TY - CONF A1 - Konnertz, Nora A1 - Böhning, Martin T1 - QCM System for the Characterization of Gas Sorption and Physical Aging of Membrane Polymers for Gas Separation Applications N2 - Polymers are favorable materials for gas separation membranes. In general, gas transport experiments are performed with films in the range of 100 µm thickness. However, in large-scale processes very thin selective polymer layers in the range of 100 nm to 1 µm are used. Moreover, it was shown that thin films behave different compared to thick films with respect to gas transport properties and physical aging as well. Thus, for fundamental research it is important to realize gas transport experiments with thin films. The Quartz Crystal Microbalance (QCM) is a very sensitive method to detect mass changes in the range of nanograms. Therefore, this method enables sorption experiments with thin films or layers attached to the QCM crystal (100 nm up to 1 µm). Here, we present the experimental set-up for using the QCM technique for characterizing the gas sorption behavior of thin polymer films in a temperature controlled pressurized environment (up to 50 bar) - also quartz crystals and crystal holders were optimized. The study aims for the characterization of long-term behavior and physical aging of high-performance polymers for gas separation membranes - such as polyimides and polymers of intrinsic microporosity (PIMs) and respective nanocomposites. Especially the differences of the behavior of thin films compared to films with thicknesses up to 100 µm as well as nanofiller induced-effects are adressed. T2 - Polydays 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - Quartz Crystal Microbalance QCM KW - Thin Films; KW - Gas Sorption KW - High Pressure PY - 2016 AN - OPUS4-37911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konnertz, Nora A1 - Ding, Y. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Enhanced gas separation performance of nanocomposites based on a polymer with intrinsic microporosity PIM-1 and phenethyl-POSS N2 - In times of the energy revolution, the need for energy efficient separation processes promotes the advancement of new high performance materials for use as highly selective separation membranes. Most promising materials in this field, especially for gas separation, are polymers with intrinsic microporosity (PIMs) which were firstly introduced by Budd and McKeown. In this study the permeability of PIM-1 was increased by 439 % by formation of nanocomposites with only 1 wt% of polyhedral oligomeric phenethyl-silsesquioxane (PhE-POSS) within the polymer matrix. As the CO2/CH4 selectivity is fully retained, this leads to a shift in the Robeson plot towards the upper bound. The Robeson plot describes the current state of the art trade-off relation between selectivity and permeability of all known membrane polymers. As molecular mobility is a key factor for gas transport as well as the often observed physical aging of such polymers, our study also includes for the first time, molecular dynamics and conductivity of pure PIM-1 and PIM-1 nanocomposites as investigated by broadband dielectric spectroscopy (BDS). T2 - Polydays 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - PIM-1 KW - POSS KW - Broadband dielectric spectroscopy KW - Permeation PY - 2016 AN - OPUS4-37701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konnertz, Nora A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Dielectric investigations of the high performance polymer PIM-1 and nanocomposites containing phenethylPOSS N2 - Especially now, in times of the energy revolution, the need for energy efficient separation processes promote the advancement of new high performance materials for use as highly selective separation membranes. Most promising materials in this field, especially for gas separation, are polymers with intrinsic microporosity (PIMs) which were firstly introduced by Budd and McKeown. Currently widespread application of PIMs for membrane technology is still restrained by their strong tendency to physical aging involving a significant loss of their good gas separation properties. This phenomenom is directly related to the molecular mobility. Here for the first time, molecular dynamics and conductivity in PIM-1, the first synthesized PIM, were investigated by broadband dielectric spectroscopy (BDS). Although an α-relaxation was not observed for PIM-1, as a thermal glass transition temperature has not yet previously been reported below its decomposition temperature at 370°C, surprisingly a conductivity contribution was found which is attributed to intermolecular agglomerates formed by π−π-stacking. Besides the studies on pure PIM-1 a polyhedral oligomeric phenethyl-silsesquioxanes (PhenethylPOSS) was used as nanofiller (0 – 40 wt%) in order to evaluate its ability to improve gas transport properties and probably control physical aging. The molecular mobility of all materials was analyzed by BDS of solution-cast films. T2 - 9th International Conference on Broadband Dielectric Spectroscopy and its Applications CY - Pisa, Italy DA - 11.09.2016 KW - Broadband dielectric spectroscopy KW - PIM-1 KW - POSS PY - 2016 AN - OPUS4-37705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, D. A1 - Konnertz, Nora A1 - Böhning, Martin A1 - Schmidt, J. A1 - Thomas, A. T1 - Light-switchable polymers of intrinsic microporosity JF - Chemistry of Materials N2 - The interest in (micro)porous systems is greater than ever before with microporous polymers finding application in areas such as gas storage/separation and catalysis. In contrast to the vast majority of publications on microporous polymers seeking ever higher values for surface area or uptake capacity for a particular gas, this work presents a means to render a microporous system responsive to electromagnetic stimuli. The incorporation of a diarylethene (DAE) derivative in the backbone of a polymer of intrinsic microporosity (PIM) produces a microporous system that exhibits photochromism as proven by UV–vis absorption and NMR studies. In the resulting DAE-PIM, surface area is not a fixed unalterable property but can be influenced by the external and nondestructive stimulus light in a reversible manner. Furthermore, in combination with Matrimid, free-standing membranes can be produced that display light-switchable diffusivity and permeability for carbon dioxide and oxygen. In this way, material scientists are offered the potential to employ only one system that can assume several states with different properties for each. KW - Gaspermeation KW - Diffusion KW - Polymer intrinsischer Mikroporosität KW - UV-VIS PY - 2016 DO - https://doi.org/10.1021/acs.chemmater.6b02619 SN - 0897-4756 VL - 28 IS - 23 SP - 8523 EP - 8529 PB - ACS CY - Whashington,DC AN - OPUS4-38735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -