Triblock Copolymer Syntheses of Mesoporous Silica with Periodic 50 to 300 Angstrom Pores
Tóm tắt
Use of amphiphilic triblock copolymers to direct the organization of polymerizing silica species has resulted in the preparation of well-ordered hexagonal mesoporous silica structures (SBA-15) with uniform pore sizes up to approximately 300 angstroms. The SBA-15 materials are synthesized in acidic media to produce highly ordered, two-dimensional hexagonal (space group
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Tài liệu tham khảo
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D. Zhao et al. in preparation.
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Pluronic poly(alkylene oxide) triblock copolymers are a trademarked product of BASF Mt. Olive NJ.
The EO 106 PO 70 EO 106 triblock copolymer yields an Im3̅m cubic ( a 0 = 176 Å) silica mesostructure. The cubic phase assignments for silica-copolymer composites formed using EO 100 PO 39 EO 100 and EO 80 PO 30 EO 80 are based on 3D TEM studies. The space group is not yet assigned.
D. Zhao J. Feng B. F. Chmelka G. D. Stucky data not shown.
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The average pore sizes estimated from the TEM image contrasts in Figs. 4 A and B are slightly less than those determined from XRD and N 2 adsorption measurements.
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For example for a calcined hexagonal SBA-15 sample with a pore size of 60 Å BET surface area of 780 m 2 /g and a pore volume of 0.80 cm 3 /g (Table 1) hydrothermal treatment in boiling water for 24 hours yields a material with an essentially identical XRD pattern a pore size of 64 Å BET surface area of 690 m 2 /g and a pore volume of 0.79 cm 3 /g.
D. Zhao N. Melosh B. F. Chmelka G. D. Stucky data not shown.
A Netzsch Thermoanalyzer STA 409 was used for thermal analysis of the solid products simultaneously performing TGA and DTA with heating rates of 5 K min –1 in air.
Firouzi A., Schaefer D. J., Tolbert S. H., Stucky G. D., Chmelka B. F., J. Am. Chem. Soc. 119, 9466 (1997) ;
Supported by NSF under grants DMR-9520971 (G.D.S.) and DMR-9257064 (B.F.C.) the U.S. Army Research Office under grant DAAH04-96-1-0443 and the David and Lucille Packard Foundation (B.F.C.). We made use of UCSB Materials Research Laboratory Central Facilities supported by NSF under award DMR-9632716. B.F.C. is a Camille and Henry Dreyfus Teacher-Scholar and an Alfred P. Sloan Research Fellow. We thank BASF (Mt. Olive NJ) for providing block copolymer surfactants.