TY - CONF A1 - Schröder, Hartmut A1 - Munz, Martin A1 - Böhning, Martin A1 - Lorenz, Edelgard A1 - Kneip, Gisela T1 - New method for testing the resistance to oxidation - Application and Evaluation: Polyolefinic Products T2 - EUROCORR 2006 CY - Maastricht, The Netherlands DA - 2006-09-25 PY - 2006 N1 - Serientitel: EFC-Event – Series title: EFC-Event IS - 280 SP - 1 EP - 8 PB - European Federation of Corrosion CY - Maastricht AN - OPUS4-13706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schröder, Hartmut A1 - Munz, Martin A1 - Böhning, Martin T1 - A new method for testing and evaluating the long-tIme resistance to oxidation of polyolefinic products T2 - 13th International Plastics Additives and Compounding Conference "Addcon World 2007" CY - Frankfurt/M. DA - 2007-09-05 PY - 2007 SN - 978-1-84735-018-3 IS - Paper 7 SP - 1 EP - 10 CY - Shawbury AN - OPUS4-15762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Hartmut A1 - Munz, Martin A1 - Böhning, Martin T1 - A new method for testing and evaluating the long-time resistance to oxidation of polyolefinic products N2 - A report is presented on the development of a test for determining the long-term oxidation resistance of polyolefin materials, which is accelerated not only by elevated temperatures but also by increased oxygen pressure and a stirred aqueous medium. The method permits durability tests to be carried out at markedly lower temperatures with reasonable testing durations and significantly reduced diffusion limited oxidation effects and allows for physical and chemical impacts of aqueous media. Oxidative durability can be assessed by autoclave immersion exposures at three different temperatures (60, 70 and 80 degrees C) and 50 bar oxygen pressure and at 80 degrees C and two different oxygen pressures (usually 10 and 20 bar). Accelerated test data are evaluated by modified Arrhenius equations with the application of a three-dimensional regression analysis. The application of the test method to various materials, including PP non-woven materials and geosynthetics is demonstrated. 10 refs. KW - Polyolefin KW - Testing KW - Oxidation KW - Durability KW - Geosynthetics PY - 2008 SN - 0967-3911 SN - 1478-2391 VL - 16 IS - 1 SP - 71 EP - 79 PB - RAPRA Technology Ltd. CY - Shrewsbury AN - OPUS4-17187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Niebergall, Ute A1 - Adam, Adeline A1 - Stark, Wolfgang T1 - Impact of biodiesel sorption on mechanical properties of polyethylene N2 - The time-dependent sorption of biodiesel in a typical polyethylene for container applications is investigated in comparison to conventional diesel fuel at three different temperatures. In this context, the desorption behavior is also addressed. Subsequently, the effects of both penetrants on mechanical properties are characterized in terms of impact strength and dynamic-mechanical analysis. The discussion of property changes is firstly based on the sorption kinetics of biodiesel and diesel, which is determined by immersion experiments allowing for the calculation of respective diffusion coefficients. Changes in impact strength as determined by the Charpy method are further characterised in more detail by analyzing the fracture surfaces, and correlated with results of dynamic-mechanical analysis. KW - Biodiesel KW - Fuel sorption KW - Desorption KW - Impact strength KW - Dynamic-mechanical analysis KW - PE-HD PY - 2014 DO - https://doi.org/10.1016/j.polymertesting.2013.12.003 SN - 0142-9418 VL - 34 SP - 17 EP - 24 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-30096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Böhning, Martin A1 - Krafft, Bernd A1 - Schartel, Bernhard T1 - Multilayer graphene chlorine isobutyl isoprene rubber nanocomposites: influence of the multilayer graphene concentration on physical and flame-retardant properties N2 - In recent years, different nanoparticles have been proposed and successfully introduced as nanofillers in rubber nanocomposites. In this study, multilayer graphene (MLG) is proposed as a nanoparticle that functions efficiently at low concentrations. MLG consists of just 10 or so graphene sheets. Chlorine isobutyl isoprene rubber (CIIR)/MLG nanocomposites with different MLG loadings were prepared using an ultrasonically assisted solution mixing procedure followed by two-roll milling. The incorporation of MLG provides a clear improvement in the rheological, mechanical, curing, and gas barrier properties of the nanocomposites. Adding only 3 phr ofMLGto CIIR increased the Young’s modulus by more than two times and reduced the permeability ofO2 andCO2 by 30%. Higher nanofiller concentrations yielded further improvement in the properties of the nanocomposites. Moreover, CIIR/MLG nanocomposites showed reduced flammability. KW - Graphene KW - Rubber KW - Nanocomposites KW - Flammability KW - Reinforcement PY - 2016 DO - https://doi.org/10.5254/rct.15.84838 SN - 0035-9475 VL - 89 IS - 2 SP - 316 EP - 334 AN - OPUS4-37595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yin, Huajie A1 - Chapala, P. A1 - Bermeshev, M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular Mobility and Physical Aging of a Highly Permeable Glassy Polynorbornene as Revealed by Dielectric Spectroscopy N2 - Polymeric membranes represent a cost- and energy efficient solution for gas separation. Recently superglassy polymers with high free volume outperform many conventional dense polymers in terms of gas permeability and selectivity. However, such polymers are prone to pronounced physical aging, resulting in a dramatic reduction in the gas permeability. Molecular mobility of polymer segments plays an important role in the physical aging and the gas transport performance of polymeric membranes. Molecular mobility and physical aging of a representative superglassy polynorbornene with very high gas permeability, PTCNSi2g, was monitored by using dielectric spectroscopy with state-of-the-art high-resolution analyzers. This work helps to shed some light on the structure−property relationship of superglassy polymers on a molecular level and to provide practical “design rules” for the development of high performance polymers for gas separation. KW - Molecular mobility KW - Gas separation membrane KW - Broadband dielectric spectroscopy KW - Polymer KW - Physical ageing PY - 2017 DO - https://doi.org/10.1021/acsmacrolett.7b00456 SN - 2161-1653 VL - 6 IS - 8 SP - 813 EP - 818 PB - ACS CY - Washington DC, USA AN - OPUS4-41354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Characterization of gas sorption in glassy polymers combining experimental and molecular modeling techniques T2 - American Chemical Society (ACS) Spring Meeting CY - New Orleans, LA, USA DA - 2008-04-06 PY - 2008 AN - OPUS4-17402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Wohlrab, Sebastian A1 - Schönhals, Andreas T1 - Polymer Based Nanocomposites with PhenethylPOSS as Nanofilter Investigated by Dielectric Spectroscopy and Gas Transport Measurements N2 - Polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) as nanofiller was incorporated within Poly(bisphenol A carbonate) (PBAC) as matrix. Dielectric spectroscopy proved an almost complete miscibility of PhenethylPOSS up to 7 wt. %. At higher concentrations phase separation yields composites with a PBAC-rich matrix and POSS-rich domains which posses well shaped interfaces. The nanocomposites were also investigated with respect to their gas transport behaviour. An increase of the gas permeability was found at higher PhenethylPOSS concentrations, which is due to the phase separated structure. KW - Dielectric measurements KW - Nanocomposites KW - Permeation KW - Polycarbonates KW - Polyhedral oligomeric silsesquioxanes PY - 2008 DO - https://doi.org/10.1002/masy.200850712 SN - 1022-1360 SN - 0258-0322 SN - 1521-3900 VL - 267 IS - 1 SP - 69 EP - 73 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-17751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Atomistic simulation of gas sorption isotherms in a polymer of intrinsic microporosity (PIM-1) T2 - EUROMEMBRANE 2009 Conference CY - Montpellier, France DA - 2009-09-06 PY - 2009 AN - OPUS4-20103 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Retzlaff, J. A1 - Bronstein, Z. A1 - Müller-Rochholz, J. A1 - Böhning, Martin A1 - Robertson, Daniela A1 - Schröder, Hartmut T1 - Oxidative resistance of geosynthetics: practical aspects and developments of testing at elevated temperature and oxygen pressure N2 - Service life of geosynthetics made of polyolefin materials is mainly limited by oxidative degradation. Durability of polyolefin products depend on formulation, morphology resulting from manufacturing, design and particularly on the antioxidants used. Although the fundamental oxidative reactions are known, the complex effect of geosynthetic characteristics and external influences mean that durability assessments require practical tests. The assessment of oxidative durability involves exposure to accelerating conditions as well as the material characterisation with respect to the state of stabilisation and/or degradation (e.g. by tensile testing and/or oxidation induction time). The autoclave test developed by BAM for durability assessments of polyolefin geosynthetics is based on the simultaneous application of moderately elevated temperatures (up to 80 degrees Celsius) and elevated oxygen pressures (up to 5.0 MPa) in combination with a surrounding aqueous medium. Thus this test method provides several advantages in comparison to conventional oven testing, especially with respect to test duration, impact of surrounding environment and the potential to differentiate and rank oxidative resistance between products of very different dimensions (surface/volume) and stabilisation. In view of the increasing demand for durability assessments of geosynthetic products with lifetimes significantly exceeding 25 years, the contribution is focused on practical aspects concerning implementation and optimisation of test procedures, conditions and evaluation of results. Furthermore, advanced approaches based on multiple exposure conditions will also be included and corresponding calculations of expected service life in typical applications will be evaluated with respect to significance and repeatability. Thereby involved standards and recommendations - such as EN ISO 13438, Part C or EAG-EDT - are considered. T2 - EuroGeo4, 4th European Geosynthetics Conference CY - Edinburgh, UK DA - 2008-09-07 KW - Ageing KW - Degradation KW - HDPE KW - Laboratory test KW - Oxidation KW - Polypropylene PY - 2008 IS - Paper 178 SP - 1 EP - 4 AN - OPUS4-18423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Retzlaff, J. A1 - Müller-Rochholz, J. A1 - Klapperich, H. A1 - Böhning, Martin T1 - The behaviour of geosynthetics under cyclic load N2 - Whenever geosynthetics are used to reinforce or stabilise infrastructural elements such as road- and railways, bridge abutments, run- and taxiways on airports or to protect coastlines of canals and other steep slopes they may be exposed to cyclic loads. Therefore, a reduction factor for dynamic effects on the geosynthetic tensile strength has been included into the calculation of the Long Term Design Strength (LTDS). An approach to assess the behaviour of geosynthetics is to adopt Woehler- or Smith graphs and Haigh-diagrams for polymers. This is because an endurance limit for polymers, which defines an infinite life under a defined cyclic load, has not been seen so far. A huge amount of mechanical testing is needed to predict the behaviour of geosynthetics against this particular background. To reduce these efforts while getting an indication of the cyclic effect on geosynthetics, a combined method of mechanical and chemical analysis has been developed. The pure tensile strength tests to determine the residual strength after cyclic stress has been amended by IR-spectroscopy and Differential Scanning Calorimetry (DSC). In this context the chain change model of PET has been proven as valid for cyclic loads as well, which helps to define the endurance limit of materials made out of PET. For polyolefins such as PP and PE, a limit for the maximum alternating load has been identified at the point of the stress strain graph where the actual and the numerical stress of a material diverge from each other. Cyclic tensile strength tests have been carried out in a hydraulic test frame. The test parameters have been set to simulate the service life of a railway bed trafficked by high speed trains (ICE). T2 - EuroGeo4, 4th European Geosynthetics Conference CY - Edinburgh, UK DA - 2008-09-07 KW - Cyclic load KW - Dynamic loads KW - Laboratory test KW - Reduction factor KW - Reinforcement KW - Stiffness PY - 2008 IS - Paper 179 SP - 1 EP - 7 AN - OPUS4-18425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Charakterization of gas sorption in glassy polymers using experimental and molecular modeling techniques T2 - 14th International Conference "Polymeric Materials" CY - Halle (Saale), Germany DA - 2010-09-15 PY - 2010 AN - OPUS4-22104 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hölck, Ole A1 - Böhning, Martin A1 - Heuchel, M. A1 - Siegert, M.R. T1 - Gas-induced structural changes in polymeric membrane materials combining experiment, phenomenological models and simulation KW - Polymer KW - Gas transport KW - Dilation KW - Plasticization KW - Free volume molecular modelling PY - 2006 DO - https://doi.org/10.1016/j.desal.2006.03.283 SN - 0011-9164 VL - 200 IS - 1-3 SP - 166 EP - 168 PB - Elsevier CY - Amsterdam AN - OPUS4-13730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hölck, Ole A1 - Siegert, M.R. A1 - Heuchel, M. A1 - Böhning, Martin T1 - CO2 Sorption Induced Dilation in Polysulfone: Comparative Analysis of Experimental and Molecular Modeling Results N2 - Experimental sorption and dilation data of the polysulfone/CO2 system at 308 K and pressures up to 50 bar were measured utilizing a gravimetric sorption balance and a dilatometer based on a capacitive distance sensor. The data of this glassy polymer/gas system were subjected to a thorough kinetic analysis on the basis of a viscoelastic model, which allows the separation of the diffusive/elastic fraction of the sorption/dilation process from the slower relaxational part. The results were interpreted in terms of the common dual mode sorption model and the site distribution model of Kirchheim. Detailed atomistic packing models of the same polymer/gas system were created for two reference states with regard to concentration and swelling. The CO2 sorption isotherms of the packing models corresponding to these two swelling states, calculated using GCMC simulations, could be combined in order to interpolate the gas uptake over the intermediate pressure range with good agreement to the experimental data. The elastic part of the gas induced dilation is successfully described by MD simulations and derived partial molar volumes are in satisfying agreement with experimental findings. Finally, the free volume of the packing models is probed and the obtained size distribution of the free volume elements is compared to the results of the analysis of experimental data according to the site distribution model. KW - Sorption KW - Dilation KW - Dual mode sorption model KW - Site distribution model KW - Molecular modelling KW - Polysulfone PY - 2006 SN - 0024-9297 SN - 1520-5835 VL - 39 IS - 26 SP - 9590 EP - 9604 PB - American Chemical Society CY - Washington, DC AN - OPUS4-14405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Goering, Harald A1 - Schönhals, Andreas T1 - Nanocomposites of Polyhedral Oligomeric Phenethylsilsesquioxanes and Poly(bisphenol A carbonate) as Investigated by Dielectric Spectroscopy N2 - Nanocomposites were prepared by solution blending of polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) into poly(bisphenol A carbonate) (PBAC). The nanocomposites were investigated by dielectric spectroscopy, differential scanning calorimetry (DSC) and density measurements. PhenethylPOSS shows one relaxation process, the α-relaxation, confirmed by DSC investigations. PBAC shows a β-relaxation at lower and an α-relaxation at higher temperatures. With increasing PhenethylPOSS content the α-relaxation of the composites shifts to lower temperatures. Thus, incorporation of PhenethylPOSS leads to a plasticization of PBAC due to a decrease of the packing density which is rationalized by density measurements. For higher concentrations of PhenethylPOSS (>10 wt %) the α-relaxation of the polycarbonate matrix splits into two peaks. Moreover, close to the α-relaxation of PhenethylPOSS a third process is observed. These results indicate a phase separation into a PBAC matrix with a few percents of molecularly solved POSS and POSS-rich domains. These POSS-rich domains are surrounded by an interfacial layer of PBAC having a higher concentration of POSS than the matrix. A phase diagram is deduced providing a miscibility criterion. For the phase separated nanocomposites an interfacial polarization phenomena is observed. Using a simplified model the time constant of this process is correlated with the size of the PhenethylPOSS-rich domains and theire increasing size with the increase of the concentration of POSS. KW - Polyhedral oligomeric silsesquioxane (POSS) KW - Polymer-based nanocomposites KW - Broadband dielectric spectroscopy KW - Interfacial polarisation PY - 2007 SN - 0024-9297 SN - 1520-5835 VL - 40 IS - 8 SP - 2955 EP - 2964 PB - American Chemical Society CY - Washington, DC AN - OPUS4-14768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Gas Transport Properties of Polymeric Nanocomposites Based on Polyhedral Oligomeric Silsesquioxanes PY - 2007 SN - 0743-0515 VL - 97 SP - 444 EP - 445 PB - Division of Polymeric Materials Science and Engineering, American Chemical Society CY - Washington, DC AN - OPUS4-15846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hölck, Ole A1 - Heuchel, M. A1 - Böhning, Martin A1 - Hofmann, D. T1 - Simulation of Experimentally Observed Dilation Phenomena During Integral Gas Sorption in Glassy Polymers N2 - A molecular modeling investigation of dilation effects induced by sorbed gas molecules in two glassy polymers is presented. As experimental reference, integral sorption of CO2 and CH4 was measured for polysulfone (PSU) and a polyimide (6FDA-TrMPD, PI4) at 308 K and a pressure of 10 bar. Simultaneously, the gas induced swelling effect was measured with a dilatometer based on a capacitive distance sensor recorded. The experimental evidence of the (on the observed time scale and concentration levels) elastic nature of the gas induced dilation is supported by the dilation and contraction behavior observed in molecular dynamics (MD) simulations of respective detailed atomistic packing models. These models were constructed in accordance with gas concentration levels obtained from the experimental sorption results. Quantitative deviations between simulated and measured dilations are discussed as a consequence of an anelastic response of the polymer matrix which is too fast to be resolved in the experiments whose kinetics is dominated by diffusional processes. In the simulation, the initial insertion of penetrant molecules into equilibrated packing models circumvents the slow diffusional process of the experiment and allows a reasonable representation of the dilation process as well as a closer investigation. Our simulation approach reveals a different behavior for PSU and PI4 on the corresponding time scale. Most likely, the different chain mobility of the two polymers is responsible for the respective response to the inserted amount of gas molecules which is discussed in terms of the different chain mobilities of the two polymers. KW - Diffusion KW - Dilation KW - Gas sorption KW - Molecular modeling KW - Poly(ether sulfones) KW - Polyimides KW - Swelling PY - 2008 DO - https://doi.org/10.1002/polb.21342 SN - 0887-6266 SN - 1099-0488 VL - 46 IS - 1 SP - 59 EP - 71 PB - Wiley CY - Hoboken, NJ AN - OPUS4-16206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hölck, Ole A1 - Böhning, Martin A1 - Heuchel, M. A1 - Siegert, M.R. A1 - Hofmann, D. T1 - Gas sorption isotherms in swelling glassy polymers - detailed atomistic simulations N2 - Detailed atomistic simulations were carried out for swelling polymer/gas systems related to experimental sorption and dilation data for CO2 and CH4 in three glassy polymers (polysulfone PSU, the polyimide 6FDA-TrMPD, and a polymer of intrinsic microporosity PIM-1) at 308 K (35 °C) and pressures up to 50 bar. Corresponding experiments were performed with a gravimetric sorption balance and a dilatometer based on a capacitance distance sensor. For each polymer/gas system molecular packing models were prepared and equilibrated for two reference states: the pure polymer is taken as reference for the respective 'unswollen' state and similarly the state of the highest penetrant pressure reached in the corresponding experiment is taken to represent the 'swollen' state. Models for the latter were constructed in agreement with experimental data (pressure, temperature, gas concentration and volume dilation). Concentration–pressure isotherms of each polymer/gas system were obtained using Grand Canonical Monte Carlo (GCMC) simulations for both reference states (depleted of gas molecules), which are in good agreement with the experimental data in the respective pressure range. As expected these isotherms – due to the simulation technique used, merely based on hole-filling in a static host matrix – do not represent the sorption behavior over a broader range of gas pressures which may involve significant structural rearrangements as well as swelling and relaxational phenomena. Nevertheless, a linear combination of the two GCMC-isotherms allows the interpolation in order to describe the nonlinear gas sorption in the glassy polymers under investigation covering the penetrant pressure range between the reference states in good agreement with the experimental results. KW - Gas sorption KW - Dilation KW - Molecular modeling KW - Polysulfone KW - Polyimide KW - Polymer of intrinsic microporosity (PIM-1) PY - 2013 DO - https://doi.org/10.1016/j.memsci.2012.10.023 SN - 0376-7388 SN - 1873-3123 VL - 428 SP - 523 EP - 532 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-27599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Battig, Alexander A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Huth, Christian A1 - Böhning, Martin A1 - Schartel, Bernhard T1 - Multifunctional Property Improvements by Combining Graphene and Conventional Fillers in Chlorosulfonated Polyethylene Rubber Composites N2 - The incorporation of nanoparticles like multilayer graphene (MLG) into elastomeric composites boosts their technical performance, such as their mechanical behavior and electrical conductivity. Common filler types (carbon black (CB) and aluminum trihydroxide (ATH)) generally fulfill single, specific purposes and are often used in high loadings. CB typically reinforces rubber mechanically, while ATH increases flame retardancy. Small amounts of MLG reduce these high filler contents and maintain the multifunctional characteristics of rubber composites. In chlorosulfonated polyethylene (CSM) + ATH, an intrinsically flame-retardant rubber was designed to achieve the highest standards such as maximum average of heat emission (MARHE) <90 kW m−2, 3 phrMLG was substituted for 15 phr CB and/or 3 phr ATH via an industrially applicable processing approach. Replacing either CB or ATH resulted in a property profile that was multifunctionally improved in terms of features such as mechanical performance, reduced sorption, and flame retardance. MLG nanocomposites are reported to show promise as an industrially utilizable route to obtain multifunctional high-performance rubbers. KW - Nanocomposites KW - Rubber KW - Multilayer graphene KW - Flame retardancy KW - Synergy KW - Nanoparticles KW - Elastomers PY - 2022 DO - https://doi.org/10.1021/acsapm.1c01469 SN - 2637-6105 VL - 4 IS - 2 SP - 1021 EP - 1034 PB - ACS Publ. CY - Washington, DC AN - OPUS4-54330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schilling, Markus A1 - Marschall, Niklas A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Dataset of comprehensive Full-notch creep tests (FNCT) of selected high-density polyethylene (PE-HD) materials N2 - The dataset provided in this repository comprises data obtained from a series of full-notch creep tests (FNCT) performed on selected high-density polyethylene (PE-HD) materials (for further details, see section 1 Materials in this document) in accordance with the corresponding standard ISO 16770. The FNCT is one of the mechanical testing procedures used to characterize polymer materials with respect to their environmental stress cracking (ESC) behavior. It is widely applied for PE-HD materials, that are predominantly used for pipe and container applications. It is based on the determination of the time to failure for a test specimen under constant mechanical load in a well-defined and temperature controlled liquid environment. The test device used here also allows for continuous monitoring of applied force, specimen elongation and temperature. KW - Polyethylene KW - Environmental Stress Cracking KW - Full-notch creep test KW - PE-HD KW - Crack growth PY - 2023 DO - https://doi.org/10.5281/zenodo.10143351 PB - Zenodo CY - Geneva AN - OPUS4-58835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Böhning, Martin A1 - Frick, B. A1 - Apple, M. A1 - Mole, R. A. A1 - De Souza, N. R. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Confined Segmental Diffusion in Nanophase Separated Janus Polynorbornenes as Investigated by Quasielastic Neutron Scattering N2 - A combination of neutron time-of-flight and neutron backscattering spectroscopy was used to investigate the molecular dynamics of Janus polynorbornenes (Janus poly(tricyclononenes)) on a microscopic level. These Janus polynorbornenes, denoted as PTCNSiOR, have a semirigid backbone with −Si(OR)3 side groups attached to it. R represents the length of the alkyl side chain. Here side chain lengths of R = 3 (propyl) and R = 8 (octyl) were considered. It is worth mentioning that these polymers have some potential as active layers in gas separation membranes, especially for the separation of higher hydrocarbons. The combination of time-of-flight and backscattering will ensure a reasonably broad time window for analysis where the incoherent intermediate scattering function SInc(q,t) is considered. Previously, it was shown by X-ray investigations that the system undergoes a nanophase separation into alkyl side chain-rich domains surrounded by a backbone-rich matrix. For PTCNSiOPr (R = 3), the alkyl side-chain-rich domains are truly isolated in the backbone-rich matrix, whereas for PTCNSiOOc (R = 8) these domains percolate through the matrix. Further, it was also previously shown that the alkyl side-chain-rich domains undergo a glass transition. The advantage of neutron scattering experiments discussed here is that besides temporal also spatial information is obtained which will allow conclusions to be drawn about the type of molecular fluctuations. At the lowest measured temperature, the decay in Sinc(q,t) is due to the methyl group rotation. The methyl group dynamics is analyzed in terms of a modified jump-diffusion in a 3-fold potential and yields to a reasonable fraction of hydrogens which contribute to the methyl group rotation. At higher temperatures, the decay in SInc(q,t) is due to both the methyl group rotation and the segmental dynamics in the alkyl side-chain-rich domains. The segmental diffusion is modeled by a sublinear diffusion. For the analysis of the scattering function SInc(q,t) of PTCNSiOPr an elastic scattering due to the immobilized backbone-rich matrix must be taken into account. The analysis reveals that the segmental dynamics is confined by the finite size of alkyl chain-rich domains and that it is intrinsically heterogeneous in nature. Both effects are more pronounced for PTCNSiOPr in comparison to those of PTCNSiOOc. KW - Polynorbornene KW - Quasielastic Neutron Scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608712 DO - https://doi.org/10.1021/acs.macromol.4c01045 SP - 1 EP - 14 PB - ACS Publications AN - OPUS4-60871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Marschall, Niklas A1 - Niebergall, Ute A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Characteristics of environmental stress cracking of PE-HD induced by biodiesel and diesel fuels N2 - In the context of the increasing effect of carbon dioxide emissions on the global climate biodiesel produced from renewable sources has emerged as a promising contender replacing fossil fuels, especially in long-range transport vehicles, using existing engines and infrastructure. High-density polyethylene is one of the prevailing materials for pipe and container applications for storage and transport of such fuels, both, from fossil and renewable resources. The contact with the respective fuels raises questions concerning material compatibility as biodiesel exhibits significant differences compared to conventional diesel fuel affecting its sorption and plasticization behavior in polyethylene. In this study, its behavior with respect to environmental stress cracking, considered one of the most frequent damage mechanisms leading to failure of polymer parts and packaging, was evaluated using the well-established Full Notch Creep Test. This approach allows for a detailed fracture surface analysis using imaging techniques, such as optical and laser scanning microscopy, as well as infrared spectroscopy. Comparing the environmental stress cracking behavior in standard surfactant solutions with that in biodiesel and diesel, respective crack propagation rates, showing different levels of acceleration, were determined and details of the underlying mechanisms could be revealed. Furthermore, the specific infrared absorption of the biodiesel’s ester functionality allows its semi-quantitative determination on the fracture surface of the tested specimens after failure. Thus, a preferred uptake of sorptive fluids in the fracture zone due to local morphological changes of the polyethylene could be directly evidenced by infrared spectroscopy. KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Confocal laser scanning microscopy (LSM) KW - Biodiesel KW - Diesel PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608591 DO - https://doi.org/10.1016/j.polymertesting.2024.108547 SN - 0142-9418 VL - 138 SP - 1 EP - 16 PB - Elsevier Ltd. AN - OPUS4-60859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Böhning, Martin A1 - De Souza, N. R. A1 - Juranyi, F. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Inelastic and Quasielastic Neutron Scattering on Polynorbornenes with Bulky Carbocyclic Side groups N2 - This study investigates the molecular mobility and vibrational properties of polynorbornenes with bulky carbocyclic side groups using inelastic and quasielastic neutron scattering techniques. The polymers, synthesized via metathesis and addition polymerization, exhibit varying degrees of microporosity, which ignificantly influences their gas separation performance. By inelastic neutron scattering experiments, it could be shown that all considered polymers have excess contributions to the low frequency vibrational density of states known as the Boson peak. The maximum frequency of the Boson peak correlates to the microporosity of the polymers. This correlation supports the sound wave interpretation of the Boson peak, suggesting that the microporous structure enhances the compressibility of the material at a microscopic length scale. The molecular mobility, particularly the methyl group rotation, was characterized using elastic scans and quasielastic neutron scattering. The study revealed a temperature dependent relaxation process, with the onset of molecular fluctuations observed around 200 K for the polymer containing methyl groups. For the polymer having no methyl groups only elastic scattering is observed. The methyl group rotation was analyzed in terms of a jump diffusion in a threefold potential with three equivalent energy minima. This leads to an almost correct description of the q dependence of the elastic incoherent scattering function when the number of hydrogen nuclei undergoing the methyl group rotation is considered. It was further evidenced that the fraction of methyl undergoing the methyl group rotation increases with increasing temperature. KW - Polymers of Intrinsic Microporosity KW - Neutron scattering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630297 DO - https://doi.org/10.1016/j.polymer.2025.128358 SN - 1873-2291 VL - 328 SP - 241 PB - Elsevier Ltd. AN - OPUS4-63029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Jalarvo, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Microscopic molecular mobility of high-performance polymers of intrinsic microporosity revealed by neutron scattering – bend fluctuations and signature of methyl group rotation N2 - Polymers of intrinsic microporosity exhibit a combination of high gas permeability and reasonable permselectivity, which makes them attractive candidates for gas separation membrane materials. The diffusional selective gas transport properties are connected to the molecular mobility of these polymers in the condensed state. Incoherent quasielastic neutron scattering was carried out on two polymers of intrinsic microporosity, PIM-EA-TB(CH3) and its demethylated counterpart PIM-EA-TB(H2), which have high Brunauer–Emmett–Teller surface area values of 1030 m2 g-1 and 836 m2 g-1, respectively. As these two polymers only differ in the presence of two methyl groups at the ethanoanthracene unit, the effect of methyl group rotation can be investigated solely. To cover a broad dynamic range, neutron time-of-flight was combined with neutron backscattering. The demethylated PIM-EA-TB(H2) exhibits a relaxation process with a weak intensity at short times. As the backbone is rigid and stiff this process was assigned to bendand-flex fluctuations. This process was also observed for the PIM-EA-TB(CH3). A further relaxation process is found for PIM-EA-TB(CH3), which is the methyl group rotation. It was analyzed by a jump-diffusion in a three-fold potential considering also the fact that only a fraction of the present hydrogens in PIM-EATB(CH3) participate in the methyl group rotation. This analysis can quantitatively describe the q dependence of the elastic incoherent structure factor. Furthermore, a relaxation time for the methyl group rotation can be extracted. A high activation energy of 35 kJ mol-1 was deduced. This high activation energy evidences a strong hindrance of the methyl group rotation in the bridged PIM-EA-TB(CH3) structure. KW - Polymers of Intrinsic Microporosity KW - Neutron Scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604114 DO - https://doi.org/10.1039/d4sm00520a SP - 1 EP - 11 PB - RSC AN - OPUS4-60411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Pedragosa-Rincon, M. A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Environmental Stress Cracking of High-Density Polyethylene Applying Linear Elastic Fracture Mechanics N2 - The crack propagation rate of environmental stress cracking was studied on high-density polyethylene compact tension specimens under static loading. Selected environmental liquids are distilled water, 2 wt% aqueous Arkopal N100 solution, and two model liquid mixtures, one based on solvents and one on detergents, representing stress cracking test liquids for commercial crop protection products. The different surface tensions and solubilities, which affect the energetic facilitation of void nucleation and craze development, are studied. Crack growth in surface-active media is strongly accelerated as the solvents induce plasticization, followed by strong blunting significantly retarding both crack initiation and crack propagation. The crack propagation rate for static load as a function of the stress intensity factor within all environments is found to follow the Paris–Erdogan law. Scanning electron micrographs of the fracture surface highlight more pronounced structures with both extensive degrees of plasticization and reduced crack propagation rate, addressing the distinct creep behavior of fibrils. Additionally, the limitations of linear elastic fracture mechanisms for visco-elastic polymers exposed to environmental liquids are discussed. KW - Crack propagation KW - Environmental stress cracking KW - Fracture toughness KW - Crop protection products KW - High-density polyethylene KW - Craze–crack mechanism KW - Linear elastic fracture mechanics KW - Stress intensity factor PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550476 DO - https://doi.org/10.3390/polym14122415 SN - 2073-4360 VL - 14 IS - 12 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-55047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrations and diffusion in disordered polymers bearing an intrinsic microporosity as revealed by neutron scattering N2 - The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules. KW - Polymer of intrisic microporosity KW - Neutron scattering KW - Boson peak KW - Methyl group rotation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538490 DO - https://doi.org/10.3390/cryst11121482 VL - 11 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Zorn, R. A1 - Böhning, Martin A1 - Wolff, M. A1 - Zamponi, M. A1 - Schönhals, Andreas T1 - Molecular mobility in high-performance polynorbornenes:A combined broadband dielectric, advanced calorimetry,and neutron scattering investigation N2 - The molecular dynamics of two addition type polynorbornenes, exo-PNBSiand PTCNSi1, bearing microporosity has been investigated by broadbanddielectric spectroscopy, fast scanning calorimetry, and neutron scattering. Bothpolymers have the same side groups but different backbones. Due to theirfavorable transport properties, these polymers have potential applications inseparation membranes for gases. It is established in literature that molecularfluctuations are important for the diffusion of small molecules through poly-mers. For exo-PNBSi, two dielectric processes are observed, which are assignedto Maxwell/Wagner/Sillars (MWS) process due to blocking of charge carriersat internal voids or pore walls. For PTCNSi1, one MWS-polarization process isfound. This points to a bimodal pore-size distribution for exo-PNBSi. A glasstransition for exo-PNBSi and for PTCNSi1 could be evidenced for the first timeusing fast scanning calorimetry. For Tgand the corresponding apparent activa-tion energy, higher values were found for PTCNSi1 compared to exo-PNBSi.For both polymers, the neutron scattering data reveal one relaxation process.This process is mainly assigned to methyl group rotation probably overlayedby carbon–carbon torsional fluctuations. KW - Advanced calorimetry KW - Dielectric spectroscopy KW - Neutron scattering KW - Polynorbornenes PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547086 DO - https://doi.org/10.1002/pen.25995 SN - 0032-3888 VL - 62 IS - 7 SP - 2143 EP - 2155 PB - Wiley AN - OPUS4-54708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Niebergall, Ute A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Evaluation of UV-induced embrittlement of PE-HD by Charpy impact test N2 - The impact fracture behavior of two common high-density polyethylene grades for container applications were intensively studied by the instrumented Charpy impact test after well-defined exposure to UV-irradiation. Individual stages of the impact event, such as crack initiation and crack propagation energy as well as maximum impact load, were investigated from the recorded load–deflection curves. UV-induced material property changes were further investigated by infrared spectroscopy, differential scanning calorimetry, and dynamic-mechanical analysis as well as density measurements. Based on the results of the Charpy impact test, three indicators were identified to describe the extend of photooxidation on high-density polyethylene: (a) a reduced Charpy impact strength—at least to half of its initial value for a distinctly brittle impact fracture, (b) a marked decrease in the crack propagation contribution to the impact strength, and (c) an increase of the brittle features of the fracture surface. KW - Degradation KW - Mechanical properties KW - Packaging KW - Polyolefins KW - Polyethylene PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509130 DO - https://doi.org/10.1002/APP.49069 SN - 0021-8995 VL - 137 IS - 36 SP - 49069 PB - Wiley AN - OPUS4-50913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Marschall, Niklas A1 - Alig, I. A1 - Böhning, Martin T1 - A phenomenological criterion for an optical assessment of PE-HD fracture surfaces obtained from FNCT N2 - The full-notch creep test (FNCT) is a common test method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD), e.g. for container materials. The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of PE-HD specimens under constant mechanical load in a well-defined liquid test environment. Since the craze-crack damage mechanism underlying the ESC phenomenon is associated with brittle failure, the occurrence of a predominantly brittle fracture surface is a prerequisite to consider an FNCT measurement as representative for ESC, i.e. a time to failure dominated by craze-crack propagation. The craze-crack propagation continuously reduces the effective residual cross-sectional area of the specimen during the test, which results in a corresponding increase of the effective mechanical stress. Thus, a transition to ductile shear deformation is inevitable at later stages of the test, leading usually to a pronounced central ligament. Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. An enhanced imaging analysis of FNCT fracture surfaces enables a detailed assessment of craze-crack Propagation during ESC. In this study, laser scanning microscopy (LSM) was employed to evaluate whether FNCT fracture surfaces are representative with respect to craze-crack propagation and ESC. Based on LSM height data, a phenomenological criterion is proposed to assess the validity of distinct FNCT measurements. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing. Its applicability is verified on a sample basis for seven different commercial PE-HD container materials. KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Laser scanning microscopy (LSM) KW - Fracture surfaces KW - Optical criterion of brittleness PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521012 DO - https://doi.org/10.1016/j.polymertesting.2020.107002 VL - 94 SP - 107002 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schönhals, Andreas A1 - Böhning, Martin A1 - Szymoniak, Paulina ED - Schönhals, Andreas ED - Szymoniak, Paulina T1 - (Nano)Composite Materials—An Introduction N2 - The chapter gives a brief introduction to (nano)compositecomposite materials having the focus on polymer-based nanocomposites. The different dimensionalities of nanoparticles are introduced, along with their distribution in the matrix. Different application fields of polymer-based nanocomposites, like flame retardancy, filled rubbers, nanofilled thermosets and thermoplastics, separation membranes and nanodielectrics, are considered in greater detail. KW - Polymer-based nanocomposites KW - Nanoparticle KW - Distribution of nanoparticles KW - Filled rubbers KW - Filled thermosets and plastics KW - Separation membranes KW - Nanodielectrics PY - 2022 DO - https://doi.org/10.1007/978-3-030-89723-9_1 SP - 1 EP - 31 PB - Springer CY - Cham, Switzerland AN - OPUS4-54565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Yin, Huajie A1 - Smales, Glen Jacob A1 - Harrison, W. J. A1 - Budd, P. M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Polymers of intrinsic microporosity - Molecular mobility and physical aging revisited by dielectric spectroscopy and X‑ray scattering N2 - Polymers of intrinsic microporosity (PIMs) are promising candidates for the active layer in gas separation membranes due to their high permeability and reasonable permselectivity. These appealing properties originate from a microporous structure as a result of inefficient segment packing in the condensed state due to a combination of a ladder-like rigid backbone and sites of contortion. However, this class of polymers suffers from a significant decrease in the permeability with time due to physical aging, whereby typically, the permselectivity increases. The initial microporous structures approach a denser state via local rearrangements, leading to the reduction of the permeability. Hence, a detailed characterization of the molecular mobility in such materials can provide valuable information on physical aging. In this work, the dielectric behavior of PIM-1 films and their behavior upon heating (aging) were revisited by isothermal frequency scans during different heating/cooling cycles over a broad temperature range between 133 and 523 K (−140 to 250 °C). In addition, the obtained results were compared with data of samples that were annealed at ambient temperatures over different time scales. Multiple dielectric processes were observed: several relaxation processes due to local fluctuations and a Maxwell−Wagner−Sillars polarization effect related to the microporosity. The temperature dependence of the rates of all processes follows the Arrhenius law where the estimated activation energy depends on the nature of the process. The influence of the thermal history (aging) on the processes is discussed in detail. KW - Polymers of intrinsic microporosity PY - 2022 DO - https://doi.org/10.1021/acs.macromol.2c00934 VL - 55 SP - 7340 EP - 7350 PB - American Chemical Society CY - Washington, DC AN - OPUS4-55485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Juranyi, Fanni A1 - Böhning, Martin A1 - Zorn, Reiner A1 - Schönhals, Andreas T1 - Low-Frequency Vibrational Density of State of Janus-Polynorbornenes: The Dependence of the Boson Peak on the Nanophase-Separated Structure N2 - Inelastic incoherent neutron time-of-flight scattering was employed to investigate the low-frequency vibrational density of states (VDOSs) for a series of glassy Janus-poly(tricyclononenes), which consist of a rigid main chain and flexible alkyl side chains. Here, the length of the flexible side chains was systematically varied from propyl to octyl. Such materials have potential applications as active separation layers in gas separation membranes as a green future technology, especially for the separation of higher hydrocarbons. From the morphological point of view, the Janus polynorbornenes undergo a nanophase separation into alkyl side chain-rich nanodomains surrounded by a rigid polynorbornene matrix. Here, the influence of the nanophase-separated structure on the low-frequency VDOS is investigated from a fundamental point of view. The low-frequency VDOSs of these Janus polynorbornene show excess contributions to the Debye type VDOS known as the Boson peak (BP) for all side chain lengths. Due to the high incoherent scattering cross-section of hydrogen, most of the scattering comes from the alkyl side chain-rich domains. Compared to conventional glass-forming materials, in the considered Janus polynorbornenes, the BP has a much lower intensity and its frequency position is shifted to higher values. These experimental results are discussed in terms of the nanophase-separated structure where the alkyl chain-rich domains were constrained by the surrounding matrix dominated by the rigid backbone. With increasing alkyl chain length, the size of the alkyl chain-rich domains increases. The frequency position of the BP shifts linearly to lower frequencies with the size of these nanodomains estimated from X-ray measurements. The obtained results support the sound wave interpretation to the BP KW - Inelastic neutron scattering PY - 2023 DO - https://doi.org/10.1021/acs.macromol.3c00913 SN - 0024-9297 SP - 1 EP - 10 PB - ACS AN - OPUS4-57972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Böhning, Martin A1 - Zorn, Reiner A1 - Schönhals, Andreas T1 - Inelastic and quasielastic neutron scattering experiments on microporous membranes fro green separation processes N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. These polymers are characterized by a high permeability and reasonable permselectivity. The latter point is somehow surprising because for microporous systems a more Knudson-like diffusion is expected then a size dependent temperature activated sieving process. It was argued in the framework of a random gate model that molecular fluctuations on a time scale from ps to ns are responsible for the permselectivity. Here series of polymers of intrinsic microporosity (PIMs) as well as microporous polynorbornenes with bulky Si side groups and a rigid backbone are considered. The polymers have different microporosity characterized by high BET surface area values. First inelastic time-of-flight neutron scattering measurements were carried out to investigate the low frequency density of state (VDOS). The measured data show the characteristic low frequency excess contribution to the VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. It was found that the frequency of the maximum position of the Boson peak correlates with the BET surface area value. Secondly elastic scans as well as quasielastic neutron scattering measurements by a combination of neutron time-of-flight and backscattering have been out. A low temperature relaxation process was found for both polymers. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized. The neutron scattering experiments were accompanied by fast scanning calorimetry and broadband dielectric investigations as well as atomistic molecular dynamic simulations. T2 - Kolloquiumsvortrag an der Technischen Universität München CY - Garching, Germany DA - 20.11.2023 KW - Polymers with intrinsic microporosity PY - 2023 AN - OPUS4-59036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Wald, Oliver A1 - Turky, Gamal A1 - Goering, Harald A1 - Brzezinka, Klaus-Werner A1 - Schartel, Bernhard A1 - Schönhals, Andreas T1 - Dielectric Relaxation and Gas Transport Properties in Polypropylene Based Nanocomposites T2 - ACS 2002 Biennial Symposium "Polymeric Nanomaterials" CY - Rohnert Park, CA, USA DA - 2002-11-17 PY - 2002 SP - 1(?) EP - 3(?) AN - OPUS4-2035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Turky, Gamal A1 - Goering, Harald A1 - Wald, Oliver A1 - Schartel, Bernhard A1 - Schönhals, Andreas T1 - Polypropylene/Clay Nanocomposites - Dielectric Relaxation and Gas Transport Properties T2 - 2nd International Conference on Broadband Dielectric Spectroscopy and Its Applications CY - Leipzig, Germany DA - 2002-09-02 PY - 2002 AN - OPUS4-2037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Goering, Harald A1 - Hao, Ning A1 - Mach, Reinhard A1 - Oleszak, Franz A1 - Schönhals, Andreas T1 - Molecular Mobility and Gas Transport Properties of Polycarbonate-Based Nanocomposites PY - 2003 UR - http://www.ipme.ru/e-journals/RAMS/no_3503/bohning/bohning.html SN - 1606-5131 VL - 5 SP - 155 EP - 159 PB - Advanced Study Center CY - St. Petersburg AN - OPUS4-2884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Dielectric and gas transport properties of polypropylene-clay nanocomposites T2 - DPG-Frühjahrstagung (Polymerphysik), Fachverband CPP, Themenkreis 3 CY - Regensburg, Germany DA - 2002-03-11 PY - 2002 AN - OPUS4-3623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas A1 - Goering, Harald A1 - Böhning, Martin A1 - Fritz, Andreas A1 - Rübner, J. T1 - Structure Analysis of Polymeric Nanomaterials by Relaxation Spectroscopy T2 - Polydays 2002 CY - Berlin, Germany DA - 2002-09-30 PY - 2002 SP - 1(?) AN - OPUS4-2044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Dielectric Relaxation and Gas Transport Properties in Polypropylene Based Nanocomposites T2 - ACS 2002 Biennial Symposium: Polymeric Nanomaterials CY - Rohnert Park, CA, USA DA - 2002-11-17 PY - 2002 AN - OPUS4-3622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goering, Harald A1 - Böhning, Martin A1 - Turky, Gamal A1 - Hao, Ning A1 - Schönhals, Andreas T1 - Molecular Dynamics in Polymer Nanocomposites T2 - Workshop "Glasübergang" CY - Rostock, Germany DA - 2002-12-16 PY - 2002 AN - OPUS4-2061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Goering, Harald A1 - Hao, Ning A1 - Schönhals, Andreas T1 - Gas Transport in Polymer based Nanocomposite Systems T2 - Workshop "Glasübergang" CY - Rostock, Germany DA - 2002-12-16 PY - 2002 AN - OPUS4-2054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Goering, Harald T1 - Herstellung und Charakterisierung von Nanopartikel/Polymer Composites T2 - BAM-Seminar der Abteilung VI "Funktion von Polymeren" CY - Berlin, BAM, Deutschland DA - 2002-09-19 PY - 2002 AN - OPUS4-2040 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Dielectric Properties of Nanocomposites Based on Polystyrene and Polyhedral Oligomeric Phenethyl-Silsesquioxanes N2 - Nanocomposites were prepared by solution blending of polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) into polystyrene (PS). The prepared materials were investigated by dielectric spectroscopy, differential scanning calorimetry (DSC), and density measurements. Additional FTIR investigations were carried out. Pure polystyrene shows two relaxation processes, an intermediate β*-process at lower and the α-relaxation at higher temperatures, the latter corresponding to segmental dynamics (dynamic glass transition). The molecular assignment of the β*-process needs further investigation. PhenethylPOSS can be incorporated into PS up to about 40 wt % without any indication of phase separation. With increasing PhenethylPOSS content, the α-relaxation of the composites shifts to lower temperatures and the loss peak broadens. Thus, the main effect of the nanofiller in the polystyrene matrix is to enhance the segmental dynamics, i.e., plasticization. The incorporation of approximately 40 wt % (approximately 5 mol %) PhenethylPOSS shifts the glass transition temperature Tg by 50 K to lower temperatures. The obtained results for polystyrene are discussed together with those reported recently for polycarbonate where a phase-separated morphology is observed for higher concentrations of PhenethylPOSS. The different behavior of PhenethylPOSS in polystyrene and polycarbonate is interpreted in terms of the different interaction of the phenyl rings within the POSS substituents with the phenyl rings of the polymers. For polystyrene, the interaction is stronger than for polycarbonate which probably leads to the enhanced miscibility of PhenethylPOSS into polystyrene. A detailed analysis of the temperature dependence of the dielectric relaxation strengths points also to additional interactions in the nanocomposites when compared to pure polystyrene. The broadening of the loss peak with increasing concentration is discussed in the framework of composition fluctuations. KW - Polyhedral oligomeric silsesquioxane (POSS) KW - Polymer-based nanocomposites KW - Broadband dielectric spectroscopy KW - Polystyrene PY - 2007 DO - https://doi.org/10.1021/ma071777g SN - 0024-9297 SN - 1520-5835 VL - 40 IS - 26 SP - 9672 EP - 9679 PB - American Chemical Society CY - Washington, DC AN - OPUS4-16492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Structure Property Relationships of Polymeric Nanocomposites based on Polyhedral Oligomeric Silsesquioxanes PY - 2007 SN - 0743-0515 VL - 97 SP - 789 EP - 790 PB - Division of Polymeric Materials Science and Engineering, American Chemical Society CY - Washington, DC AN - OPUS4-15848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Böhning, Martin A1 - Goering, Harald A1 - Hao, Ning A1 - Mach, Reinhard A1 - Schönhals, Andreas ED - Cassidy, P. T1 - Polycarbonate/SiC nanocomposites - Influence of nanoparticle dispersion on molecular mobility and gas transport T2 - 7th International Symposium on Polymers for Advanced Technologies CY - Fort Lauderdale, FL, USA DA - 2005-09-21 KW - Nanocomposites KW - Nanoparticles KW - Polycarbonates KW - Dielectric properties KW - Gas permeation PY - 2005 VL - 16 IS - 2-3 SP - 262 EP - 268 PB - Wiley CY - Chichester AN - OPUS4-7062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Tidjani, Adams A1 - Wald, Oliver A1 - Turky, Gamal A1 - Goering, Harald A1 - Brzezinka, Klaus-Werner A1 - Schartel, Bernhard A1 - Schönhals, Andreas T1 - Polypropylene/Clay Nanocomposites - Gas Transport Characteristics and Molecular Mobility T2 - Polydays 2002 CY - Berlin, Germany DA - 2002-09-30 PY - 2002 SP - 1(?) EP - 2(?) AN - OPUS4-2038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas Transport Characterisation and Molecular Modelling - Possible Corelations and Methodological Extensions T2 - Workshop Glasübergang CY - Berlin, Germany DA - 2003-12-14 PY - 2003 AN - OPUS4-4197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuchel, M. A1 - Böhning, Martin A1 - Hölck, Ole A1 - Siegert, M.R. A1 - Hofmann, D. T1 - Atomistic Packing Models for Experimentally Investigated Swelling States Induced by CO2 in Glassy Polysulfone and Poly(ether sulfone) N2 - Atomistic packing models have been created, which help to better understand the experimentally observed swelling behavior of glassy polysulfone and poly (ether sulfone), under CO2 gas pressures up to 50 bar at 308 K. The experimental characterization includes the measurement of the time-dependent volume dilation of the polymer samples after a pressure step and the determination of the corresponding gas concentrations by gravimetric gas-sorption measurements. The models obtained by force-field-based molecular mechanics and molecular dynamics methods allow a detailed atomistic analysis of representative swelling states of polymer/gas systems, with respect to the dilation of the matrix. Also, changes of free volume distribution and backbone mobility are accessible. The behavior of gas molecules in unswollen and swollen polymer matrices is characterized in terms of sorption, diffusion, and plasticization. KW - Molecular modeling KW - Volume dilation KW - Gas sorption KW - Poly(ether sulfones) KW - Free volume KW - Swelling KW - Molecular dynamics KW - Diffusion KW - Plasticization PY - 2006 DO - https://doi.org/10.1002/polb.20844 SN - 0887-6266 SN - 1099-0488 VL - 44 IS - 13 SP - 1874 EP - 1897 PB - Wiley CY - Hoboken, NJ AN - OPUS4-12398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuchel, M. A1 - Böhning, Martin A1 - Hölck, Ole A1 - Siegert, M.R. A1 - Hofmann, D. T1 - Atomistic packing models for experimentally investigated swelling states induced by CO2 in glassy polymers KW - Glassy polymers KW - Sorption KW - Swelling KW - Molecular Modelling PY - 2006 DO - https://doi.org/10.1016/j.desal.2006.03.100 SN - 0011-9164 VL - 199 IS - 1-3 SP - 443 EP - 444 PB - Elsevier CY - Amsterdam AN - OPUS4-13708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Hao, Ning A1 - Schönhals, Andreas T1 - Gas transport and molecular mobility in polymer/POSS nanocomposites PY - 2006 DO - https://doi.org/10.1016/j.desal.2006.03.127 SN - 0011-9164 VL - 200 IS - 1-3 SP - 142 EP - 143 PB - Elsevier CY - Amsterdam AN - OPUS4-13707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, N. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - CO2 gas transport properties of nanocomposites based on polyhedral oligomeric phenethyl-silsesquioxanes and poly(bisphenol A carbonate) N2 - Polymer-based nanocomposites were prepared by solution blending of polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) into poly(bisphenol A carbonate) (PBAC). First investigations focused on structure, morphology and dynamics, addressed mainly by dielectric relaxation spectroscopy are substantially extended in this study by the investigation of the CO2 gas transport behavior of these materials, i.e., permeation experiments using the time-lag technique as well as gravimetric gas sorption measurements. The nanocomposite materials were prepared with nanofiller contents ranging from 0 to about 40 wt % by solution blending and films of about 50-100 µm thickness were cast from this solution and used for the investigation of gas transport properties after drying and annealing. From the time-lag measurements the permeability and an effective diffusion coefficient for CO2 is obtained in dependence of POSS concentration and temperature. As main results, both, the permeability and the diffusivity, increase whereas the solubility decreases with increasing POSS concentration. These findings are discussed in the framework of a microphase separated morphology of the nanocomposite systems for POSS concentrations greater than a value cPOSScrit of ca. 7 wt % consisting of a polycarbonate-rich matrix and POSS-rich domains which are surrounded by an interfacial layer. The experimental solubility data suggest that the POSS-rich domains are more or less impermeable for CO2. On the basis of this assumption a quantitative model is provided to correct the solubility data for the phase separated morphology. Moreover the importance of the interfacial layer between the POSS particles or its domains for the properties of nanocomposites especially for the gas transport behavior is addressed by analyzing the sorption isotherms. Also, for the first time results from gas transport measurements and dielectric spectroscopy were quantitatively related to each other by taking the activation energies of CO2 diffusion and of the dielectric β-relaxation into consideration. The obtained clear correlation indicates that the CO2 gas transport is due to localized molecular fluctuations. As a further result, the diffusion coefficient obtained from time-lag and gas sorption measurements is in good agreement with respect to both their absolute values and in their concentration dependence. PY - 2010 DO - https://doi.org/10.1021/ma101463m SN - 0024-9297 SN - 1520-5835 VL - 43 IS - 22 SP - 9417 EP - 9425 PB - American Chemical Society CY - Washington, DC AN - OPUS4-22378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Möglichkeiten der Abschätzung der Langzeitbeständigkeit von Kunststoffdichtungsbahnen (KDB) auf Polyolefinbasis für den Tunnelbau T2 - Fachtagung der Kompetenzplattformen "Life Cycle Assessment (LCA)" neuer Kunststoffe der FH Münster und "Polymere Materialien" der FH Aachen CY - Münster, Germany DA - 2010-02-25 PY - 2010 AN - OPUS4-21019 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Oxidationsbeständigkeit von Geokunststoffen T2 - 10. Schwarzheider Kunststoffkolloquium CY - Schwarzheide, Germany DA - 2010-09-08 PY - 2010 AN - OPUS4-22103 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Characterization of structural changes in irradiated UHMWPE T2 - 11. Schwarzheider Kunststoffkolloquium CY - Schwarzheide, Germany DA - 2011-09-21 PY - 2011 AN - OPUS4-24423 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Schmaucks, G. A1 - von der Ehe, Kerstin A1 - Böhning, Martin T1 - Effect of well dispersed amorphous silicon dioxide in flame retarded styrene butadiene rubber N2 - Spherically shaped amorphous silicon dioxide with broad size particle distribution was used in combination with aluminium trihydroxide (ATH) in styrene butadiene rubber composites. The pyrolysis, flammability, fire properties, flame spread and gas diffusion were investigated. The kind and amount of ATH, but in particular the fine silicon dioxide chosen as an additive, influenced the thermal decomposition and fire behaviour of styrene butadiene rubber composites. Gravimetric gas sorption measurements showed that the gas diffusion was systematically lower with silicon dioxide. The initial pyrolysis gas release was hindered, increasing the temperature at which decomposition begins as well as the ignition time in fire tests. During combustion, ATH and silicon dioxide accumulate on the surface of the specimen, forming a residual protective layer. A reduced peak heat release rate and fire spread were observed. The addition of a special kind of silicon dioxide is proposed to play a key role in optimising fire retardancy. KW - Flame retardancy KW - Styrene butadiene rubber KW - SBR KW - Silicon dioxide KW - Aluminium trihydroxide KW - ATH PY - 2013 DO - https://doi.org/10.1179/1743289812Y.0000000012 SN - 1465-8011 SN - 1743-2898 VL - 42 IS - 1 SP - 34 EP - 42 PB - IOM Communications CY - London, UK AN - OPUS4-27626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Niebergall, Ute A1 - Adam, Adeline A1 - Stark, Wolfgang T1 - Influence of biodiesel sorption on temperature-dependent impact properties of polyethylene N2 - In a previous paper we investigated the influence of sorbed biodiesel or diesel on mechanical properties of a typical polyethylene grade for tank applications. Besides the basic sorption and desorption behavior of these two fuels, the study addressed the concentration-dependent mechanical properties as revealed by a non-instrumented Charpy impact test and dynamic mechanical analysis (DMA). In the present paper we extend this investigation focusing on the temperature-dependent impact fracture behavior. Therefore, an instrumented Charpy impact test was employed, allowing a more detailed analysis of the fracture behavior. Furthermore, from the load-time-diagrams obtained from the instrumented impact test, corresponding fracture times can be calculated, allowing a clear correlation of the fuel sorption induced changes in fracture toughness with the enhanced ß-relaxation observed by DMA. As in the previous study, the fracture surfaces of the impact tested specimens were analyzed in order to confirm the brittle or ductile character of the fracture indicated by impact strength and the corresponding load-deflection diagrams. KW - Biodiesel KW - Fuel sorption KW - Impact strength KW - Charpy impact test KW - Dynamic-mechanical analysis KW - Relaxation KW - PE-HD PY - 2014 DO - https://doi.org/10.1016/j.polymertesting.2014.09.001 SN - 0142-9418 VL - 40 SP - 133 EP - 142 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-31583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Hao, Ning A1 - Schönhals, Andreas T1 - Correlation of activation energies of gas diffusivity and local matrix mobility in polycarbonate/POSS nanocomposites N2 - According to basic phenomenological models describing the solution-diffusion based mechanism of penetrant diffusion in dense polymers, a connection between the diffusive transport of gas molecules in a polymeric matrix and the molecular mobility of that matrix on a certain length scale is, in principle, established for a long time. However, experimental data directly showing this correlation are rare. The investigation of a series of nanocomposites based on a polyhedral oligomeric silsesquioxane (POSS) and a polycarbonate matrix allows a systematic change of the molecular mobility on a local length scale (β-relaxation) and of the corresponding activation energy EA, both determined by broadband dielectric spectroscopy. Independently, activation energies of penetrant diffusion (ED) of these nanocomposites were determined for N2, O2, CO2, and CH4 and a clear linear correlation between the two activation energies was established for the first time. KW - Broadband dielectric spectroscopy KW - Diffusion KW - Dielectric properties KW - Gas permeation KW - Molecular mobility KW - Nanocomposites KW - Polyhedral oligomeric silsesquioxane (POSS) KW - Relaxation KW - Beta-relaxation PY - 2013 UR - http://onlinelibrary.wiley.com/doi/10.1002/polb.23381/full DO - https://doi.org/10.1002/polb.23381 SN - 0887-6266 SN - 1099-0488 VL - 51 IS - 22 SP - 1593 EP - 1597 PB - Wiley CY - Hoboken, NJ AN - OPUS4-29284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Böhning, Martin A1 - Krafft, Bernd A1 - Schartel, Bernhard T1 - Chlorbutylkautschuk/Multilayergraphen-Nanocomposites N2 - In den letzten Jahren werden zunehmend Nanopartikel als Füllstoff für Polymere vorgeschlagen und auch erfolgreich in Elastomer-Nanocomposites eingesetzt. In dieser Arbeit wird Multilayergraphen (MLG) als Nanofüllstoff näher untersucht, der sich bereits bei geringen Konzentrationen als effizient erweist. MLG besteht aus nur etwa zehn Graphenlagen. Chlorbutylkautschuk (CIIR)/MLG-Nanocomposites mit verschiedenen MLG-Gehalten wurden mit Hilfe eines ultraschallunterstützen Mischverfahrens in Lösung hergestellt und auf einem Walzwerk weiterverarbeitet. Das Einmischen von MLG führt zu einer deutlichen Verbesserung der rheologischen und mechanischen Eigenschaften, des Vernetzungsverhaltens sowie der Barrierewirkung gegenüber Gasen. Bereits der Zusatz von 3 phr MLG zu CIIR führt zu einem mehr als zweifach höheren E-Modul und zu einer Reduktion der Permeabilität von O2 und CO2 um 30 %. Höhere Konzentrationen an Nanofüllstoff resultieren in einer weiteren Verbesserung der Eigenschaften der Nanocomposites. Weiterhin zeigten die CIIR/MLG-Nanocomposites auch eine geringere Entflammbarkeit. KW - Elastomere KW - Nanokomposite KW - Graphen KW - Chlorbutylkautschuk PY - 2017 SN - 0176-1625 VL - 70 IS - 5 SP - 311 EP - 322 PB - Dr. Gupta Verlag CY - Ratingen AN - OPUS4-40327 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thuy, Maximilian A1 - Brauch, N. A1 - Niebergall, Ute A1 - Alig, I. A1 - Oehler, H. A1 - Böhning, Martin T1 - Environmental Stress Cracking of PE-HD Induced by Liquid Test Media Representing Crop Protection Formulations N2 - Packaging containers for dangerous goods that include aggressive liquids require that any packaging material that is based on high-density polyethylene has a high degree of stability and durability. This work is focused on testing the environmental stress cracking of the high-density polyethylenes used for such containers in contact with crop protection formulations, in particular, two model liquids established in Germany as standardized test media representatives for crop protection formulations containing the various admixtures typical for such products. One of the liquids is water-based and contains mostly surface-active ingredients, while the other is solvent-based and includes some emulsifiers. Originally established for pin impression tests, these model liquids and their individual components were here used for the first time as environmental media in the Full Notch Creep Test, which addresses the resistance against environmental stress cracking. The Full Notch Creep Test was carried out on five high-density polyethylene types with both model liquids, and also on one selected material with its components. The evaluation was focused on the fracture surface structures, which were visualized by a scanning electron microscope and by optical in situ imaging of the notch opening. While the water-based model liquid and its surface-active individual components induced environmental stress cracking with the characteristic pattern for a craze-crack mechanism and so-called brittle fracture on the surface, the solvent-based model liquid and its soluble ingredients exhibited rather ductile failure behavior, caused by the plasticizing effect on the polymer that reduced the yield stress of the high-density polyethylene. For both cases, fracture surface analysis, together with side views of the crack opening, showed a clear relation between surface pattern, notch deformation (e.g., by blunting), or crack opening due to crack growth with time to failure and the solubility of the liquids in high-density polyethylene. KW - Environmental stress cracking KW - Fracture surface KW - Full Notch Creep Test KW - Crop protection formulations KW - High-density polyethylene PY - 2023 DO - https://doi.org/10.1520/STP164320210095 SP - 317 EP - 341 PB - ASTM International CY - West Conshohocken, PA (USA) AN - OPUS4-57459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Böhning, Martin A1 - Oehler, H. A1 - Alig, I. A1 - Niebergall, Ute T1 - Environmental stress cracking of polyethylene high density (PE-HD) induced by liquid media – Validation and verification of the full-notch creep test (FNCT) T1 - Umgebungsinduzierte Spannungsrissbildung von Polyethylen- Werkstoffen hoher Dichte durch flüssige Medien – Validierung und Verifizierung des Kriechversuchs an Probekörpern mit umlaufender Kerbe N2 - The full-notch creep test (FNCT) is widely used to characterize the slow crack growth (SCG) behavior of polyolefin materials in “inert” media as well as effects of environmental stress cracking (ESC) in which the medium has decisive influence on damage mechanism and time to failure. The test is of greatest importance for pipe and blow molding types of polyethylene, high density (PE-HD). Usually the full-notch creep test is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100. In our study, selected relevant polyethylene, high density materials are investigated also in real media – practical formulations as well as representative pure chemicals – and influences of temperature and geometry of specimen and notch are explicitly addressed. Furthermore, the investigations comprise also the environmental stress cracking behavior of polyethylene, high density in media that are sorbed to a significant extent – examples are diesel and biodiesel – based on comparison with samples previously saturated with those media. Thus, also the underlying diffusion controlled sorption process has to be assessed before. The investigations were performed using a full-notch creep testing device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation. N2 - Der Kriechversuch an Probekörpern mit umlaufender Kerbe (FNCT) wird flächendeckend angewendet, um das Verhalten von Polyolefinen sowohl gegenüber langsamen Risswachstums (SCG) bei Kontakt mit „inerten“ Medien als auch gegenüber umgebungsbedingtem Spannungsrisswachstum (ESC), bei welchem das umgebende Medium entscheidenden Einfluss auf den Schädigungsmechanismus und die Standzeit hat, zu charakterisieren. Der Test ist von großer Bedeutung bei der Analyse von hochdichten Polyethylen-Typen, die als Rohr- und Blasformwerkstoffe angewendet werden – dabei besonders für Transport und Verpackung von Gefahrstoffen, aber auch für weitere Hochleistungsanwendungen. Üblicherweise wird der Kriechversuch an Probekörpern mit umlaufender Kerbe als Normmethode (ISO 16770) unter Verwendung einiger weniger universeller Modellflüssigkeiten, wie z. B. Arkopal N 100, durchgeführt. In dieser Studie werden ausgewählte, marktrelevante Polyethylen-Werkstoffe hoher Dichte in realen Medien – praktisch verwendete Gefahrgüter sowie repräsentative reine Chemikalien – untersucht und explizit die Einflüsse von Temperatur und Prüfkörper- sowie Kerbgeometrie adressiert. Weiterhin beinhalten die Untersuchungen die Analyse des umgebungsbedingten Spannungsriss-Verhaltens von Polyethylen hoher Dichte in Medien, die maßgeblich vom Werkstoff sorbiert sind – beispielsweise mit Kraftstoffen wie diesel und biodiesel – basierend auf dem Vergleich mit vorgesättigten Probekörpern. Der dabei vorliegende diffusionsgesteuerte Sorptionsprozess muss dementsprechend zuvor evaluiert werden. Alle Untersuchungen wurden mithilfe einer Kriechversuchsanlage an Probekörpern mit umlaufender Kerbe mit 12 Stationen durchgeführt, welche jeweils mit einer individuell ansteuerbaren elektronischen Spannungs- und Temperatursteuerung sowie fortwährender Online-Überwachung der Prüfkörperdehnung ausgestattet sind. KW - Full-notch creep test (FNCT) KW - Polyethylene (PE-HD) KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Biodiesel PY - 2017 DO - https://doi.org/10.1002/mawe.201700065 SN - 1521-4052 SN - 0933-5137 VL - 48 IS - 9 SP - 846 EP - 854 PB - Wiley-VCH CY - Weinheim AN - OPUS4-41885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Dielectric investigations of nanocomposites based on matrimid and polyhedral oligomeric phenethyl-silsesquioxanes (POSS) N2 - Matrimid and Matrimid/PhenethylPOSS nanocomposites films were prepared by solution casting. They can be considered as potential membrane materials for gas separation. Theire dielectric properties were investigated using Broadband Dielectric Spectroscopy (BDS) in combination with standard techniques. Matrimid shows one relaxation process assigned as beta*-relaxation and a conductivity contribution. The relaxation process has a high activation energy of 99 kJ/mol. Thus this process is supposed to be of cooperative nature due to a π-π stacking of the phenyl rings of Matrimid. The influence of the thermal history on Matrimid was analyzed with BDS as well where an annealing effect is found. The Matrimid/PhenethylPOSS nanocomposites show up to a concentration of about 4 wt% PhenethylPOSS a miscibility on a molecular level. For higher concentrations a phase separated structure was indicated. The conductivity of both systems is explained by π-π stacking of the phenyl rings which enhances charge transport. KW - Matrimid KW - POSS KW - Nanocomposites KW - Broadband dielectric spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.polymer.2016.02.060 SN - 0032-3861 VL - 90 SP - 89 EP - 101 PB - Elsevier Science AN - OPUS4-35616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Ding, Yi A1 - Harrison, W.J. A1 - Budd, P.M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility and gas transport properties of nanocomposites based on PIM-1 and polyhedral oligomeric phenethyl-silsesquioxanes (POSS) N2 - 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. KW - Broadband Dielectric Spectroscopy KW - Gas separation KW - Gas permeation KW - Polymers of intrinsic microporosity KW - Nanocomposite KW - POSS KW - PIM-1 PY - 2017 DO - https://doi.org/10.1016/j.memsci.2017.02.007 SN - 0376-7388 SN - 1873-3123 VL - 529 SP - 274 EP - 285 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-39169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Alig, I. A1 - Oehler, H. A1 - Lellinger, D. A1 - Meinel, Dietmar A1 - Böhning, Martin T1 - Crack propagation in PE-HD induced by environmental stress cracking (ESC) analyzed by several imaging techniques N2 - Different imaging techniques were employed to monitor Full Notch Creep Test (FNCT) experiments addressing environmental stress cracking in more detail. The FNCT is a well-established test method to assess slow crack growth and environmental stress cracking of polymer materials, especially polyethylene. The standard test procedure, as specified in ISO 16770, provides a simple comparative measure of the resistance to crack growth of a certain material based on the overall time to failure when loaded with a well-defined mechanical stress and immersed in a liquid medium promoting crack propagation. Destructive techniques which require a direct view on the free fracture surface, such as light microscopy and laser scanning microscopy, are compared to non-destructive techniques, i.e. scanning acoustic microscopy and xray micro computed tomography. All methods allow the determination of an effective crack length. Based on a series of FNCT specimens progressively damaged for varied Durations under standard test conditions, the estimation of crack propagation rates is also enabled. Despite systematic deviations related to the respective Imaging techniques, this nevertheless provides a valuable tool for the detailed evaluation of the FNCT and its further development. KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Full notch creep test (FNCT) KW - X-ray computed tomography (CT) KW - Laser scanning microscopy (LSM) KW - Scanning acoustic microscopy (SAM) PY - 2018 DO - https://doi.org/10.1016/j.polymertesting.2018.08.014 SN - 0142-9418 SN - 1873-2348 VL - 70 SP - 544 EP - 555 PB - Elsevier AN - OPUS4-45766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Full notch creep test (FNCT) of PE-HD – Characterization and differentiation of brittle and ductile fracture behavior during environmental stress cracking (ESC) N2 - The damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC), relevant for PE-HD materials are characterized based on improved full notch creep testing (FNCT) of two selected typical PE-HD materials for container applications. In this context, a distinction of the failure mechanisms as well as a categorization of involved media is suggested. Employing a novel FNCT device, elongation data were obtained in addition to conventional time-to-failure results of stress-dependent as well as temperature-dependent measurements. Changes in failure behavior, as determined by fracture surface analysis based on light microscopy (LM) and laser scanning microscopy (LSM), are correlated with FNCT results and used to introduce an additional possibility for the identification of brittle/ductile fracture behavior. KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Full notch creep test (FNCT) KW - High-density polyethylene (PE-HD) PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.09.043 SN - 0142-9418 SN - 1873-2348 VL - 64 SP - 156 EP - 166 PB - Elsevier CY - Amsterdam AN - OPUS4-42484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Marschall, Niklas A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Modernizing FNCT data handling in polymer labs: Towards efficient management N2 - A streamlined Python-based workflow for transforming Full-Notch Creep Test (FNCT) data into organized, machine-actionable formats is presented. The workflow automates the conversion of raw FNCT data from classic CSV and Excel files into structured outputs that facilitate future semantic integration. Emphasizing practical data handling, the approach includes automation scripts for efficient data extraction, transformation, and storage, which culminate in well-ordered files. This transformation paves the way for potential semantic data integration and facilitates access for users with varying levels of digital experience to enhanced data management in polymer research and testing. KW - PE-HD KW - Full-Notch Creep Test (FNCT) KW - Environmental Stress Cracking (ESC) KW - Data Interoperability KW - FAIR Data KW - Semantic Data PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637826 DO - https://doi.org/10.1016/j.commatsci.2025.114085 SN - 0927-0256 VL - 259 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-63782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Marschall, Niklas A1 - Meinel, Dietmar A1 - Böhning, Martin T1 - Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene N2 - The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements. Highlights - Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques - Determined growth rates depend on distinction between craze zone and crack - The ratio of the present crack to the anteceding craze zone is validated theoretically - The transition from crack propagation to ductile shear deformation is identified - An already formed craze zone may still fail by ductile mechanisms KW - Craze-crack mechanism KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Laser scanning microscopy (LSM) KW - Slow crack growth (SCG) KW - X-ray computed tomography (CT) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601831 DO - https://doi.org/10.1002/pen.26698 SN - 1548-2634 VL - 64 IS - 6 SP - 2387 EP - 2403 PB - Wiley AN - OPUS4-60183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Mosane Razavi, Negar A1 - Bojdys, M. J. A1 - Forster, A. B. A1 - Budd, P. M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Mobility and Gas Transport Properties of Mixed Matrix Membranes Based on PIM‑1 and a Phosphinine Containing Covalent Organic Framework N2 - Polymers with intrinsic microporosity (PIMs) are gaining attention as gas separation membranes. Nevertheless, they face limitations due to pronounced physical aging. In this study a covalent organic framework containing λ5-phosphinine moieties, CPSF-EtO were incorporated as a nanofiller (concentration range 0-10 wt%) into a PIM-1 matrix forming dense films with a thickness of ca. 100 μm. The aim of the investigation was to investigate possible enhancements of gas transport properties and mitigating effects on physical aging. The incorporation of the nanofiller occurred on aggregate level with domains up to 100 nm as observed by T-SEM and confirmed by X-ray scattering. Moreover, the X-ray data show that the structure of the microporous network of the PIM-1 matrix is changed by the nanofiller. As the molecular mobility is fundamental for gas transport as well as for physical aging, the study includes dielectric investigations of pure PIM-1 and PIM-1/CPSF-EtO mixed matrix membranes to establish a correlation between the molecular mobility and the gas transport properties. Using the time-lag method the gas permeability and the permselectivity were determined for N2, O2, CH4 and CO2 for samples with variation in filler content. A significant increase in the permeability of CH4 and CO2 (50 % increase compared to pure PIM-1) was observed for a concentration of 5 wt% of the nanofiller. Furthermore, the most pronounced change in the permselectivity was found for the gas pair CO2/N2 at a filler concentration of 7 wt%. KW - Polymers of Intrinsic Microporosity KW - Nanocomposites PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595031 DO - https://doi.org/10.1021/acs.macromol.3c02419 SN - 0024-9297 VL - 57 IS - 4 SP - 1829 EP - 1845 PB - ACS Publications AN - OPUS4-59503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Damaging effect of admixtures used in crop protection products on high density polyethylene packaging material N2 - The phenomenon of environmental stress cracking is still a major issue in materials engineering as well as from a scientific perspective. Especially in the case of packaging materials made of high-density polyethylene, assessing the potential of premature damage due to environmental stress cracking is complex because of the large number of components in possible liquid filling goods. As a first guideline, the well-known effect of detergents and dispersants is usually considered, but the interplay with other components, such as organic solvents is often unknown. Particularly challenging in this respect are crop protection products, consisting of several different admixtures in addition to the biologically active ingredients. This study is based on two model liquids representing these admixtures that were established for testing in this context. The model liquids as well as their constituting components were used as liquid media in the Full Notch Creep Test to characterize the environmental stress cracking behavior of a typical high-density polyethylene. Complementary to the time-to failure of a notched specimen obtained from these tests, the crack opening was monitored optically, and the fracture surface was analyzed post-failure by laser scanning microscopy as well as scanning electron microscopy. Based on the results, the effect of various surfactants as well as the influence of organic solvents on environmental stress cracking are discussed. KW - Environmental stress cracking KW - High-density polyethylene KW - Crop protection products KW - Full notch creep test KW - Fracture surface analysis KW - Crack opening displacement PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554631 DO - https://doi.org/10.1016/j.polymertesting.2022.107672 SN - 0142-9418 VL - 114 SP - 1 EP - 16 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-55463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Schulze, Dietmar A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - Networking Skills: The Effect of Graphene on the Crosslinking of Natural Rubber Nanocomposites with Sulfur and Peroxide Systems N2 - Tailored crosslinking in elastomers is crucial for their technical applications. The incorporation of nanoparticles with high surface-to-volume ratios not only leads to the formation of physical networks and influences the ultimate performance of nanocomposites, but it also affects the chemical crosslinking reactions. The influence of few-layer graphene (FLG) on the crosslinking behavior of natural rubber is investigated. Four different curing systems, two sulfur-based with different accelerator-to-sulfur ratios, and two peroxide-based with different peroxide concentrations, are combined with different FLG contents. Using differential scanning calorimetry (DSC), vulcametry (MDR) and swelling measurements, the results show an accelerating effect of FLG on the kinetics of the sulfur-based curing systems, with an exothermic reaction peak in DSC shifted to lower temperatures and lower scorch and curing times in the MDR. While a higher accelerator-to-sulfur ratio in combination with FLG leads to reduced crosslinking densities, the peroxide crosslinkers are hardly affected by the presence of FLG. The good agreement of crosslink densities obtained from the swelling behavior confirms the suitability of vulcameter measurements for monitoring the complex vulcanization process of such nanocomposite systems in a simple and efficient way. The reinforcing effect of FLG shows the highest relative improvements in weakly crosslinked nanocomposites. KW - Nanocomposite KW - Elastomers KW - Graphene KW - Crosslinking KW - Network KW - Rubber KW - Vulcanization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560409 DO - https://doi.org/10.3390/polym14204363 VL - 14 IS - 20 PB - MDPI AN - OPUS4-56040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Schulze, Dietmar A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - The quantification of anisotropy in graphene/natural rubber nanocomposites: Evaluation of the aspect ratio, concentration, and crosslinking N2 - In the processing of nanocomposites, high shear stresses at elevated tempera-tures orient two-dimensional nanoparticles like graphene. This orientationleads to anisotropic mechanical, thermal or barrier properties of the nanocom-posite. This anisotropy is addressed in this study by comparing graphene (few-layer graphene, FLG) with a nanoscaled carbon black (nCB) at a filler contentof 3 phr, by varying the vulcanization, and by comparing different FLG con-tents. Transmission electron microscopy gives insight into the qualitative ori-entation in the nanocomposite with FLG or nCB. The storage moduli paralleland normal to the orientation reveal the direction dependency of reinforce-ment through dynamic mechanical analysis (DMA). Dimensional swellingmeasurements show a restriction of the expansion parallel to the FLG orienta-tion, and an increased expansion normal to the orientation. The vulcanizationsystem and crosslinking determine the respective level of property values, andhigher crosslinking densities increase the anisotropy in DMA resulting invalues of up to 2.9 for the quantified anisotropy factor. With increasing FLGcontent, the anisotropy increases. A comparison of the results reveals swellingmeasurements as the most suitable method for the determination of anisot-ropy. Compared to recent literature, the presented processing induces higheranisotropy, leading to higher reinforcing effects in the direction of orientation KW - Natural rubber KW - Graphene KW - Nanocomposite KW - Mechanical properties KW - Swelling PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571522 DO - https://doi.org/10.1002/app.53753 SN - 1097-4628 VL - 140 IS - 16 SP - 1 EP - 15 PB - Wiley online library CY - Hoboken, New Jersey (USA) AN - OPUS4-57152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Szymoniak, Paulina A1 - Bojdys, M. J. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Structure and molecular mobility of phosphinine-based covalent organic frameworks – glass transition of amorphous COFs N2 - Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy. Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials. KW - Covalent Organic frameworks PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596770 DO - https://doi.org/10.1039/d3ma01123b SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Lohstroh, W. A1 - Zamponi, M. A1 - Harrison, W. A1 - Budd, P. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular mobility of a polymer of intrinsic microporosity revealed by quasielastic neutron scattering N2 - Quasielastic neutron scattering by employing a combination of time-of-flight and backscattering techniques is carried out to explore the molecular mobility of a polymer of intrinsic microporosity (PIM-1) at microscopic time scales in comparison with a high-performance polyimide. Molecular fluctuations can change the structure of the temporary network of micropores and open or close pathways for gas molecules. Therefore, the investigation might help to understand the selectivity of PIMs in gas separation processes. The performed neutron scattering experiments provide evidence for a low-temperature relaxation process, which was assigned to methyl group rotation. This methyl group rotation was analyzed in terms of jump diffusion in a three-fold potential. The analysis results in a fraction of methyl groups which are immobilized. For PIM-1 it was found that the fraction of immobilized methyl groups decreases with increasing temperature up to 350 K. At higher temperatures the number of immobilized methyl group increases gain due to an underlying relaxation process. This motional process on a somewhat larger length scale might lead to a reversible structural rearrangement which partially hinders the strongly localized methyl group rotation. In addition, it was found that the activation energy for the methyl group rotation for PIM-1 and the polyimide is significantly higher than for conventional polymers. KW - Polymer of intrinsic microporosity KW - Quasielastic neutron scattering PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c00963 SN - 0024-9297 SN - 1520-5835 VL - 53 IS - 15 SP - 6731 EP - 6739 PB - American Chemical Society CY - Washington, DC AN - OPUS4-51147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation N2 - For the first time, dielectric and calorimetric investigations of an homologous series of Janus polynorbornenes with rigid main backbones and flexible -Si(OR)3 side groups, of differing length alkyl chains (R = Propyl, Butyl, Hexyl, Octyl, Decyl) is reported. Generally, this class of polymers has some potential for applications in the field of gas separation membranes. Two dielectrically active processes are observed at low temperatures, denoted as β- and α- relaxation. The former can be assigned to localized fluctuations, whilst the latter is related to the glassy dynamics of the flexible -Si(OR)3 side groups, creating a nanophase separation in both the alkyl chain rich and backbone rich domains. This is confirmed through temperature modulated DSC measurements and X-ray scattering experiments. The glass transition temperatures of the backbone rich domains, which are beyond or near to their degradation temperatures in terms of conventional DSC, are determined for the first time using Fast Scanning Calorimetry employing both fast heating and cooling rates. This is complimented with scattering experiments that show how the size of the alkyl chain rich domains increases with chain length. Alongside these results, a significant conductivity contribution was observed for all poly(tricyclononenes) with -Si(OR)3 side groups, which is interpreted in terms of a percolation model. KW - Polynorbornenes KW - Broadband Dielectric Spectrscopy KW - Advanced calorimetry PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c01450 VL - 53 IS - 17 SP - 7410 EP - 7419 PB - ACS AN - OPUS4-51196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönhals, Andreas A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Böhning, Martin A1 - Zamponi, M. A1 - Frick, B. A1 - Appel, M. A1 - Günther, G. A1 - Russina, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Zorn, R. T1 - Microscopic dynamics of highly permeable super glassy polynorbornenes revealed by quasielastic neutron scattering N2 - The molecular dynamics of addition-type poly(tricyclononenes) with Si-substituted bulky side groups has been investigated by a combination of neutron time-of-flight and neutron backscattering spectroscopy methods on a time scale from 0.1 ps to ca. 3 ns. The investigated poly(tricyclononenes) PTCNSi1 and PTCNSi2g both bear a high microporosity which makes them promising candidates for active separation layers for gas separation membranes. At least for larger gas molecules it is assumed that the pathways for diffusion require an enlargement of pre-existing micropores in terms of an activated zone. A low temperature relaxation process was found for both polymers by the performed neutron scattering experiments. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized. For PTCNSi1 (3 methyl groups in the monomeric unit) it was found that all methyl groups take part in the methyl group rotation whereas for PTCNSi2g (6 methyl groups in monomeric unit) a considerable number of methyl groups are blocked in their rotation. This immobilization of methyl groups is due to the sterically demanding arrangement of the methyl groups in PTCNSi2g. This conclusion is further supported by the result that the activation energy for the methyl group rotation is three times higher for PTCNSi2g than that of PTCNSi1. KW - Highly permeably polynorbornenes KW - Polymers of intrinsic microporosity KW - Gas separation membranes KW - Quasielastic neutron scattering PY - 2021 DO - https://doi.org/10.1016/j.memsci.2021.119972 SN - 0376-7388 VL - 642 PB - Elesevier B.V. AN - OPUS4-53508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Bermeshev, M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility of polynorbornenes with trimethylsiloxysilyl side groups: Influence of the polymerization mechanism N2 - We report dielectric and calorimetric studies on metathesis and addition-type polytricyclononenes, both based on the same monomer bearing three pendant OSiMe3 groups. For the addition-type polymer, dielectric spectroscopy reveals a β*-process related to the microporosity, whereas for its metathesis counterpart, the segmental dynamics manifests as an α-process related to a glass transition. Besides active dielectric processes, a significant conductivity contribution is detected for both samples which for the microporous additiontype polymer is three orders of magnitude greater than for the metathesis polymer. The broadband dielectric spectroscopy is complemented by detailed calorimetric investigations, comprising DSC, FSC, and TMDSC. The calorimetric methods detected the glass transition for the metathesis polymer in agreement with the observed dielectric α-process. Furthermore, the already reported gas transport properties for both polymers are compared, setting them in correlation with the observed molecular mobility and conductivity behavior. The discussed results reflect significant differences in molecular mobility of the two polymers affecting the appearance of microporosity which strongly determines the gas transport properties. KW - Microporous polymers KW - Molecular mobility KW - Electrical conductivity KW - Membrane polymers KW - Gas separation PY - 2022 DO - https://doi.org/10.22079/JMSR.2021.538060.1495 SN - 2476-5406 VL - 8 IS - 3 SP - 1 EP - 9 PB - Membrane Processes Research Laboratory (MPRL) CY - Tehran AN - OPUS4-54303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Wolf, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrational density of state of highly permeable super glassy polynorbornenes – The Boson peak N2 - Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes. All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak. KW - Polynorbornes KW - Neutron Scattering PY - 2020 DO - https://doi.org/10.1039/d0cp03360j SN - 1463-9076 VL - 22 IS - 33 SP - 18381 EP - 18387 PB - Royal Chemical Society AN - OPUS4-51165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Böhning, Martin A1 - Goering, Harald A1 - Hao, Ning A1 - Schönhals, Andreas T1 - Polymer-based Nanocomposites - Particle Dispersion and Physical Properties T2 - Nanofair 2005 CY - Dresden, Germany DA - 2005-11-29 KW - Polymerbasierte Nanokomposite PY - 2005 SN - 3-18-091920-5 N1 - Serientitel: VDI-Berichte – Series title: VDI-Berichte IS - 1920 SP - 263 EP - 267 PB - VDI-Verl. CY - Düsseldorf AN - OPUS4-11589 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 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 - TY - CONF A1 - Robertson, Daniela A1 - Böhning, Martin A1 - Schröder, Hartmut A1 - Brummermann, K. A1 - Kaudinya, I. A1 - Saathoff, F. T1 - Möglichkeiten der Abschätzung der Langzeitbeständigkeit von Kunststoffdichtungsbahnen (KDB) auf Polyolefinbasis für den Tunnelbau N2 - Im Rahmen eines von der Bundesanstalt für Straßenwesen (BASt) initiierten Forschungsvorhabens (15.449/2007/ERB: „Prüfverfahren zur Beurteilung der Lebensdauer von Kunststoffdichtungsbahnen für Straßentunnel“) wurden anhand von Untersuchungen an Kunststoffdichtungsbahnen (KDB) auf Basis von Polyolefinwerkstoffen die Möglichkeiten der Beurteilung der oxidativen Langzeitbeständigkeit sondiert. Im Mittelpunkt stand die Erprobung des Autoklaventests in Anlehnung an DIN EN ISO 13438 (Methode C1/C2) an ausgewählten, für den Tunnelbau repräsentativen marktüblichen KDB-Produkten. Die Untersuchungen im Autoklaven bei erhöhten Temperaturen (60 °C, 70 °C und 80 °C) und Sauerstoffdrücken (11, 21 und 51 bar) wurden durch vergleichende Versuche im Wärmeschrank (Ofen) bei erhöhter Temperatur (85 °C) in Anlehnung an DIN EN 14575 ergänzt. Die KDBProdukte wurden außerdem einer eingehenden Materialcharakterisierung (Zugprüfung, DMA, DSC) unterzogen. Weiterhin wurden Bauwerksdaten recherchiert und auf ihre Nutzbarkeit zur Bewertung und Prüfbarkeit der Langzeitbeständigkeit von KDB in Tunneln betrachtet. Ziel war auch, die Anwendbarkeit des bisher vorgeschlagenen Extrapolationsmodells zur Auswertung der Ergebnisse von Autoklaventests an im Tunnelbau marktüblichen Produkten für Nutzungsdauern über 25 Jahre zu überprüfen und zur Entwicklung eines geeigneten Prüfverfahrens beizutragen. Der Beitrag geht auf Ergebnisse des Vorhabens ein und zeigt erste Schlussfolgerungen und weiteren Untersuchungsbedarf auf. Die Ergebnisse werden in den „Empfehlungen zu Dichtungssystemen im Tunnelbau EAG-EDT“ des Arbeitskreises 5.1 „Kunststoffe in der Geotechnik und im Wasserbau“ berücksichtigt, deren 2. Auflage in Vorbereitung ist. Aspekte des thermischen Verhaltens der eingesetzten Werkstoffe sowie mögliche Anpassungen der Prüfrandbedingungen für die Autoklaventests werden ergänzt und Hinweise zur Interpretation von Prüfergebnissen gegeben. Außerdem wurden inzwischen ausgehend von den Ergebnissen des Forschungsvorhabens erste Autoklaven-Ringversuche in drei Prüfinstitutionen initiiert. T2 - 12. Informations- und Vortragstagung über "Kunststoffe in der Geotechnik" CY - Munich, Germany DA - 03.03.2011 KW - Kunststoffdichtungsbahnen auf Polyolefinbasis KW - Oxidative Langzeitbeständigkeit KW - Autoklaventest - beschleunigte Alterung KW - DSC KW - DMA PY - 2011 SN - 978-3-940476-26-5 IS - Geotechnik Sonderheft 2011 SP - 35 EP - 42 AN - OPUS4-24399 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Goering, Harald A1 - Fritz, Andreas A1 - Brzezinka, Klaus-Werner A1 - Turky, Gamal A1 - Schönhals, Andreas A1 - Schartel, Bernhard T1 - Dielectric Study of Molecular Mobility in Poly(propylene-graft-maleic anhydride)/Clay Nanocomposites N2 - Polymer/clay nanocomposite materials based on poly(propylene-graft-maleic anhydride) (PPgMAH) and two different organophilic modified clays were investigated by dielectric relaxation spectroscopy (DRS). In contrast to ungrafted polypropylene (PP), PPgMAH shows a dielectrically active relaxation process which can be assigned to localized fluctuations of the polar maleic anhydride groups. Its relaxation rate exhibits an unusual temperature dependence, which could be attributed to a redistribution of water molecules in the polymeric matrix. This is confirmed by a combination of Raman spectroscopy and thermogravimetric experiments (TGA) with real-time dielectric measurements under controlled atmospheres. In the nanocomposites this relaxation process is shifted to higher frequencies up to 3 orders of magnitude compared to the unfilled polymer. This indicates a significantly enhanced molecular mobility in the interfacial regions. In the nanocomposite materials a separate high-temperature process due to Maxwell-Wagner-Sillars (MWS) polarization was observed. The time constant of this MWS process can be correlated with characteristic length scales in nanocomposites and therefore provides additional information on dispersion and delamination/exfoliation of clay platelets in these materials. These properties also influence the diffusivity of the water molecules as revealed by real-time dielectric investigations. KW - Polymer clay nanocomposites KW - Molecular mobility KW - Dielectric relaxation spectroscopy PY - 2005 DO - https://doi.org/10.1021/ma048315c SN - 0024-9297 SN - 1520-5835 VL - 38 IS - 7 SP - 2764 EP - 2774 PB - American Chemical Society CY - Washington, DC AN - OPUS4-7281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Tidjani, Adams A1 - Wald, Oliver A1 - Brzezinka, Klaus-Werner A1 - Turky, Gamal A1 - Goering, Harald A1 - Schartel, Bernhard A1 - Schönhals, Andreas T1 - Dielectric and gas transport properties of polypropylene-clay nanocomposites T2 - Frühjahrstagung des Arbeitskreises Festkörperphysik bei der DPG CY - Regensburg, Germany DA - 2002-03-11 PY - 2002 SN - 0420-0195 SN - 0372-5448 SN - 0343-9216 IS - CPP 5.4 SP - 425 CY - Bad Honnef AN - OPUS4-2036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas transport and molecular mobility in polymer/POSS nanocomposites T2 - Euromembrane 2006 CY - Taormina, Italy DA - 2006-09-24 PY - 2006 AN - OPUS4-11214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Investigation of swollen polymer/gas-systems: atomistic packing models based on experimental properties T2 - Frühjahrstagung der Deutschen Physikalischen Ges. / AKF Condensed Matter CY - Dresden, Germany DA - 2006-03-26 PY - 2006 AN - OPUS4-11316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas Transport and Molecular Mobility in Polymer Based Nanocomposite Systems T2 - 1st International Conference on Advanced Materials and their application, National Research Centre, Physics Division CY - Cairo, Egypt DA - 2005-12-12 PY - 2005 AN - OPUS4-10976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Small Molecules in Polymers and Polymer based Nanocomposites - Molecular Probes for Material Characterization and Design T2 - Polydays 2004 (Berliner Polymerentage); Universität Potsdam, Campus "Am Neuen Palais" CY - Potsdam, Germany DA - 2004-10-04 PY - 2004 AN - OPUS4-7297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Goering, Harald T1 - Preparation and Characterisation of Nanoscaled Nanostructured Materials T2 - Nanofair 2004 CY - Karlsruhe, Germany DA - 2004-11-22 PY - 2004 AN - OPUS4-7296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin A1 - Robertson, Daniela A1 - Schröder, Hartmut T1 - Autoclave testing: a new approach for the evaluation of oxidative long-term resistance of geosynthetics N2 - Oxidative long time resistance is essential for many polyolefin based products, especially if repair or exchange is not possible as encountered in many building and geotechnical applications. Current regulations and recommendations for geosynthetics cover mainly the needs of a maximum lifetime of 25 years, though many applications require longer lifetimes up to 100 years and more. Reliable testing of the long time oxidation resistance is complicated by the complex interplay of physicochemical processes and reactions in combination with the need of relatively short testing durations, usually not exceeding 12 months. Thus for conventional atmospheric oven testing, the use of temperatures higher than 100 °C is inevitable, making conclusive Arrhenius extrapolations often questionable. Practical assessments of oxidative durability consist of exposures under accelerated ageing conditions with subsequent characterization of exposed material samples with respect to their residual stabilization and/or their mechanical properties. The autoclave test combines exposures at elevated temperatures with higher oxygen pressures and is performed with material samples immersed in a well defined aqueous medium representing critical environments in geosynthetic applications and including extraction of additives. Under these conditions meaningful results can be obtained within reasonable testing durations at only moderately elevated temperatures up to 80 °C. Application of different physicochemical methods, such as tensile testing, OIT /HP-OIT and analysis of residual antioxidant content (ICOT), in order to determine the time dependent degradation behaviour, reveal valuable information about mechanisms and effectiveness of the used antioxidants. Corresponding results for exposures at different temperatures and oxygen pressures are the basis for a 3D-extrapolation in order to estimate the expected service life. Different empirical models are presented and discussed with respect to their practical impact. T2 - EuroGeo4, 4th European Geosynthetics Conference CY - Edinburgh, UK DA - 2008-09-07 KW - Ageing KW - Degradation KW - Geotextiles KW - Polyolefin KW - Polypropylene KW - Oxidative resistance KW - Lifetime prediction PY - 2008 IS - Paper 143 SP - 1 EP - 8 AN - OPUS4-18424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuchel, M. A1 - Hölck, Ole A1 - Böhning, Martin A1 - Siegert, R. A1 - Hofmann, D. ED - Qi, Y. ED - H.E. Fang, ED - N. Reynolds, ED - Liu, Z.-K. T1 - Knowledge-based approach to gas sorption in glassy polymers by combining experimental and molecular simulation techniques N2 - We present a method which allows to calculate gas sorption in complex polymers where, as slow processes, gas induced plasticization and volume dilation are important factors. Since the relaxational swelling of the polymer matrix that is observed at elevated gas concentrations takes hours or days, the swelling process is orders of magnitudes too slow to simulate the respective molecular dynamics in reasonable time and effort. To address this apparent incompatibility of experiment and simulation, we use single representative reference states from experiment and construct atomistic packing models according to these specifications. Gas sorption of CO2 and CH4 was successfully calculated on polysulfone, a 6FDA-polyimide, and a polymer of intrinsic microporosity, PIM-1, at 308 K and pressures up to 50 bar. T2 - MRS Fall Meeting 2008 - Symposium W - Computational Materials Design via Multiscale Modeling CY - Boston, MA, USA DA - 2008-12-01 KW - Gas sorption KW - Molecular modelling KW - Simulation KW - Glassy polymers PY - 2009 DO - https://doi.org/10.1557/PROC-1130-W06-10 VL - 1130 SP - W06 EP - W10 AN - OPUS4-19106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas sorption in glassy polymers - Comparative characterization using experimental and molecular modeling techniques T2 - EUROMEMBRANE 2009 Conference CY - Montpellier, France DA - 2009-09-06 PY - 2009 AN - OPUS4-20018 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Hölck, Ole A1 - Heuchel, M. A1 - Hofmann, D. T1 - Characterization of gas sorption in glassy polymers combining experimental and molecular modeling techniques KW - Glassy Polymers KW - Gas Sorption KW - Molecular Modelling KW - Diffusion PY - 2008 SN - 0743-0515 VL - 98 SP - 875 EP - 876 PB - Division of Polymeric Materials Science and Engineering, American Chemical Society CY - Washington, DC AN - OPUS4-17485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Autoclave testing - a new approach for the evaluation of oxidative long-term resistance of geosynthetics T2 - 4th European Geosynthetics Conference CY - Edinburgh, Scotland DA - 2008-09-07 PY - 2008 AN - OPUS4-18295 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas transport in glassy polymers and PNCs - experiment, analysis, modeling of diffusion, sorption and dilation T2 - Workshop: Polymers, University of Zagreb, Faculty of Mechanical Engineering and Naval Architecture, Laboratory for Non-Metals CY - Zagreb, Croatia DA - 2012-05-23 PY - 2012 AN - OPUS4-25969 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Gas transport in glassy polymers and PNCs - experiment, analysis, modeling of diffusion, sorption and dilation T2 - Workshop: Nanostructured and Nanocomposite Membranes for Gas und Vapour Separation CY - Cetraro, Italy DA - 2012-05-15 PY - 2012 AN - OPUS4-26631 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Correlation of gas diffusivity and local chain mobility in polycarbonate/POSS nanocomposites as determined by broadband dielectric relaxation spectroscopy T2 - Euromembrane 2012 CY - London, England DA - 2012-09-23 PY - 2012 AN - OPUS4-26629 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böhning, Martin T1 - Kinetic analysis of gas sorption and gas induced dilation and relaxation behaviour of PIM-1 compared to other glassy polymers T2 - Euromembrane 2012 CY - London, England DA - 2012-09-23 PY - 2012 AN - OPUS4-26630 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Wachtendorf, Volker A1 - Krafft, Bernd A1 - Morys, Michael A1 - Böhning, Martin A1 - Rybak, Thomas T1 - Multilayer graphene rubber nanocomposites N2 - Multilayer Graphene (MLG), a nanoparticle with a specific surface of BET = 250 m²/g and thus made of only approximately 10 graphene sheets, is proposed as a nanofiller for rubbers. When homogenously dispersed, it works at low loadings enabling the replacement of carbon black (CB), increase in efficiency, or reduction in filler concentration. Actually the appropriate preparation yielded nanocomposites in which just 3 phr are sufficient to significantly improve the rheological, curing and mechanical properties of different rubbers, as shown for Chlorine-Isobutylene-Isoprene Rubber (CIIR), Nitrile-Butadiene Rubber (NBR), Natural Rubber (NR), and Styrene-Butadiene Rubber (SBR). A mere 3 phr of MLG tripled the Young’s modulus of CIIR, an effect equivalent to 20 phr of carbon black. Similar equivalents are observed for MLG/CB mixtures. MLG reduces gas permeability, increases thermal and electrical conductivities, and retards fire behavior. The later shown by the reduction in heat release rate in the cone calorimeter. The higher the nanofiller concentration is (3 phr, 5 phr, and 10 phr was investigated), the greater the improvement in the properties of the nanocomposites. Moreover, the MLG nanocomposites improve stability of mechanical properties against weathering. An increase in UV-absorption as well as a pronounced radical scavenging are proposed and were proved experimentally. To sum up, MLG is interesting as a multifunctional nanofiller and seems to be quite ready for rubber development. T2 - TOP 2016, VIII International Conference on “Times of Polymers and Composites” CY - Naples, Italy DA - 19.06.2016 KW - Graphene KW - Nanocomposite KW - Rubber PY - 2016 SN - 978-0-7354-1390-0 DO - https://doi.org/10.1063/1.4949621 SN - 0094-243X SN - 1551-7616 VL - 1736 SP - 020046, 1 EP - 4 PB - AIP AN - OPUS4-36864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Ding, Yi A1 - Harrison, W.J. A1 - Budd, P.M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility of the high performance membrane polymer PIM-1 as investigated by dielectric spectroscopy N2 - The increasing demand for energy efficient separation processes fosters the development of new high performance polymers as selective separation layers for membranes. PIM-1 is the archetypal representative of the class of polymers of intrinsic microporosity (PIM) which are considered most promising in this sector, especially for gas separations. Since their introduction, PIMs stimulated a vast amount of research in this field and meanwhile evolved to the state of the art in membrane technology for gas separation. The major obstacle for extending the practical membrane application is their strong tendency to physical aging. For the first time, investigations by broadband dielectric spectroscopy (BDS) addressing molecular dynamics and conductivity in PIM 1 are presented. As chain packing during film formation from the casting solution and physical aging are key factors determining the separation performance of PIMs as membrane materials, characterization of the molecular mobility in such materials as revealed by BDS will provide valuable information for further development and optimization. KW - PIM-1 KW - BDS broadband dielectric spectroscopy KW - Relaxation KW - Membrane PY - 2016 DO - https://doi.org/10.1021/acsmacrolett.6b00209 SN - 2161-1653 VL - 5 IS - 4 SP - 528 EP - 532 PB - ACS American Chemical Society CY - Washington, DC, USA AN - OPUS4-35798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konnertz, Nora A1 - Böhning, Martin A1 - Schönhals, Andreas A1 - Ding, Yi T1 - Molecular mobility and gas transport properties of PIM-1 and nano composites based on PIM-1 and phenethylPOSS N2 - Polymers with intrinsic microporosity are of highly interest in the field of gas separation membranes. Especially the first synthesized PIM-1 shows extraordinary permeabilities and selectivities. Unfortunately, PIM-1 tends to physical aging and loses its good properties. Physical aging is related to the molecular mobility of PIM-1 which was here investigated by broadband dielectric spectroscopy (BDS). Besides the studies on pure PIM-1 a polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) was used as nanofiller (0 - 40 wt-%) in the PIM-1 matrix to improve the gas transport properties and prevent physical aging. The molecular mobility of the solution casted nano composite films was analyzed by BDS as well. Furthermore, gas transport properties were determined with the time lag method (0 - 20 bar) in a temperature range of 35°C to 65°C with N2, O2, CH4 and CO2. T2 - 80. Jahrestagung der DPG und DPG-Frühjahrstagung CY - Regensburg, Germany DA - 06.03.2016 KW - PIM-1 PY - 2016 AN - OPUS4-35541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niebergall, Ute A1 - Zanotto, M. A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Impact of biodiesel sorption on tensile properties of PE-HD for container applications N2 - In previous papers, we investigated the influence of biodiesel or diesel on mechanical properties of a high-density polyethylene (PE-HD) for tank applications using Charpy impact tests and dynamicmechanical analysis (DMA). In this work, covering two more PE-HD materials, we extend our study to addressing the tensile properties, especially changes of Young's modulus, after immersion in biodiesel or diesel at 60 °C. As we cover sorption and desorption behavior, during desorption, i.e. storage at 60 °C in a circulating air oven, ageing or degradation phenomena were also observed and characterized in some detail using spectral reflectance measurements and FT-IR spectroscopy. The results obtained here support the concept of co-oxidation, i.e. the faster oxidation of the PE-HD matrix if the samples were previously saturated with biodiesel, itself easily oxidizable. KW - polyethylene KW - biodiesel KW - biofuels KW - sorption KW - plasticization KW - degradation PY - 2016 DO - https://doi.org/10.1016/j.polymertesting.2016.01.025 SN - 0142-9418 VL - 50 SP - 315 EP - 324 PB - Elsevier AN - OPUS4-35369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agroui, K. A1 - Collins, G. A1 - Oreski, G. A1 - Böhning, Martin A1 - Hadj Arab, A. A1 - Ouadjaout, D. T1 - Effect of crosslinking on EVA-based encapsulant properties during photovoltaic module fabrication process N2 - The key objective of this work is to create a comprehensive comparison between experimental analysis methods for detecting crosslinking reaction in EVA encapsulant material during PV module fabrication process. Several analytical methods, spanning from classical gel content extraction measurements over different thermo-analytic and mechanical approaches to spectroscopic analysis as Thermally Stimulated Current (TSC), have been investigated as to their ability to reveal the crosslinking state of ethylene vinyl acetate (EVA). The basic results show that TSC complements perfectly other thermal analysis methods like as Differential Scanning Calorimetry (DSC), Dynamic Mechanical Thermal Analysis (DMTA) to determine fundamental properties of EVA such as molecular mobility characteristics and also to monitor the crosslinking reaction. Exothermic peak as revealed by DSC analysis can be used to estimate the crosslinking rate of EVA during PV module encapsulation process as fast quality control test. ------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------ L'objectif principal de ce travail est de permettre une meilleure compréhension entre les différentes techniques analyses expérimentales pour détecter la réaction de réticulation au niveau de l’encapsulant Ethylène-Vinyle Acétate (EVA), durant le process de fabrication d'un module PV. Plusieurs méthodes d'analyse, allant du test classique d'extraction du taux de gel aux différentes techniques d'analyses thermomécaniques ainsi que les techniques d'analyse de spectroscopie comme le courant stimulé thermiquement (TSC), ont été étudiés pour permettre de révéler le phénomène de la réaction de réticulation de l'encapsulant l'EVA. Les résultats de base montrent que la TSC complète parfaitement d'autres méthodes d'analyses thermiques comme la calorimétrie différentielle à balayage (DSC), l'analyse mécanique dynamique (DMTA) pour déterminer les propriétés fondamentales de l'EVA. Ces techniques permettent de déterminer les caractéristiques relatives à la mobilité moléculaire et aussi pour mieux mettre en évidence la réaction de réticulation. Le pic exothermique comme révélé par l'analyse par DSC, peut être utilisé pour estimer le taux de réticulation de l'EVA au cours du process d'encapsulation du module PV comme un test rapide de contrôle de qualité. KW - EVA KW - Photovoltaic module KW - Crosslinking process KW - Thermal properties KW - Mechanical properties PY - 2015 SN - 1112-2242 VL - 18 IS - 2 SP - 303 EP - 314 AN - OPUS4-34994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Yin, Huajie A1 - Lohstroh, W. A1 - Harrison, W. A1 - Budd, P.M. A1 - Pauw, Brian Richard A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Anomalies in the low frequency vibrational density of states for a polymer with intrinsic microporosity - the Boson peak of PIM-1 N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering. KW - Polymers KW - Boson peak KW - Neutron scattering KW - Physical aging KW - Polymer of intrinsic microporosity PY - 2018 DO - https://doi.org/10.1039/C7CP07141H SN - 1463-9076 SN - 1463-9084 VL - 20 IS - 3 SP - 1355 EP - 1363 PB - The Royal Society of Chemistry AN - OPUS4-43808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -