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Abstract

Preparation and properties of hierarchically structured porous silica monoliths have been discussed from the viewpoint of their application as continuous microreactors for liquid-phase synthesis of fine chemical in multi kilogram scales. The results of recent topical papers published by two research teams of Institute of Chemical Engineering Polish Academy of Sciences (ICE) and Department of Chemical Engineering and Process Design, Chemical Faculty, Silesian University of Technology (SUT) have been analyzed to specify the governing traits of microreactors. It was concluded that even enhancement factor of 100 in activity, seen in enzyme catalyzed reactions, can be explained by a proportional reduction of its physical constraints, i.e. huge enhancement of external mass transfer and micromixing. It is induced by very chaotic flows of liquid in tens of thousands of waving connected channels of ca. 25–50 mm in diameter, present in the skeleton. The scale of enhancement in the case of less active catalysts was smaller, but still large enough to consider the most practical applications.

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Authors and Affiliations

Julita Mrowiec-Białoń
Agnieszka Ciemięga
Katarzyna Maresz
Katarzyna Szymańska
Wojciech Pudło
Andrzej B. Jarzębski
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Abstract

One of the ways to decrease thermal conductivity is nano structurization. Cobalt triantimonide (CoSb3) samples with added indium or tellurium were prepared by the direct fusion technique from high purity elements. Ingots were pulverized and re-compacted to form electrodes. Then, the pulsed plasma in liquid (PPL) method was applied. All materials were consolidated using rapid spark plasma sintering (SPS). For the analysis, methods such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) with a laser flash apparatus (LFA) were used. For density measurement, the Archimedes’ method was used. Electrical conductivity was measured using a standard four-wire method. The Seebeck coefficient was calculated to form measured Seebeck voltage in the sample placed in a temperature gradient. The preparation method allowed for obtaining CoSb3 nanomaterial with significantly lower thermal conductivity (10 Wm–1K–1 for pure CoSb3 and 3 Wm–1K–1 for the nanostructured sample in room temperature (RT)). The size of crystallites (from SEM observations) in the powders prepared was about 20 nm, joined into larger agglomerates. The Seebeck coefficient, α, was about –200 µVK–1 in the case of both dopants, In and Te, in microsized material and about –400 µVK–1 for the nanomaterial at RT. For pure CoSb3, α was about 150 µVK–1 and it stood at –50 µVK–1 for nanomaterial at RT. In bulk nanomaterial samples, due to a decrease in electrical conductivity and inversion of the Seebeck coefficient, there was no increase in ZT values and the ZT for the nanosized material was below 0.02 in the measured temperature range, while for microsized In-doped sample it reached maximum ZT = 0.7 in (600K).

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Authors and Affiliations

R. Zybała
M. Schmidt
K. Kaszyca
M. Chmielewski
M.J. Kruszewski
M. Jasiński
M. Rajska
Ł. Ciupiński

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