samples. Broad and isotropic electron paramagnetic resonance (EPR) lineshapes of S1-S4 at 300, 77 and 8 K having giso-values ~2.053±0.008?2.304±0.008 show rapid spin-lattice relaxation process in magnetic Cu2+ (3d9) sites as well as delocalized electrons in Au (6s1) nano-micro size particles in the Cu2?x ICu2 IIO3?δ (x ? 0.20; δ ? 0.10) oxides. Broad and weak UV-Vis diffuse reflectance optical absorption band ~725 nm is assigned to 2B1g→ 2A1g transitions, and the weak band ~470 nm is due to 2B1g→ 2Eg transitions from the ground state 2B1g (|dx 2 -y 2>) of Cu2+ (3d9) ions in octahedral coordination having tetragonal distortion.
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KEYWORD
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Sol-gel growth, Powder X-ray diffraction, Hysteresis loop, Electron paramagnetic resonance (EPR)
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