Abstract
A series of aminopropyl-silica-magnesia hybrid materials has been prepared by the sol–gel method from tetraethoxysilane (TEOS), magnesium chloride (MgCl2) and aminopropyltriethoxysilane (APTES) under acid conditions. The APTES:TEOS ratio was varied between 0:1 and 1:0. The aminopropyl coverage concentrations for APTES-silica-Mg samples were in the range of 0.3–2.3 mmol g−1. The hybrid materials were characterized by numerous techniques, including X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), Fourier transform Raman spectroscopy (FT-Raman), solid-state 13C and 29Si nuclear magnetic resonance (13C- and 29Si-NMR), thermogravimetry (TGA), N2 adsorption–desorption, small-angle X-ray scattering (SAXS), and scanning electron microscopy (SEM). The increase of APTES content in the silica network resulted in the increase of six-membered siloxane rings. The hybrid systems were shown to be formed from fully-condensed, trifunctional APTES species. The porosity and morphology of the hybrid materials were influenced by the initial TEOS/APTES ratio. The radius of gyration of the primary particles, determined by SAXS, was between 1.1 and 2.9 nm.
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References
Schubert U, Hüsing N (2005) Synthesis of inorganic materials. Wiley, Weinheim
Macan J, Tadanaga K, Tatsumisago M (2010) J Sol-Gel Sci Technol 53:31–37
Li S, Shah A, Hsieh AJ, Haghighat R, Praveen S, Mukherjee I, Wei E, Zhang Z, Wei Y (2007) Polymer 48:3982–3989
Vansant EF, Van Der Voort P, Vrancken KC (1995) Characterization and chemical modification of the silica surface. Elsevier, Amsterdam
Brinker CJ, Scherer GW (1990) Sol–gel science. Academic Press, NewYork
Wu Z, Xiang H, Kim T, Chun M, Lee K (2006) J Colloid Interface Sci 304:119–124
Lee B, Kim Y, Lee H, Yi J (2001) Microporous Mesoporous Mater 50:77–90
Araki S, Doi H, Sano Y, Tanaka S, Miyake Y (2009) J Colloid Interface Sci 339:382–389
Shi BF, Wang YS, Guo YL, Wang YQ, Wang Y, Guo Y, Zhang ZG, Liu XH, Lu GZ (2009) Catal Today 148:184–188
Sartori G, Bigi F, Maggi R, Sartorio R, Macquarrie DJ, Lenarda M, Storaro L, Coluccia S, Martra G (2004) J Catal 222:410–418
Lopez T, Llanos ME, Navarrete J, Schifter I, Salas P, Gomez R (1997) J Sol–Gel Sci Technol 8:321–325
Katayama S, Iwata K, Kubo Y, Yamada N (2003) J Sol–Gel Sci Technol 26:397–401
Lopez T, Gomes R, Llanos ME, López-Salinas E (1999) Mater Lett 38:283–288
Yamamoto K (2009) Appl Catal A 368:65–70
Brambilla R, Radtke C, dos Santos JHZ, Miranda MSL (2009) J Sol–Gel Sci Technol 51:70–77
Müller CA, Schneider M, Mallat T, Baiker A (2000) Appl Catal A 201:253–261
Samantary SK, Parida K (2005) Catal Commun 6:578–581
Photong S, Boonamnuayvitaya V (2009) J Env Sci 21:1741–1746
Ilavsky J, Jemian PR (2009) J Appl Crystallogr 42:347–353
Beaucage G (1995) J Appl Crystallogr 28:717–728
Beaucage G (1996) Appl Crystallogr 29:134–146
D’Acquarica I (2000) J Pharm Biomed Anal 23:3–13
Brambilla R, Pires GP, dos Santos JHZ, Miranda MSL, Chornik BJ (2007) Electron Spectrosc Relat Phenom 156–158:413–420
Kallury KMR, Macdonald PM, Thompson M (1994) Langmuir 10:492–499
Caravajal GS, Leyden DE, Quinting GR, Maciel GE (1998) Anal Chem 60:1776–1786
Pursch M, Brindle R, Ellvanger A, Sander LC, Bell CM, Handel H, Albert K (1997) Solid State Nucl Magn Reson 9:191–201
Bereznitski Y, Jaroniec M (1998) J Chromatogr A 828:51–58
Legrand AP, Hommel H, d’Espinose de la Caillerie JB (1999) Colloids Surf A 158:157–163
Pesek JJ, Matyska MT, Yu RJ (2002) J Chromatogr A 947:195–203
Bruch MD, Fatunmbi HO (2003) J Chromatogr A 1021:61–70
Capel-Sanchez MC, Barrio L, Campos-Martin JM, Fierro LG (2004) J Colloid Interface Sci 277:146–153
Luan Z, Fournier JA, Wooten JB, Miser DE (2005) Microporous Mesoporous Mater 83:150–158
Wiberg N, Holleman A, Wiberg E (2001) Holleman–Wiberg’s inorganic chemistry. Academic Press, New York
Fidalgo A, Iharco LM (2004) Chem Eur J 10:392–398
Fidalgo A, Ciriminna R, Ilharco LM, Pagliaro M (2005) Chem Mater 17:6686–6694
Gregg SJ, Sing KW (1982) Adsorption, surface area and porosity. Academic, New York
Unger K, Becker N, Roumeliotis P (1976) J Chromatogr 125:115–127
Zdravkov BD, Čermák JJ, Šefara M, Janků J (2007) Central European J Chem 5(2):385–395
Cardoso MB, Luckarift HR, Urban VS, Neill H, Johnson GR (2010) Adv Funct Mat 20(18):3031–3038
Capeletti LB, Bertotto FL, dos Santos JHZ, Moncada E, Cardoso MB (2010) Sens Act B 151:169–176
Acknowledgments
R. Brambilla thanks CNPq for a graduate fellowship. This work was financed by operating and travel grants from the CNPq (Brazil) and the NSERC (Canada). The authors are grateful to the LNLS for the SAXS measurements (Project SAXS1-8043).
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Brambilla, R., Poisson, J., Radtke, C. et al. Sol–gel preparation of aminopropyl-silica-magnesia hybrid materials. J Sol-Gel Sci Technol 59, 135–144 (2011). https://doi.org/10.1007/s10971-011-2471-2
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DOI: https://doi.org/10.1007/s10971-011-2471-2