Magnetic field alignment of ordered silicate-surfactant composites and mesoporous silica

Science

Volumn 278, Issue 5336, 1997, Pages 264-268

  Tolbert, Sarah H ^a,b   Firouzi, Ali ^c   Stucky, Galen D ^b   Chmelka, Bradley F ^c  

^a UNIVERSITY OF CALIFORNIA   (United States)

^b UNIVERSITY OF CALIFORNIA   (United States)

^c University of California   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

SILICATE; SILICON DIOXIDE; SURFACTANT;

ARTICLE; CERAMICS; LIQUID CRYSTAL; MAGNETIC FIELD; MATERIALS; POLYMERIZATION; PRIORITY JOURNAL; SURFACE PROPERTY;

EID: 0030773001     PISSN: 00368075     EISSN: None     Source Type: Journal    
DOI: 10.1126/science.278.5336.264     Document Type: Article

References (62)

1. C. T. Kresge, M. E. Leonowitz, W. J. Roth, J. C. Vartuli, J. S. Beck, Nature 359, 710 (1992); J. S. Beck et al., J. Am. Chem. Soc. 114, 10834 (1992).
2. C. T. Kresge, M. E. Leonowitz, W. J. Roth, J. C. Vartuli, J. S. Beck, Nature 359, 710 (1992); J. S. Beck et al., J. Am. Chem. Soc. 114, 10834 (1992).
3. A. Firouzi et al., Science 267, 1138 (1995).
4. D. M. Antonelli, A. Nakahira, J. Y. Ying, Inorg. Chem. 35, 3126 (1996); D. M. Antonelli and J. Y. Ying, Chem. Mater. 8, 874 (1996); Angew. Chem. Int. Ed. Eng. 35, 426 (1996).
5. D. M. Antonelli, A. Nakahira, J. Y. Ying, Inorg. Chem. 35, 3126 (1996); D. M. Antonelli and J. Y. Ying, Chem. Mater. 8, 874 (1996); Angew. Chem. Int. Ed. Eng. 35, 426 (1996).
6. D. M. Antonelli, A. Nakahira, J. Y. Ying, Inorg. Chem. 35, 3126 (1996); D. M. Antonelli and J. Y. Ying, Chem. Mater. 8, 874 (1996); Angew. Chem. Int. Ed. Eng. 35, 426 (1996).
7. T. Abe, A. Taguchi, M. Iwamoto, Chem. Mater. 7, 1429 (1995); J. A. Knowles and M. J. Hudson, J. Chem. Soc. Chem. Commun. 1995, 2083 (1995); D. M. Antonelli and J. Y. Ying, Angew. Chem. Int. Ed. Eng. 34, 2014 (1995); U. Ciesla, S. Schacht, G. D. Stucky, K. K. Unger, F. Schüth, ibid. 35, 541 (1996); Z.-R. Tian et al., Science 276, 926 (1997).
8. T. Abe, A. Taguchi, M. Iwamoto, Chem. Mater. 7, 1429 (1995); J. A. Knowles and M. J. Hudson, J. Chem. Soc. Chem. Commun. 1995, 2083 (1995); D. M. Antonelli and J. Y. Ying, Angew. Chem. Int. Ed. Eng. 34, 2014 (1995); U. Ciesla, S. Schacht, G. D. Stucky, K. K. Unger, F. Schüth, ibid. 35, 541 (1996); Z.-R. Tian et al., Science 276, 926 (1997).
9. T. Abe, A. Taguchi, M. Iwamoto, Chem. Mater. 7, 1429 (1995); J. A. Knowles and M. J. Hudson, J. Chem. Soc. Chem. Commun. 1995, 2083 (1995); D. M. Antonelli and J. Y. Ying, Angew. Chem. Int. Ed. Eng. 34, 2014 (1995); U. Ciesla, S. Schacht, G. D. Stucky, K. K. Unger, F. Schüth, ibid. 35, 541 (1996); Z.-R. Tian et al., Science 276, 926 (1997).
10. T. Abe, A. Taguchi, M. Iwamoto, Chem. Mater. 7, 1429 (1995); J. A. Knowles and M. J. Hudson, J. Chem. Soc. Chem. Commun. 1995, 2083 (1995); D. M. Antonelli and J. Y. Ying, Angew. Chem. Int. Ed. Eng. 34, 2014 (1995); U. Ciesla, S. Schacht, G. D. Stucky, K. K. Unger, F. Schüth, ibid. 35, 541 (1996); Z.-R. Tian et al., Science 276, 926 (1997).
11. T. Abe, A. Taguchi, M. Iwamoto, Chem. Mater. 7, 1429 (1995); J. A. Knowles and M. J. Hudson, J. Chem. Soc. Chem. Commun. 1995, 2083 (1995); D. M. Antonelli and J. Y. Ying, Angew. Chem. Int. Ed. Eng. 34, 2014 (1995); U. Ciesla, S. Schacht, G. D. Stucky, K. K. Unger, F. Schüth, ibid. 35, 541 (1996); Z.-R. Tian et al., Science 276, 926 (1997).
12. G. Fu, C. Fyfe, W. Schwieger, G. T. Kokotailo, Angew. Chem. Int. Ed. Eng. 34, 1499 (1995).
13. P. T. Tanev and T. J. Pinnavaia, Science 267, 865 (1995).
14. P. Y. Feng, Y. Xia, J. L. Feng, X. H. Bu, G. D. Stucky, Chem. Commun. 1997, 949 (1997); D. Y. Zhao, Z. H. Luan, L. Kevan, ibid., p. 1009.
15. P. Y. Feng, Y. Xia, J. L. Feng, X. H. Bu, G. D. Stucky, Chem. Commun. 1997, 949 (1997); D. Y. Zhao, Z. H. Luan, L. Kevan, ibid., p. 1009.
16. Q. Huo, D. I. Margolese, G. D. Stucky, Chem. Mater. 8, 1147 (1996).
17. P. V. Braun, P. Osenar, S. I. Stupp, Nature 380, 325 (1996).
18. S. L. Burkett, S. D. Sims, S. Mann, Chem. Commun. 1996, 1367 (1996).
19. A. Sayari, Chem. Mater. 8, 1840 (1996).
20. T. Bein, ibid., p. 1636.
21. J. Caro et al., Adv. Mater. 4, 273 (1992).
22. G. D. Stucky and J. E. MacDougall, Science 247, 669 (1990).
23. C.-G. Wu and T. Bein, ibid. 266, 1013 (1994); ibid. 264, 1757 (1994).
24. C.-G. Wu and T. Bein, ibid. 266, 1013 (1994); ibid. 264, 1757 (1994).
25. Notable exceptions are the recent syntheses of mesoporous silicas as hard spheres, hollow spheres, sheets, and fibers. Transmission electron microscopy suggests that the pores in the sheets and hollow spheres are perpendicular to the film or sphere surfaces. The pores of the optically transparent fibers are parallel to the fiber axis [S. Schacht, Q. Huo, I. G. Voigt-Martin, G. D. Stucky, F. Schüth, Science 273, 768 (1996); Q. S. Huo, J. L. Feng, F. Schüth, G. D. Stucky, Chem. Mater. 9, 14 (1997); Q. S. Huo et al., Adv. Mater., in press].
26. Notable exceptions are the recent syntheses of mesoporous silicas as hard spheres, hollow spheres, sheets, and fibers. Transmission electron microscopy suggests that the pores in the sheets and hollow spheres are perpendicular to the film or sphere surfaces. The pores of the optically transparent fibers are parallel to the fiber axis [S. Schacht, Q. Huo, I. G. Voigt-Martin, G. D. Stucky, F. Schüth, Science 273, 768 (1996); Q. S. Huo, J. L. Feng, F. Schüth, G. D. Stucky, Chem. Mater. 9, 14 (1997); Q. S. Huo et al., Adv. Mater., in press].
27. Notable exceptions are the recent syntheses of mesoporous silicas as hard spheres, hollow spheres, sheets, and fibers. Transmission electron microscopy suggests that the pores in the sheets and hollow spheres are perpendicular to the film or sphere surfaces. The pores of the optically transparent fibers are parallel to the fiber axis [S. Schacht, Q. Huo, I. G. Voigt-Martin, G. D. Stucky, F. Schüth, Science 273, 768 (1996); Q. S. Huo, J. L. Feng, F. Schüth, G. D. Stucky, Chem. Mater. 9, 14 (1997); Q. S. Huo et al., Adv. Mater., in press].
28. 3 sponge phase as a glassy solid provides a 3D, random pore system with uniform pore dimensions [K. M. McGrath, D. M. Dabbs, N. Yao, I. A. Aksay, S. M. Gruner, Science 277, 552 (1997)].
29. H. Yang, A. Kuperman, N. Coombs, S. Mamiche-Afara, G. A. Ozin, Nature 379, 703 (1996); H. Yang, N. Coombs, I. Sakolov, G. A. Ozin, ibid. 381, 589 (1996).
30. H. Yang, A. Kuperman, N. Coombs, S. Mamiche-Afara, G. A. Ozin, Nature 379, 703 (1996); H. Yang, N. Coombs, I. Sakolov, G. A. Ozin, ibid. 381, 589 (1996).
31. I. A. Aksay et al., Science 273, 892 (1996).
32. S. H. Tolbert, T. E. Schäffer, J. Feng, P. K. Hansma, G. D. Stucky, Chem. Mater., in press.
33. R. Ganguli et al., Nature 389, 364 (1997).
34. A. Monnier et al., Science 261, 1299 (1993).
35. A. Firouzi, F. Atef, A. G. Oertli, G. D. Stucky, B. F. Chmelka, J. Am. Chem. Soc. 119, 3596 (1997); A. Firouzi, G. D. Stucky, B. F. Chmelka, in Synthesis of Microporous Materials, M. L. Occelli and H. Kessler, Eds. (Dekker, New York, 1996), pp. 379-389.
36. A. Firouzi, F. Atef, A. G. Oertli, G. D. Stucky, B. F. Chmelka, J. Am. Chem. Soc. 119, 3596 (1997); A. Firouzi, G. D. Stucky, B. F. Chmelka, in Synthesis of Microporous Materials, M. L. Occelli and H. Kessler, Eds. (Dekker, New York, 1996), pp. 379-389.
37. A. Firouzi, D. J. Schaefer, S. H. Tolbert, G. D. Stucky, B. F. Chmelka, J. Am. Chem. Soc. 119, 9466 (1997).
38. 2H NMR line shapes using the measured quadrupolar splitting of each Pake powder pattern as an input parameter and fitting both the fraction of oriented material in the sample and the width of the orientation distribution. A Gaussian distribution of domain directors about the uniaxial orientation direction was assumed (24). 26. This degree of alignment can be improved in many cases by slowly temperature cycling the sample through the anisotropic-to-isotropic transition in the presence of the applied magnetic field. In addition, the degree of orientation can be expected to be improved by an increase in the strength of the orienting magnetic field or by changes in the mixture composition, particularly the choice of the surfactant molecules and organic solutes (24). For example, recent experiments with the double-headed surfactant (p-phenylenedimethylene)bis(hexadecyl-dimethylammonium) dibromide [F. M. Menger and C. A. Littau, J. Am. Chem. Soc. 115, 10083 (1993)], which has a larger absolute molecular diamagnetic susceptibility than CTAB, have shown that a FWHM distribution of only 40° can be achieved with 76% of the hexagonal domains oriented parallel to the applied magnetic field.
39. A related procedure has been used by other researchers [C. A. Fyfe and G. Fu, J. Am. Chem. Soc. 117, 9709 (1995)].
40. Oriented fractions were calculated by comparison of scaled integrated diffraction intensities for the on-and off-axis 30° integrations in Fig. 3. We scaled on-axis integrations by numerically integrating a 30° slice of a 49° (uncalcined) or 53° (calcined) Gaussian (FWHM); we scaled off-axis integrations by using a 30° slice of an isotropic scattering ring.
41. 2.
42. o) of 0.9837. Pore-size distributions were determined by the Barrett-Joyner-Halenda (BJH) method. The accuracies of the BJH and BET methods in this small size regime are limited, and, therefore, the resulting pore-size distributions and surface areas should be considered approximate.
43. (100) spacing of 30 Å corresponds to a lattice constant a of 2d√3 or 35 Å.
44. L. Powers and P. S. Pershan, Biophys. J. 20, 137 (1977); L. Powers and N. A. Clark, Proc. Natl. Acad. Sci. U.S.A. 72, 840 (1977); G. G. Barclay, S. G. McNamee, C. K. Ober, K. I. Papathomas, D. W. Wang, J Polym. Sci. Part A Polym. Chem. 30, 1845 (1992); M. Lukaschek, D. A. Grabowski, C. Schmidt, Langmuir 11, 3590 (1995); J. A. Müller, R. S. Stein, H. H. Winter, Rheol. Acta 35, 160 (1996).
45. L. Powers and P. S. Pershan, Biophys. J. 20, 137 (1977); L. Powers and N. A. Clark, Proc. Natl. Acad. Sci. U.S.A. 72, 840 (1977); G. G. Barclay, S. G. McNamee, C. K. Ober, K. I. Papathomas, D. W. Wang, J Polym. Sci. Part A Polym. Chem. 30, 1845 (1992); M. Lukaschek, D. A. Grabowski, C. Schmidt, Langmuir 11, 3590 (1995); J. A. Müller, R. S. Stein, H. H. Winter, Rheol. Acta 35, 160 (1996).
46. L. Powers and P. S. Pershan, Biophys. J. 20, 137 (1977); L. Powers and N. A. Clark, Proc. Natl. Acad. Sci. U.S.A. 72, 840 (1977); G. G. Barclay, S. G. McNamee, C. K. Ober, K. I. Papathomas, D. W. Wang, J Polym. Sci. Part A Polym. Chem. 30, 1845 (1992); M. Lukaschek, D. A. Grabowski, C. Schmidt, Langmuir 11, 3590 (1995); J. A. Müller, R. S. Stein, H. H. Winter, Rheol. Acta 35, 160 (1996).
47. L. Powers and P. S. Pershan, Biophys. J. 20, 137 (1977); L. Powers and N. A. Clark, Proc. Natl. Acad. Sci. U.S.A. 72, 840 (1977); G. G. Barclay, S. G. McNamee, C. K. Ober, K. I. Papathomas, D. W. Wang, J Polym. Sci. Part A Polym. Chem. 30, 1845 (1992); M. Lukaschek, D. A. Grabowski, C. Schmidt, Langmuir 11, 3590 (1995); J. A. Müller, R. S. Stein, H. H. Winter, Rheol. Acta 35, 160 (1996).
48. L. Powers and P. S. Pershan, Biophys. J. 20, 137 (1977); L. Powers and N. A. Clark, Proc. Natl. Acad. Sci. U.S.A. 72, 840 (1977); G. G. Barclay, S. G. McNamee, C. K. Ober, K. I. Papathomas, D. W. Wang, J Polym. Sci. Part A Polym. Chem. 30, 1845 (1992); M. Lukaschek, D. A. Grabowski, C. Schmidt, Langmuir 11, 3590 (1995); J. A. Müller, R. S. Stein, H. H. Winter, Rheol. Acta 35, 160 (1996).
49. P. A. Winsor, in Liquid Crystals and Plastic Crystals, G. W. Gray and P. A. Winsor, Eds. (Ellis Harwood, Chichester, UK, 1974), vol. 2, pp. 122-143; K. Amundson, E. Helfand, X. Quan, S. D. Hudson, S. D. Smith, Macromolecules 27, 6559 (1994).
50. P. A. Winsor, in Liquid Crystals and Plastic Crystals, G. W. Gray and P. A. Winsor, Eds. (Ellis Harwood, Chichester, UK, 1974), vol. 2, pp. 122-143; K. Amundson, E. Helfand, X. Quan, S. D. Hudson, S. D. Smith, Macromolecules 27, 6559 (1994).
51. A. M. Figueredo Neto and L. Q. Amaral, Mol. Cryst. Liq. Cryst. 74, 109 (1981).
52. H. Gutman, Z. Luz, E. J. Wachtel, R. Poupko, J. Charvolin, Liq. Cryst. 7, 335 (1990); M. Jansson, R. L. Thurmond, T. P. Trouard, M. F. Brown, Chem. Phys. Lipids 54, 157 (1990); H. Gutman, A. Loewenstein, Z. Luz, R. Poupko, H. Zimmermann, Liq. Cryst. 9, 607 (1991); W. Schnepp, S. Disch, C. Schmidt, ibid. 14, 843 (1993).
53. H. Gutman, Z. Luz, E. J. Wachtel, R. Poupko, J. Charvolin, Liq. Cryst. 7, 335 (1990); M. Jansson, R. L. Thurmond, T. P. Trouard, M. F. Brown, Chem. Phys. Lipids 54, 157 (1990); H. Gutman, A. Loewenstein, Z. Luz, R. Poupko, H. Zimmermann, Liq. Cryst. 9, 607 (1991); W. Schnepp, S. Disch, C. Schmidt, ibid. 14, 843 (1993).
54. H. Gutman, Z. Luz, E. J. Wachtel, R. Poupko, J. Charvolin, Liq. Cryst. 7, 335 (1990); M. Jansson, R. L. Thurmond, T. P. Trouard, M. F. Brown, Chem. Phys. Lipids 54, 157 (1990); H. Gutman, A. Loewenstein, Z. Luz, R. Poupko, H. Zimmermann, Liq. Cryst. 9, 607 (1991); W. Schnepp, S. Disch, C. Schmidt, ibid. 14, 843 (1993).
55. H. Gutman, Z. Luz, E. J. Wachtel, R. Poupko, J. Charvolin, Liq. Cryst. 7, 335 (1990); M. Jansson, R. L. Thurmond, T. P. Trouard, M. F. Brown, Chem. Phys. Lipids 54, 157 (1990); H. Gutman, A. Loewenstein, Z. Luz, R. Poupko, H. Zimmermann, Liq. Cryst. 9, 607 (1991); W. Schnepp, S. Disch, C. Schmidt, ibid. 14, 843 (1993).
56. Q. Huo and G. D. Stucky, manuscript in preparation.
57. Q. Huo, R. Leon, P. M. Petroff, G. D. Stucky, Science 268, 1324 (1995).
58. G. S. Attard, J. C. Glyde, C. G. Göltner, Nature 378, 366 (1995).
59. Some cationic surfactant is expelled from the composite as the anionic silica charge density is reduced because of polymerization (22). The crystalline CTAB peaks are oriented because the plate-like crystals tend to lie flat on the surfaces of the bulk composite.
60. Powder Diffraction File entry 80-1746 (International Center for Diffraction Data, Newtown Square, PA, 1992).
61. P. I. Ravikovitch, S. C. Odomhnaill, A. V. Neimark, F. Schüth, K. K. Unger, Langmuir 11, 4765 (1995).
62. Supported by NSF grants CHE-9626523 (S.H.T.), DMR-9520971 (G.D.S.), and DMR-9257064 (B.F.C.); the U.S. Army Research Office (DAAH04-96-1-0443); a Henkel Foundation-American Chemical Society Research Fellowship in Colloid and Surface Chemistry (A.F.); the David and Lucile Packard Foundation (B.F.C.); and Shell Research B.V. (B.F.C.). This work made use of instrumentation supported in part by the NSF Division of Materials Research under grant DMR-922257 and through the University of California, Santa Barbara, Materials Research Laboratory under award DMR-9632716. B.F.C. is a Camille and Henry Dreyfus Teacher-Scholar and an Alfred P. Sloan Research Fellow.