The past 15 years have seen an astonishing increase in Nuclear Magnetic Resonance (NMR) sensitivity and accessible pressure range in high-pressure NMR experiments, owing to a series of new developments of NMR spectroscopy applied to the diamond anvil cell (DAC). Recently, with the application of electro-magnetic lenses, so-called Lenz lenses, in toroidal diamond indenter cells, pressures of up to 72 GPa with NMR spin sensitivities of about 10 spin/Hz has been achieved. Here, we describe the implementation of a refined NMR resonator structure using a pair of double stage Lenz lenses driven by a Helmholtz coil within a standard DAC, allowing to measure sample volumes as small as 100 pl prior to compression.
View Article and Find Full Text PDFNanoporous silicon produced by electrochemical etching of highly B-doped p-type silicon wafers can be prepared with tubular pores imbedded in a silicon matrix. Such materials have found many technological applications and provide a useful model system for studying phase transitions under confinement. This paper reports a joint experimental and simulation study of diffusion in such materials, covering displacements from molecular dimensions up to tens of micrometers with carefully selected probe molecules.
View Article and Find Full Text PDFNanoporous materials find widespread applications in our society: from drug delivery to environmentally friendly catalysis and separation technologies. The efficient design of these processes depends crucially on understanding the mass transfer mechanism. This is conventionally determined by uptake or release experiments, carried out with assemblages of nanoporous crystals, assuming all crystals to be identical.
View Article and Find Full Text PDFAngew Chem Int Ed Engl
November 2015
Diffusion in nanoporous host-guest systems is often considered to be too complicated to comply with such "simple" relationships as Fick's first and second law of diffusion. However, it is shown herein that the microscopic techniques of diffusion measurement, notably the pulsed field gradient (PFG) technique of NMR spectroscopy and microimaging by interference microscopy (IFM) and IR microscopy (IRM), provide direct experimental evidence of the applicability of Fick's laws to such systems. This remains true in many situations, even when the detailed mechanism is complex.
View Article and Find Full Text PDFUnder certain conditions, during binary mixture adsorption in nanoporous hosts, the concentration of one component may temporarily exceed its equilibrium value. This implies that, in contrast to Fick's Law, molecules must diffuse in the direction of increasing rather than decreasing concentration. Although this phenomenon of 'overshooting' has been observed previously, it is only recently, using microimaging techniques, that diffusive fluxes in the interior of nanoporous materials have become accessible to direct observation.
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