Structure of Silica Xerogels Synthesized with Organoalkoxysilane Co-reactants Hints at Multiple Phase Separation

2006 ◽  
Vol 110 (15) ◽  
pp. 7757-7765 ◽  
Author(s):  
Cédric J. Gommes ◽  
Monika Basiura ◽  
Bart Goderis ◽  
Jean-Paul Pirard ◽  
Silvia Blacher
2000 ◽  
Vol 15 (9) ◽  
pp. 1998-2005 ◽  
Author(s):  
G. Mountjoy ◽  
J. S. Rigden ◽  
R. Anderson ◽  
G. W. Wallidge ◽  
R. J. Newport ◽  
...  

The small-angle x-ray scattering (SAXS) technique was used to investigate inhomogeneities on the scale of 10 to 600 Å in acid-catalyzed titania–silica and zirconia–silica xerogels. SAXS of (TiO2)x(SiO2)1−x and (ZrO2)x(SiO2)1−x xerogels with x < 0.1, in which there was no phase separation, showed the presence of two types of inhomogeneity. For Q < 0.05 Å−1 there was a clear departure from Porod scattering which showed that xerogel powder particle surfaces were rough. For 0.1 < Q < 0.4 Å−1 there was a plateau feature corresponding to micropores within the silica-based network, and this feature changes with heat treatment. SAXS of xerogels with x > 0.3 showed the presence of phase-separated regions of metal oxide, which were initially amorphous and crystallized at higher temperatures. A (TiO2)0.18(SiO2)0.82 xerogel that was not initially phase separated became phase separated after heat treatment at 750 °C due to reduced solubility of Ti in the silica network.


Author(s):  
P. Echlin ◽  
M. McKoon ◽  
E.S. Taylor ◽  
C.E. Thomas ◽  
K.L. Maloney ◽  
...  

Although sections of frozen salt solutions have been used as standards for x-ray microanalysis, such solutions are less useful when analysed in the bulk form. They are poor thermal and electrical conductors and severe phase separation occurs during the cooling process. Following a suggestion by Whitecross et al we have made up a series of salt solutions containing a small amount of graphite to improve the sample conductivity. In addition, we have incorporated a polymer to ensure the formation of microcrystalline ice and a consequent homogenity of salt dispersion within the frozen matrix. The mixtures have been used to standardize the analytical procedures applied to frozen hydrated bulk specimens based on the peak/background analytical method and to measure the absolute concentration of elements in developing roots.


Author(s):  
J. Tong ◽  
L. Eyring

There is increasing interest in composites containing zirconia because of their high strength, fracture toughness, and its great influence on the chemical durability in glass. For the zirconia-silica system, monolithic glasses, fibers and coatings have been obtained. There is currently a great interest in designing zirconia-toughened alumina including exploration of the processing methods and the toughening mechanism.The possibility of forming nanocrystal composites by a phase separation method has been investigated in three systems: zirconia-alumina, zirconia-silica and zirconia-titania using HREM. The morphological observations initially suggest that the formation of nanocrystal composites by a phase separation method is possible in the zirconia-alumina and zirconia-silica systems, but impossible in the zirconia-titania system. The separation-produced grain size in silica-zirconia system is around 5 nm and is more uniform than that in the alumina-zirconia system in which the sizes of the small polyhedron grains are around 10 nm. In the titania-zirconia system, there is no obvious separation as was observed in die alumina-zirconia and silica-zirconia system.


Author(s):  
Oleg Bostanjoglo ◽  
Peter Thomsen-Schmidt

Thin GexTe1-x (x = 0.15-0.8) were studied as a model substance of a composite semiconductor film, in addition being of interest for optical storage material. Two complementary modes of time-resolved TEM were used to trace the phase transitions, induced by an attached Q-switched (50 ns FWHM) and frequency doubled (532 nm) Nd:YAG laser. The laser radiation was focused onto the specimen within the TEM to a 20 μm spot (FWHM). Discrete intermediate states were visualized by short-exposure time doubleframe imaging /1,2/. The full history of a transformation was gained by tracking the electron image intensity with photomultiplier and storage oscilloscopes (space/time resolution 100 nm/3 ns) /3/. In order to avoid radiation damage by the probing electron beam to detector and specimen, the beam is pulsed in this continuous mode of time-resolved TEM,too.Short events ( <2 μs) are followed by illuminating with an extended single electron pulse (fig. 1c)


1998 ◽  
Vol 95 (2) ◽  
pp. 131-135 ◽  
Author(s):  
DOUGLAS HENDERSON DEZSO BODA KWONG-YU CHAN
Keyword(s):  

1998 ◽  
Vol 77 (2) ◽  
pp. 333-340 ◽  
Author(s):  
A. Fontana, F. Rossi, G. Carini, G. D'

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