Under inert gas flow and high temperature, carbonization of aluminum‐based metal–organic frameworks (MOFs) was carried out. The formation rate of carbonized MOFs (CMOFs) was monitored by the variation of the Raman D band to G band intensity ratio with heat treatment duration. Powder x‐ray diffraction (PXRD) and scanning electron microscope (SEM) techniques were used to confirm the formation of CMOFs. The activation energy was extracted from the temperature‐dependent rate constants using the Arrhenius equation and correlated with the structural properties of precursor MOFs such as pore size and the number of carbon atoms per ligand. A reaction mechanism is proposed and discussed for the formation of CMOFs based on Raman observation. Copyright © 2016 John Wiley & Sons, Ltd.
The carbonization of various types of metal–organic frameworks (MOFs) was carried out under N2 gas flow and high temperature. The formation of carbonized MOFs (CMOFs) was monitored by Raman spectroscopy. In addition to the well-known D and G bands in Raman spectra, the salient G′ band feature was observed only in Mn-, Fe-, Co-, and Ni-containing CMOFs. On the other hand, CMOFs containing other metals (Al, Cr, V, Cu, and Zr) do not show the G′ band. Furthermore, the G′ band was also observed when we mixed the nitrate salts of Mn(II), Fe(III), and Co(II) with Al-containing MOFs using the same treatment conditions as in the formation of CMOFs. The G′ band is known to be related to the stacking order of graphitic layers. The presence of the Raman G′ band in CMOFs can be ascribed to the catalytic activity of Mn, Fe, Co, and Ni. The trend of the G′ band to G band intensity ratio resembles the “volcano curve” in the description of the behavior of catalytic activities of transition metals. The G′ bands in Mn-, Fe-, Co-, and Ni-containing CMOFs were well-fitted with two-component peaks which indicates that these CMOFs have well-stacked graphitic structures.
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