New Generation of Mesoporous Silica Membranes Prepared by a Stöber-Solution Pore-Growth Approach.

Membranes consisting of uniform and vertically organized mesopores are promising systems for molecular filtration because of the possibility to combine high-flux and high-rejection properties. In this work, a new generation of mesoporous silica membranes (MSMs) have been developed, in which an organized mesoporous layer is directly formed on top of a porous ceramic support via a Stöber-solution pore-growth approach. Relevant characterization methods have been used to demonstrate the growth of the membrane separation layer and the effect of reaction time and the concentration of the reactants on the microstructure of the membrane. Compared to previous studies using the evaporation-induced self-assembly method to prepare MSMs, an important increase in water permeability was observed (from 1.0 to at least 3.8 L m-2 h-1 bar-1), indicating an improved pore alignment. The water permeability, cyclohexane permporometry tests, and molecular cut-off measurements (MWCO ≈ 2300 Da) were consistent with membranes composed of 2-3 nm accessible pores.

Development of nanoscale inhomogeneities during drying of sol-gel derived amorphous lead zirconate titanate precursor thin films.

The structural evolution of sol-gel derived lead zirconate titanate (PZT) precursor films during and after physical drying was investigated by transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), selected area electron diffraction (SAED), and time-resolved X-ray diffraction (XRD). Films were deposited from initial 0.3 mol/dm(3) precursor sols with varying hydrolysis ratios. Zr-rich grains of 1-10 nm size, embedded in a Pb-, Zr-, and Ti-containing amorphous matrix were found in as-dried films. The Zr-rich regions were crystalline at hydrolysis ratios [H(2)O]/[PZT] < 27.6, and amorphous at ratios > 100. X-ray diffraction analysis of PZT and zirconia sols revealed that the crystalline nanoparticles in both sols are identical and are probably composed of nanosized zirconium oxoacetate-like clusters. This study demonstrates that time-resolved X-ray diffraction combined with electron energy loss spectroscopy mapping is a powerful tool to monitor the nanoscale structural evolution of sol-gel derived thin films.