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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.
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).
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.
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.
Polymers with intrinsic microporosity (PIMs) are of great interest in the field of gas separation membranes. Already the first synthesized PIM-1 shows extraordinary permeability and selectivity. Unfortunately, PIM-1 is susceptible to physical aging and thus gradually loses its outstanding properties. In this study a polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) was used as a nanofiller (0–40 wt%) in the PIM-1 matrix to potentially improve the gas transport properties and prevent physical aging. The molecular mobility of the solution-cast nanocomposite films was analyzed by Broadband Dielectric Spectroscopy (BDS). Furthermore, gas permeability was determined with the time lag method (0–20 bar upstream pressure) at 35 °C for N2, O2, CH4 and CO2.