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Thomas Wittmann Dr. Renée Siegel Nele Reimer Dr. Wolfgang Milius Prof. Dr. Norbert Stock Prof. Dr. Jürgen Senker 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(1):314-323
The resistance of metal–organic frameworks towards water is a very critical issue concerning their practical use. Recently, it was shown for microporous MOFs that the water stability could be increased by introducing hydrophobic pendant groups. Here, we demonstrate a remarkable stabilisation of the mesoporous MOF Al‐MIL‐101‐NH2 by postsynthetic modification with phenyl isocyanate. In this process 86 % of the amino groups were converted into phenylurea units. As a consequence, the long‐term stability of Al‐MIL‐101‐URPh in liquid water could be extended beyond a week. In water saturated atmospheres Al‐MIL‐101‐URPh decomposed at least 12‐times slower than the unfunctionalised analogue. To study the underlying processes both materials were characterised by Ar, N2 and H2O sorption measurements, powder X‐ray diffraction, thermogravimetric and chemical analysis as well as solid‐state NMR and IR spectroscopy. Postsynthetic modification decreased the BET equivalent surface area from 3363 to 1555 m2 g?1 for Al‐MIL‐101‐URPh and reduced the mean diameters of the mesopores by 0.6 nm without degrading the structure significantly and reducing thermal stability. In spite of similar water uptake capacities, the relative humidity‐dependent uptake of Al‐MIL‐101‐URPh is slowed and occurs at higher relative humidity values. In combination with 1H‐27Al D ‐HMQC NMR spectroscopy experiments this favours a shielding mechanism of the Al clusters by the pendant phenyl groups and rules out pore blocking. 相似文献
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We discuss an error estimation procedure for the global error of collocation schemes applied to solve singular boundary value problems with a singularity of the first kind. This a posteriori estimate of the global error was proposed by Stetter in 1978 and is based on the idea of Defect Correction, originally due to Zadunaisky. Here, we present a new, carefully designed modification of this error estimate which not only results in less computational work but also appears to perform satisfactorily for singular problems. We give a full analytical justification for the asymptotical correctness of the error estimate when it is applied to a general nonlinear regular problem. For the singular case, we are presently only able to provide computational evidence for the full convergence order, the related analysis is still work in progress. This global estimate is the basis for a grid selection routine in which the grid is modified with the aim to equidistribute the global error. This procedure yields meshes suitable for an efficient numerical solution. Most importantly, we observe that the grid is refined in a way reflecting only the behavior of the solution and remains unaffected by the unsmooth direction field close to the singular point. 相似文献
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Norbert Auner Larissa Zherlitsyna Michael Bolte 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(5):m199-m200
The title compound, [Cu8(C8H24O2Si)2(C3H7NO)8]·C4H4N2·C3H7NO, features a sandwich‐like cage enclosing a pyrazine molecule, both situated on a centre of inversion. In addition, the crystal structure contains one dimethylformamide molecule which is disordered over a centre of inversion. The copper layer, containing eight atoms, is located between two siloxanolate fragments. The whole structure of Cu atoms and siloxanolate rings is distorted by the pyrazine molecule, leading to an oval form. As a result, the angles between the Cu atoms differ at the copper layer. The difference in the angles could lead to some deviations in the Cu–Cu exchange interactions within the copper ring, which is of interest for molecular magnetism. 相似文献
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In the present article, we aim at treating the existence of fundamental solutions of linear partial differential operators with constant coefficients from the viewpoint of setting up explicit formulae yielding fundamental solutions. 相似文献
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Peter Karduck Norbert Ammann Hans Günter Esser Jörg Winter 《Fresenius' Journal of Analytical Chemistry》1991,341(5-6):315-319
Summary The first wall of the fusion device TEXTOR at the Forschungszentrum Jülich has been coated in situ with an amorphous hydrogen rich carbon/boron film (a-C/B:H) which reduces plasma impurities caused by the plasma surface interaction. The results of the coating process of the 35 m2 large inner wall surface have been controlled by a recently developed modification of the quantitative electron probe microanalysis, which has been applied to 12 samples from specified positions inside the tokamak. The quantification itself is based on a Monte Carlo simulation of electron trajectories providing very accurate results for X-ray intensities emitted by elements present in the electron bombarded sample. The Monte Carlo results are used in the present work to calibrate the measured X-ray intensities emitted by boron and carbon from the a-C/B:H layers deposited on pure silicon substrates. As a result the total deposited mass of the layer per area unit as well as the composition of the layers (except hydrogen) could be determined very accurately. The relative errors were less than 7%. The limit of detectability were found to be in the range of one monolayer for boron as well as for carbon. 相似文献