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Published on: March 27, 2018
Lamellar α‑Titanium Phosphate Modified with Magnesium Sulfate: Effects on Structural, Thermal, Morphological, and
Gerson Alberto Valencia Albitres1, Carlos Magno Fialho Soares1, Enzo Erbisti Garcia1
1Instituto de Macromoléculas Professora Eloisa Mano, Centro de Tecnologia, Bloco J, Universidade Federal do Rio de Janeiro, Ilha do Fundão, Rio de Janeiro 21941-598, Brazil.
Abstract:
Broadly speaking, hierarchically structured materials are those in which their structural regularity in different length scales can permit the enhancement of their multifunctional properties. α-Titanium phosphate (α-TiP) is considered like a material with a hierarchical arrangement. In this context, this study intended to investigate the effect of the incorporation of magnesium sulfate (MgSO4) on α-TiP physicochemical properties. α-TiP was synthesized using titanium isopropoxide and phosphoric acid. Either synthesized or intercalated with ethylamine aqueous solution, MgSO4 was added into ETiP via solvent-based and dry handling mixing routes. Structural, thermal, morphological, and electrochemical properties were analyzed. X-ray diffraction revealed that the presence of an ethylamine aqueous solution influenced the interlamellar layer of phosphate. The route of MgSO4 intercalation induced variation on its amount inside the phosphate galleries as seen by SEM/EDS. A possible interaction between magnesium salt and ethylamine through hydrogen bond formation was hypothesized. Raman spectroscopy indicated spectral changes depending on the route of magnesium salt incorporation. Spin-lattice (T1H) and spin-spin (T2H) time relaxations revealed that the role of ethylamine aqueous solution as an intercalator was crucial on the phosphate molecular mobility after addition of MgSO4. Electrochemical impedance showed that the ETiP/EMgSO4 sample showed the best Nyquist and Bode diagrams. Plot of current versus voltage indicated that solvent-based sample ETiP/EMgSO4 showed electrical conductivity while that named dry handling mixing αTiP/MgSO4(MF) is an insulator. The ETiP/EMgSO4 sample exhibited lower impedance around 2 to 3 orders of magnitude lower than precursors. Ethylamine aqueous solution played a key role in modulating phosphate properties and MgSO4 mobility within the phosphate matrix.