Abstract:Silica xerogels were synthesized and annealed at 1000 degrees C for different durations to yield stable silica materials. The samples were prepared through base-catalyzed hydrolysis and condensation of tetramethyl orthosilicate in methanol. After aging and drying steps, clear and solid xerogels exhibiting a narrow pore size distribution were achieved. The annealing treatment of these xerogels was performed at 1000 degrees C and proved in the present study to lead to a monolithic glass when a progressive heat-t… Show more
“…Note that, for such heat treatment, silica-titania waveguides may not be completely densified [17]. On the other hand, a faster densification of the sol-gel derived materials has been claimed to occur in the presence of silver [18], which may also have contributed to the PL enhancement. Extending the heat treatment from 2 to 6 min at 700°C, the PL signal ratio, between waveguides with and without silver, was reduced from $57 to $3 times only.…”
“…Note that, for such heat treatment, silica-titania waveguides may not be completely densified [17]. On the other hand, a faster densification of the sol-gel derived materials has been claimed to occur in the presence of silver [18], which may also have contributed to the PL enhancement. Extending the heat treatment from 2 to 6 min at 700°C, the PL signal ratio, between waveguides with and without silver, was reduced from $57 to $3 times only.…”
“…The SEM micrographs of the samples heat treated at 1000°C reveal that the silicate matrix undergo a profound structural change reminding a silica foam (Fig. 10) [20].…”
Section: Study Of Crystallization Behaviour Using Xrd and Semmentioning
“…Given the high sensitivity of the 23 Na nuclei, it is relatively easy to deconvolute the central resonance lines in order to extract the relative ratio between the crystalline and mobile phases (Fig. 7).…”
Section: Solid-state Nmr Approachmentioning
confidence: 99%
“…7). Taking into account the 23 Na magnetisation distributed in the satellite transitions, we nd that, for the sample studied, 25% of the SNP complexes are in a 'liquid like' state. Since we know from our previous study that water molecules can easily exchange between the matrix pores and the atmosphere, we also decided to study the effect of hydration on the conned nanoparticles.…”
Transparent mesoporous silica monoliths of well-controlled porosity and a narrow pore size distribution around 6 nm have been used to prepare sodium nitroprusside (SNP) nanocomposites. The obtained nanomaterials could be characterised using X-ray total scattering coupled to atomic pair distribution function analysis (PDF) and solid-state NMR spectroscopy. The PDF analysis allows for a structural description of the confined species, as well as for the identification of the various coexisting phases: SNP isolated molecules and SNP crystalline nanoparticles. The model obtained suggests that the nanocrystals have the same molecular structure as the bulk crystalline material and measure about 6 nm in diameter.This result is quite exceptional because the space available inside the pores is only about ten times the size of the molecules. The multi-nuclei solid state NMR investigation confirms the structural model proposed by the PDF analysis and assigns the isolated molecules to the dynamic disorder of a solvated phase. The latter approach additionally provides quantitative information on the relative ratio between the dynamic molecules and the rigid nanocrystals. This result is exploited to study the evolution of the two confined SNP phases with respect to solvating water molecules. We show that the confined SNP nanocrystals can be easily dissolved when storing the nanocomposites at increasing atmospheric relative humidity.
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