Abstract
Mesoporous TiO2–octylphosphonate hybrid materials were prepared in one step by a nonhydrolytic sol–gel method involving the reaction of Ti(OiPr)4, acetophenone (2 equiv) and diethyl octylphosphonate (from 0 to 0.2 equiv) at 200 °C for 12 hours, in toluene. The different samples were characterized by 31P magic angle spinning nuclear magnetic resonance, Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, and nitrogen physisorption. For P/Ti ratios up to 0.1, the hybrid materials can be described as aggregated, roughly spherical, crystalline anatase nanoparticles grafted by octylphosphonate groups via Ti–O–P bonds. The crystallite size decreases with the P/Ti ratio, leading to an increase of the specific surface area and a decrease of the pore size of the hybrid samples. For a P/Ti ratio of 0.2, the volume fraction of organic octyl groups exceeds 50%. The hybrid material becomes nonporous and can be described as amorphous TiO2 clusters modified by octylphosphonate units, where the octyl chains form an organic continuous matrix.
Highlights
The development of porous hybrid organic–inorganic materials has been a major goal for materials scientists for more than 25 years [1,2,3]
We present an original one-step NHSG synthesis of mesoporous TiO2–octylphosphonate hybrid materials, using a nonhydrolytic sol–gel method involving the reaction of titanium tetraisopropoxide and diethyl octylphosphonate precursors at 200 °C in the presence of acetophenone as an oxygen donor
Elemental analysis by energy dispersive X-ray spectroscopy (EDX) of these materials showed that in all cases the measured P/Ti ratios were close to the nominal ones, indicating that all the octylphosphonate units were incorporated in the materials (Table 1)
Summary
The development of porous hybrid organic–inorganic materials has been a major goal for materials scientists for more than 25 years [1,2,3]. The reaction of alkoxides in acetophenone (used as a solvent and an oxygen donor) has already been described for the synthesis of TiO2 [33] and BaTiO3 [34] nanoparticles, but it has never been used to prepare mesoporous oxides or hybrid materials.
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