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- Acid-leaching (1)
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- Viscous sintering (1)
Organisationseinheit der BAM
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The nucleophilic substitution of fluorine of aromatic compounds with n-aminoalkyl trialkoxysilanes and consecutive sol-gel process have been used for the fabrication of various chromophoric sol-gel materials. The displacement of the fluoro substituent of an activated aromatic molecule occurs by a primary or secondary amino group of (CH3O)3Si-(CH2)3-NHR [R- = H-; CH3-, (CH3O)3Si-(CH2)3-] in tetraalkoxysilane or alcohol as solvent and the sol-gel process can be carried in the same vessel. The HF formed is trapped by a tertiary amine and simultaneously serves as the catalyst for the sol-gel process. Various aromatic compounds have been checked for this purpose: 1-(4-fluorophenyl)-2-nitroethylene, 1-(4-fluorophenyl)-2,2-dicyanoethylene, 4-fluorobenzonitrile, 4-fluoronitrobenzene, 4,4prime-difluorobenzophenone, 4,4prime-difluorobenzil, 7,7prime-difluorodibenzylideneacetone, tetrafluoro-p-benzoquinone, and 1,5-difluoro-2,4-dinitrobenzene. Mono and disubstitution has been studied by UV/Vis- and solid state NMR spectroscopy of the xerogels.
The process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down.