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AFM-Investigations , Structural Visualization Studies, and Temperature Optimization of Single Metal Cyclotetraphosphates Synthesized at Elevated Temperature

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Khaled M. Elsabawy , A. El-Maghraby
» doi: 10.17628/ECB.2012.1.223


The precursor metal dihydrogen phosphate dihydrate was synthesized by a rapid and simple precipitation method using phosphoric acid, cobalt nitrate at ambient temperature (cobalt(II) was selected as model for metal in these investigations). The precursor was heated and sintered at different temperatures (600, 800, 1000 and 1100 °C) respectively, to optimize the conditions to obtain Co2P4O12 crystal form with high purity. The products were monitored by both of XRD, IR spectra by additional to accurate imaging via scanning electron microscope (SEM) and AFM-microscope to analyze surface topology and microstructural features of the metal cyclotetraphosphate. Structural investigations via XRD proved that the product obtained at 1100°C is the best and have fine structure with monoclinic structure phase and C12/c1 space group with lattice parameter a = 11.809(2), b = 8.293(1), c = 9.923(2) Å, respectively. A visualized investigations were performed to confirm structure validity and stability at sintering temperature (1100 °C) . Visualization studies indicated that variations in bond distances between Co1, Co2, P1 and P2 and different six oxygen atoms (O1 ,O2 , O3 ,O4 ,O5 and O6) inside crystal lattice are responsible for increasing lattice flexibility factor (by controlling in shrinkage and expansion coefficient) and consequently increase its bonds stability to break .

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