Synthesis, growth, structure and characterization of nickel(II)-doped hexaaquacobalt(II) dipotassium tetrahydrogen tetra-o-phthalate tetrahydrate crystals

Abstract

Single crystals of K2[Co(1−x)Nix(H2O)6] (C8H5O4)4·4H2O (x = 0.25) (PCNHP), a semiorganic black colored transparent crystal of size ∼20 × 13 × 4 mm3, are grown from an aqueous solution of potassium hydrogen phthalate enriched with cobalt chloride and nickel chloride by slow evaporation solution growth technique at room temperature. Structural analysis by single crystal X-ray diffraction reveals that the crystal belongs to monoclinic system with space group P21/c and the cell parameters are a = 10.41(3) Å, b = 6.84(2) Å, c = 29.46(9) Å, Z = 4. Incorporation of both Co(II) and Ni(II) into the potassium hydrogen phthalate (KHP) crystal lattice is well confirmed by EDS and chemical tests. Powder XRD profiles indicate the crystallinity and FT-IR studies reveal the vibrational patterns. The UV–vis optical absorption spectrum of PCNHP shows the lower optical cut-off at ∼300 nm and the crystal was transparent in the entire visible region. The crystalline perfection of the grown crystal analysed by high-resolution X-ray diffraction (HRXRD) analysis reveals that the diffraction curve (DC) contains multi-peaks with low angular spread indicating the possibility of low angle structural grain boundaries. Scanning electron microscope (SEM) studies indicate the structure defect centers. The dielectric, thermal and mechanical behaviors of the specimen were also investigated.