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Synthesis, characterization, and reversible hydrogen sorption study of sodium-doped fullerene


Herein is presented a novel, straightforward route to the synthesis of an alkali metal-doped fullerene as well as a detailed account of its reversible and enhanced hydrogen sorption properties in comparison to pure C60. This work demonstrates that a reaction of sodium hydride with fullerene (C60) results in the formation of a sodium-doped fullerene capable of reversible hydrogen sorption via a chemisorption mechanism. This material not only demonstrated reversible hydrogen storage over several cycles, it also showed the ability to reabsorb over three times the amount of hydrogen (relative to the hydrogen content of NaH) under optimized conditions. The sodium-doped fullerene was hydrogenated on a pressure
composition temperature (PCT) instrument at 275 C while under 100 bar of hydrogen pressure. The hydrogen desorption behavior of this sodium-doped fullerene hydride was observed over a temperature range up to 375 C on the PCT and up to 550 C on the thermogravimetric analysis (TGA). Powder x-ray diffraction verifies the identity of this material as being Na6C60. Characterization of this material by thermal decomposition analysis (e.g. PCT and TGA methods), as well as FT-IR and mass spectrometry, indicates that the hydrogen sorption activity of this material is due to the reversible formation of a hydrogenated fullerene (fullerane). However, the reversible formation of fullerane was found to be greatly enhanced by the presence of sodium. It was also demonstrated that the addition of a catalytic amount of titanium (via TiO2 or Ti.OBu/4) further enhances the hydrogen sorption process of the sodium-doped fullerene material.