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Investigation of chromium oxide clusters grafted on SBA-15 using Cr-polycation sol

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Abstract

A comparative study of chromium oxide clusters grafted on mesoporous silica SBA-15 was carried out using samples synthesized by one-pot, impregnation and Cr-polycation sol grafting methods. The nature of CrOx species incorporated into SBA-15 by direct hydrothermal one-pot method as well as impregnation of Cr(NO3)3·9H2O and Cr-polycation precursors was characterized by XRD, BET isotherms, UV–Vis DRS, FTIR, TGA, O1s XPS, 29Si-MAS NMR, H2-TPR, NH3-TPD, SEM and TEM. Powder XRD did not show the presence of Cr2O3 in the calcined samples obtained by one-pot method. It, however, shows the rhombohedral clusters of α-Cr2O3 dispersed over SBA-15 for CrOx/SBA-15 samples prepared by impregnation and polycation sol grafting methods. The absorption band at 296 nm, observed for Cr3+ in solution, is absent for the aqueous Cr-polycation sol. There is evidence that the presence of chromium precursor in the reaction medium can influence the morphology of SBA-15 as seen in the SEM micrographs. Charge transfer transitions demonstrate the insertion of CrOx species on SBA-15 matrix synthesized by one-pot method. Cr-polycation grafted SBA-15 sample shows unique vibrational features at 573 and 624 cm−1 attributed to extra-framework CrOx species. The ratio of Cr6+/Cr3+ species present in CrOx/SBA-15 samples depends on the Cr-precursor employed for grafting on SBA-15. One-pot synthesized samples predominantly contain coordinated water (δH–O–H at 1,635 cm−1) on SBA-15 while impregnated samples show water molecules associated with CrOx species (δH–O–H at 1,594 cm−1).

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Acknowledgments

Financial support from DRDO, New Delhi, through Grant ERIP/ER/0600319/M/01/1052 is gratefully acknowledged. We thank SERC division of DST, Ministry of Science and Technology, New Delhi, for providing powder XRD, TGA, TPR/TPD and BET facilities (under FIST Schemes). We also thank Mr. A. Narayanan and Mrs. S. Srividya for data collection using these facilities.

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  1. Department of Chemistry, Indian Institute of Technology Madras, Chennai, 600 036, India

    P. Hari Krishna Charan & G. Ranga Rao

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  1. P. Hari Krishna Charan
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  2. G. Ranga Rao
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Correspondence to G. Ranga Rao.

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Hari Krishna Charan, P., Ranga Rao, G. Investigation of chromium oxide clusters grafted on SBA-15 using Cr-polycation sol. J Porous Mater 20, 81–94 (2013). https://doi.org/10.1007/s10934-012-9577-y

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