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Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia.

Ward AJ, Pujari AA, Costanzo L, Masters AF, Maschmeyer T - Nanoscale Res Lett (2011)

Bottom Line: A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route.The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy.Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

View Article: PubMed Central - HTML - PubMed

Affiliation: Laboratory for Advanced Catalysis for Sustainability, School of Chemistry, The University of Sydney, Bldg, F11, Sydney, NSW 2006, Australia. th.maschmeyer@chem.usyd.edu.au.

ABSTRACT
A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

No MeSH data available.


High-angle X-ray diffraction patterns of the prepared sulphated zirconia-silica materials.
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Figure 2: High-angle X-ray diffraction patterns of the prepared sulphated zirconia-silica materials.

Mentions: The lack of a significant peak at low angle suggests little long-range mesostructure in the material [21,53]. The diminution in peak intensity compared to the purely siliceous material 1 is attributable to the decrease in pore size and the filling of the mesopores with zirconium oxide nanoparticles at the highest loadings. The absence of additional absorptions at low angle indicates that there is no ordering within the silica. The high-angle (2θ > 10°) X-ray diffraction patterns of the mesoporous SZ-SiO2 materials 2 to 9 (Figure 2) reveal a broad peak from 20° to 35° 2θ which is due to the amorphous nature of the silica support. In the case of 8 and 9, this peak is significantly broadened compared to that observed for materials 2 to 6, and this broadness may be due to the significant amounts of zirconium that have been incorporated into the silica framework. In all cases, there is no diffraction associated with a crystalline phase of ZrO2, indicating no bulk crystalline zirconia is present.


Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia.

Ward AJ, Pujari AA, Costanzo L, Masters AF, Maschmeyer T - Nanoscale Res Lett (2011)

High-angle X-ray diffraction patterns of the prepared sulphated zirconia-silica materials.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3211248&req=5

Figure 2: High-angle X-ray diffraction patterns of the prepared sulphated zirconia-silica materials.
Mentions: The lack of a significant peak at low angle suggests little long-range mesostructure in the material [21,53]. The diminution in peak intensity compared to the purely siliceous material 1 is attributable to the decrease in pore size and the filling of the mesopores with zirconium oxide nanoparticles at the highest loadings. The absence of additional absorptions at low angle indicates that there is no ordering within the silica. The high-angle (2θ > 10°) X-ray diffraction patterns of the mesoporous SZ-SiO2 materials 2 to 9 (Figure 2) reveal a broad peak from 20° to 35° 2θ which is due to the amorphous nature of the silica support. In the case of 8 and 9, this peak is significantly broadened compared to that observed for materials 2 to 6, and this broadness may be due to the significant amounts of zirconium that have been incorporated into the silica framework. In all cases, there is no diffraction associated with a crystalline phase of ZrO2, indicating no bulk crystalline zirconia is present.

Bottom Line: A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route.The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy.Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

View Article: PubMed Central - HTML - PubMed

Affiliation: Laboratory for Advanced Catalysis for Sustainability, School of Chemistry, The University of Sydney, Bldg, F11, Sydney, NSW 2006, Australia. th.maschmeyer@chem.usyd.edu.au.

ABSTRACT
A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

No MeSH data available.