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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.%.

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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.


HRTEM images of the prepared SZ-SiO2 samples 7 to 9. a Dark field image of silica 7 (26.89 wt.% Zr). b Silica 8 (27.77 wt.% Zr). c Silica 9 (41.40 wt.% Zr).
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Figure 4: HRTEM images of the prepared SZ-SiO2 samples 7 to 9. a Dark field image of silica 7 (26.89 wt.% Zr). b Silica 8 (27.77 wt.% Zr). c Silica 9 (41.40 wt.% Zr).

Mentions: The dark field and HRTEM images of several of the sulphated zirconia-silica samples are shown in Figure 4. Dark field images show strong atomic number (Z) contrast, thus allowing heavier elements to be visualized. Hence, the dark field image of 7 (Figure 4a) shows the dispersion of the Zr atoms within the silicon matrix and is representative of similar images obtained for materials 8 and 9 (not shown). In all of the TEM images, small crystalline particles associated with the walls of the silica surface are observable. In the case of silica 7, it was very difficult to observe the very small crystalline ZrO2 particles in the HRTEM, but careful analysis of the electron diffraction pattern clearly indicates that polydispersed ZrO2 particles are present. From the diffraction pattern, it is evident that the material is polycrystalline with some crystal orientation evident. The HRTEM images of 8 and 9 clearly show the crystalline phase of ZrO2 on the surface of the silica, with the particles being in the size range of 5 to 10 nm.


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)

HRTEM images of the prepared SZ-SiO2 samples 7 to 9. a Dark field image of silica 7 (26.89 wt.% Zr). b Silica 8 (27.77 wt.% Zr). c Silica 9 (41.40 wt.% Zr).
© Copyright Policy - open-access
Related In: Results  -  Collection

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getmorefigures.php?uid=PMC3211248&req=5

Figure 4: HRTEM images of the prepared SZ-SiO2 samples 7 to 9. a Dark field image of silica 7 (26.89 wt.% Zr). b Silica 8 (27.77 wt.% Zr). c Silica 9 (41.40 wt.% Zr).
Mentions: The dark field and HRTEM images of several of the sulphated zirconia-silica samples are shown in Figure 4. Dark field images show strong atomic number (Z) contrast, thus allowing heavier elements to be visualized. Hence, the dark field image of 7 (Figure 4a) shows the dispersion of the Zr atoms within the silicon matrix and is representative of similar images obtained for materials 8 and 9 (not shown). In all of the TEM images, small crystalline particles associated with the walls of the silica surface are observable. In the case of silica 7, it was very difficult to observe the very small crystalline ZrO2 particles in the HRTEM, but careful analysis of the electron diffraction pattern clearly indicates that polydispersed ZrO2 particles are present. From the diffraction pattern, it is evident that the material is polycrystalline with some crystal orientation evident. The HRTEM images of 8 and 9 clearly show the crystalline phase of ZrO2 on the surface of the silica, with the particles being in the size range of 5 to 10 nm.

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.