Communications
[12] Q. Lu, F. Gao, S. Komarneni, T. E. Mallouk, J. Am. Chem. Soc.
2004, 126, 8650.
[13] D. Wang, R. Kou, Z. Yang, J. He, Z. Yang, Y. Lu, Chem.
Commun. 2005, 166.
[14] B. Yao, D. Fleming, M. A. Morris, S. E. Lawrence, Chem. Mater.
2004, 16, 4851.
[15] K. Jin, B. Yao, N. Wang, Chem. Phys. Lett. 2005, 409, 172.
[16] A. Y. Ku, S. T. Taylor, S. M. Loureiro, J. Am. Chem. Soc. 2005,
127, 6934.
[17] A. Monnier, F. Schüth, Q. Huo, D. Kumar, D. Margolese, R. S.
Maxwell, G. D. Stucky, M. Krishnamurty, P. Petroff, A. Firouzi,
M. Janicke, B. F. Chmelka, Science, 1993, 261, 1299.
[18] J. Y. Cheng, A. M. Mayes, C. A. Ross, Nat. Mater. 2004, 3, 823.
[19] M. L. Cohen, Mater. Sci. Eng. C 2001, 15, 1.
[20] Y. Xia, P. Yang, Y. Sun, Y. Wu, B. Mayers, B. Gates, Y. Yin, F.
Kim, H. Yan, Adv. Mater. 2003, 15, 353.
Experimental Section
Preparation of the samples: The deposition mixtures were prepared
by applying a two-step synthesis procedure: First, tetraethyl ortho-
silicate (Aldrich; 2.08 g, 0.01 mol) was mixed with 0.2m HCl (3 g),
H2O (1.8 g), and EtOH (5 mL), and the mixture was heated at 608C
for 1 h to carry out acid-catalyzed hydrolysis–condensation of the
silica precursor. For the preparation of CTAB-containing deposition
mixtures, this solution was mixed with CTAB (0.644 g, 1.77 mmol for
sample CTAB1; or 0.947 g, 2.6 mmol for CTAB2) dissolved in EtOH
(10 mL). The Brij56-containing samples were prepared using Brij56
(0.906 g, 1.33 mmol dissolved in ethanol (15 mL) or 1.81 g, 2.65 mmol
dissolved in ethanol (30 mL) for samples B1–B3 and C1–C3,
respectively). For the preparation of the P123-containing solutions,
the prehydrolyzed silica was mixed with 5 wt% solutions of P123 in
ethanol: 15 mL (0.13 mmol P123 for sample D1–D3) or 20 mL
(0.17 mmol P123 for sample E1–E3). The AAMs (47 mm, Anodisc,
Whatman) with average pore diameters of 120–200 nm and a
thickness of approximately 60 mm were soaked with the prepared
mixtures of the precursor by distributing 0.75 mL of the solutions over
the whole membrane surface. After 3–5 h at room temperature and
under controlled humidity, the membrane appeared dry and homo-
geneously filled with the mixture.
Characterization of the embedded silica mesostructures: GI-
SAXS measurements were performed with a SAXSess small-angle X-
ray scattering system by Anton Paar after alignment of the X-ray
beam with the surface of the sample as shown in Figure 3. The
incident beam was shadowed with a circular beam stop, and the signal
was recorded on image plates after collecting the pattern for 1 h. The
TEM images were obtained with a JEOL 2010 transmission electron
microscope operating at 200 kV. Samples for electron microscopy
were prepared by the following method: 1) the alumina matrix was
dissolved in phosphoric acid to release the embedded mesoporous
silica; 2) plan views and cross-sections were prepared by dimple
grinding followed by Ar ion polishing. The elemental composition
and surface morphology of the samples were determined by SEM
using a JEOL JSM 6500F field emission scanning electron microscope
equipped with an Oxford EDX detector.
Received: September 16, 2005
Published online: January 3, 2006
Keywords: host–guest systems · membranes ·
.
mesoporous materials · surfactants · template synthesis
[1] A. P. Wight, M. E. Davis, Chem. Rev. 2002, 102, 3589.
[2] B. J. Scott, G. Wirnsberger, G. D. Stucky, Chem. Mater. 2001, 13,
3140.
[3] C. J. Brinker, Y. Lu, A. Sellinger, H. Fan, Adv. Mater. 1999, 11, 579.
[4] D. Grosso, F. Babonneau, P.-A. Albouy, H. Amenitsch, A. R.
Balkenende, A. Brunet-Bruneau, J. Rivory, Chem. Mater. 2002,
14, 931.
[5] M. Klotz, P.-A. Albouy, A. Ayral, C. Menager, D. Grosso, A.
van der Lee, V. Cabuil, F. Babonneau, C. Guizard, Chem. Mater.
2000, 12, 1721.
[6] G. Kickelbick, Small 2005, 1, 168 – 170.
[7] Z. Yang, Z. Niu, X. Cao, Z. Yang, Y. Lu, Z. Hu, C. C. Han,
Angew. Chem. 2003, 115, 4333 – 4335; Angew. Chem. Int. Ed.
2003, 42, 4201 – 4203.
[8] F. Marlow, I. Leike, C. Weidenthaler, C. W. Lehmann, U.
Wilczok, Adv. Mater. 2001, 13, 307 – 310.
[9] F. Kleitz, F. Marlow, G. D. Stucky, F. Schüth, Chem. Mater. 2001,
13, 3587.
[10] A. Yamaguchi, F. Uejo, T. Yoda, T. Uchida, Y. Tanamura, T.
Yamashita, N. Teramae, Nat. Mater. 2004, 3, 337.
[11] Y. Wu, G. Cheng, K. Katsov, S. W. Sides, J. Wang, J. Tang, G. H.
Fredrickson, M. Moskovits, G. D. Stucky, Nat. Mater. 2004, 3,
816.
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