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  • Morphology, physical, and s...
    Srinivasa Rao, Linganaboina; Chennakesava Rao, B.; Battula, Sahith; Alla, Nived

    Inorganic chemistry communications, August 2024, 2024-08-00, Letnik: 166
    Journal Article

    Display omitted •SEM morphographs showed rise in grain size of the nanocompounds with ZnO content.•EDAX studies were corelated with radiation shielding properties of the samples.•XRD showed zinc-pyrophosphate (Zn2P2O7) and copper-pyrophosphate (Cu2P2O7) phases.•FTIR spectra identified ZnO4, CuO4 structural units along with PO4 units.•EPR spectra displayed hyperfine spectra of paramagnetic Cu2+ ions of CuO6 units. The inorganic nanocompounds were synthesized by solid state reaction with the composition 10Li2O+(30-x)Sb2O3 + xZnO + 59.5P2O5 + 0.5Cu (in mol%). SEM morphographs of the samples confirmed the grain size ≈0.5–2.5 μm. The EDAX spectra of the samples confirmed presence of copper (Cu) nanoparticles (<2 wt%) in the composition. The EDAX studies showed energy dispersion of Kα- photons by reactivity of elements P, Cu, and Zn, while the element Sb has shown dispersion of Lα- photons up to 10 keV. Mass attenuation coefficient (MAC) has exhibited a few discontinuities (bumps) at low energies (<10 keV) due to K, L- absorption edges of various elements (such as P, Cu, Zn, and Sb) presented in the samples. The shrinking of Phosphorous-Phosphorous separation (dP-P) from 4.716 Ao to 3.990 Ao indicated the greater solidity (or density) of the prepared nanocompounds at higher content of ZnO. XRD spectra showed the presence of major crystallites such as LiPO3, Li3PO4, Li6P6018, SbPO4, Cu3PO4, Cu2P2O7, Cu3PO42, ZnPO32, Zn2P2O7, ZnP4O11, and LiZnPO4 in the prepared nanocompounds. The average crystallite size was determined in the range of 35–83 nm. FTIR spectra of these compounds displayed the PO2−, PO3−, PO43−, and ZnO4 units along with linkages P─O─P, O─P─O, Sb─O─Sb, Cu─O─Cu, etc. A band due to vibrations of Cu─O bond has been observed in the range of 466–478 cm−1, which endorses the contribution of copper nanoparticles in the solid state reaction of the metal phosphate nanocompounds. A partially resolved hyperfine structure of magnetic resonance signals corresponding to g|| ≈2.4 and g⊥ ≈2.05 were observed due to the presence of an anisotropic hyperfine interaction of the electron spin (S = 1/2) with the nuclear spin (I = 3/2) of copper isotopes (63Cu and 65Cu) in the samples.