Hydrothermal and postsynthesis surface modification of cubic, MCM-48, and ultralarge pore SBA-15 mesoporous silica with titanium
The authors describe the introduction of titanium centers to cubic MCM-48 was hydrothermally prepared with a gemini surfactant that favors the cubic phase and leads to a high degree of long-range pore ordering. This phase was chosen due to its high surface area (1100--1300 m{sup 2}/g) and its three-dimensional, bicontinuous pore array. SBA-15, synthesized with a block copolymer template under acidic conditions, has a surface area from 600 to 900 m{sup 2}/g and an average pore diameter of 69 {angstrom}, compared to 24--27 {angstrom} for MCM-48. Alkoxide precursors of titanium were used to prepare samples of Ti-MCM-48 and Ti-SBA-15. The authors have detailed the bulk and molecular structure of both the silica framework and the local bonding environment of the titanium ions within each matrix. X-ray powder diffraction and nitrogen adsorption shows the pore structure is maintained despite some shrinkage of the pore diameter at high Ti loadings by grafting methods. UV-visible and Raman spectroscopy indicate that grafting produces the least amount of Ti-O-Ti bonds and instead favors isolated tetrahedral and octahedral titanium centers. High-resolution photoacoustic FTIR spectra demonstrated the presence of intermediate range order within the silicate walls of MCM-48, established the consumption of surface silanols to form Si-O-Ti bonds by grafting, and resolved the characteristic IR absorbance at 960 cm{sup {minus}1}, occurring in titanium silicates, into two components. All three spectroscopic techniques, including in situ Raman, reveal the reactive intermediates formed when the materials are contacted with hydrogen peroxide.
- Research Organization:
- Univ. of California, Santa Barbara, CA (US)
- OSTI ID:
- 20075547
- Journal Information:
- Chemistry of Materials, Vol. 12, Issue 4; Other Information: PBD: Apr 2000; ISSN 0897-4756
- Country of Publication:
- United States
- Language:
- English
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