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1.
Chemistry ; 14(11): 3311-5, 2008.
Article in English | MEDLINE | ID: mdl-18286555

ABSTRACT

Mesoporous pure silicas and functionalized silica with a narrow pore size distribution centered at 3.8 nm were prepared by a novel template, amphiphilic dendritic polyglycerol. The resulting silica materials were characterized by electron microscopy; nitrogen adsorption; (1)H, (13)C, and (29)Si solid-state cross-polarization magic-angle spinning NMR spectroscopy. It was shown that the template could be completely removed from the pure and functionalized silica in an environmentally friendly way by means of a simple water extraction procedure. Furthermore, it was shown that these materials could be easily functionalized, for example, by employing aminopropyl groups. Thus, a new environmentally friendly pathway to this fascinating class of silica material has been opened.


Subject(s)
Silicon Dioxide/chemical synthesis , Magnetic Resonance Spectroscopy , Microscopy, Electron, Transmission
2.
Phys Chem Chem Phys ; 9(35): 4843-53, 2007 Sep 21.
Article in English | MEDLINE | ID: mdl-17912415

ABSTRACT

In the last fifteen years several novel porous silica materials, which are periodically structured on the mesoscopic length scale, have been synthesized. They are of broad interest for fundamental studies of surface-substrate interactions, for studies of the dynamics of guest molecules in confinement and for studies of the effect of confinement on the structural and thermophysical properties of fluids. Examples of such confinement effects include the change of the freezing and melting points or glass transitions of the confined liquids. These effects are studied by combinations of several NMR techniques, such as (15)N- and (2)H-solid-state NMR line shape analysis, MAS NMR and NMR diffusometry with physico-chemical characterization techniques such as nitrogen adsorption and small angle diffraction of neutrons or X-rays. This combination does not require crystalline samples or special clean and well defined surfaces such as conventional surface science techniques, but can work with typical ill-defined real world systems. The review discusses, after a short introduction, the salient features of these materials and the applied NMR experiments to give the reader a basic knowledge of the systems and the experiments. The rest of the review then focuses on the structural and dynamical properties of guest molecules confined in the mesoporous silica. It is shown that the confinement into the pores leads to fascinating new features of the guests, which are often not known for their bulk phases. These features depend strongly on the interplay of the their interactions with the silica surface and their mutual interactions.

3.
J Colloid Interface Sci ; 303(2): 450-9, 2006 Nov 15.
Article in English | MEDLINE | ID: mdl-16996074

ABSTRACT

The dissolution of a technical, nanodispersed gamma-alumina in water was studied at 25 degrees C in the pH range 3.0 < or = pH < or = 11.0. The obtained kinetic dissolution curves showed a distinct pH dependency, whereas only for pH > or = 4.5 the typical behavior of nanodispersed materials could be observed. X-ray powder diffraction analysis and nitrogen adsorption, as well as IR and UV-Raman spectroscopy, were used to characterize the solid material collected during and at the end of each dissolution experiment. As a result the formation of a new aluminum phase-bayerite-could be proven. The analysis of the equilibrium concentration enabled us to determine the solubility constant of the corresponding phase assuming a pH-dependent species distribution. The rate constants of the dissolution process were evaluated using the model of Gibbs free energy of cluster formation, which considers the size effect, among other things. As a result, we could show that the observed maxima in the concentration profiles are due to a size effect of the starting material having a primary particle radius of 10.1 nm.

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