TY - CONF A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Kuchenbecker, Petra A1 - Würth, Christian A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - Fine iron oxide nanoparticles as a candidate reference material for reliable measurement of particle size N2 - Background, Motivation and Objective Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds. Statement of Contribution/Methods Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents. Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution. Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum). Results/Discussion In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm. T2 - Nanosafe 2020 CY - Online meeting DA - 16.11.2020 KW - Reference nanomaterials KW - Imaging techniques KW - Size and size distribution KW - Reliable characterization KW - Iron oxide nanoparticles PY - 2020 AN - OPUS4-51767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von Hartrott, P. A1 - Rockenhäuser, Christian A1 - Metzger, M. A1 - Skrotzki, Birgit T1 - Assessment of EN AW-2618A for high temperature applications considering aging effects N2 - The alloy EN AW-2618A was assessed regarding its properties for high temperature applications considering aging effects. T2 - BAM TMF-Workshop 2019 CY - Berlin, Germany DA - 13.11.2019 KW - Alloy 2618A KW - Degradation KW - Coarsening KW - Transmission electron microscopy KW - Dark-field transmission electron microscopy (DFTEM) PY - 2019 AN - OPUS4-49808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Balzer, R. A1 - Kiefer, P. A1 - Reinsch, Stefan A1 - Behrens, H. A1 - Deubener, J. T1 - Subcritical crack growth in hydrous soda-lime silicate glass N2 - Glass strength and fatigue is limited by surface cracks. As subcritical crack growth (SCCG) is governed by ambient humidity, stress corrosion at the crack tip is widely accepted to be the underlying mechanism. However, as water is known to have decisive effect on glass properties and can rapidly enter the crack tip near glass region, SCCG could be affected by such water related phenomena. We tried to mimic these effects studying water dissolution and speciation, mechanical properties, and SCCG in water-bearing glasses. For this purpose, glasses up to 8 wt% water have been prepared by means of high-pressure melting of glass powder - water mixtures. As part of this effort, SCCG in dry and hydrous commercial micros¬cope slide glass (CW = 6 wt%) was studied in double cantilever beam (DCB) geometry and sub-Tg relaxation was measured by Dynamic Mechanical Analysis (DMA). For SCCG in ambient air (24% r.h.), SCCG was promoted by the presence of 6wt% bulk water with respect to the dry glass. On the other hand, stress intensity values, KI, required to cause slow crack growth (v < 10-6 ms-1) resemble literature findings for float glass of similar composition in liquid water, which might represent the maximum possible promoting effect of ambient water on SCCG. For SCCG in vacuum (10-3 mbar), dissolved bulk water causes even more pronounced effects. Most strikingly, it strongly decreases the slope of the log v(KI)-curve, which is a measure of dissipated energy during fracture. A strong increase of sub-Tg relaxation with increasing water content was confirmed by DMA. As a consequence, slow crack growth occurs at KI values as measured in the dry glass whereas fast crack growth occurs at much larger KI than that of the dry glass. Kinks and shoulders shown by the inert log v(KI)-curve indicate that bulk water does not simply affect bulk mechanical properties. T2 - 9th Otto Schott Colloquium CY - Jena, Germany DA - 09.09.2019 KW - Internal friction KW - Soda-lime silicate glass KW - Crack growth KW - Water content KW - DCB PY - 2019 AN - OPUS4-49534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Sub-critical crack growth in silicate glass N2 - Premature failure of glass under load is caused by sub-critical crack growth (SCCG) originate from microscopic flaws at the surface. While SCCG is related to the humidity of the ambient atmosphere, leading to stress corrosion phenomena at the crack tip, the detailed mechanism and the effect of different network formers are still not fully understood. For more clarity, various soda silicate glasses with a second network former were investigated by double cantilever beam technique: Na2O*Al2O3*SiO2 (NAS), Na2O*B2O3*SiO2 (NBS), Na2O*PbO*SiO2 (NPbS). Three effects on the crack growth velocity, v, versus stress intensity, KI, curves were found out. The slope in region I, which is limited by corrosion, increases in the order NAS < NBS ≲ NPbS. The velocity range of region II reflecting the transition between corrosion effected and inert crack growth (region III), varies within one order of magnitude between the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For comparison, crack growth at different humidity in commercial soda lime silicate glass (NCS) was measured. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Risswachstum KW - DCB KW - Glas PY - 2018 AN - OPUS4-45702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Deubener, J. A1 - Waurischk, Tina A1 - Balzer, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. T1 - Statistical analysis of Vickers induced subcritical crack growth in soda-lime silicate glasses N2 - Studies on Vickers induced subcritical crack growth are controversially discussed since the stresses that drive the crack growth are distributed three dimensionally within the material and cannot be retraced by available methods. Hence, empirical approaches are used to calculate mechanical material parameters such as the stress intensity factor KI. However, the results of these approaches show large deviations from those measured by standardized techniques such as double cantilever beam (DCB) or double cleavage drilled compression (DCDC). Yet, small specimen sizes and low specimen quantities can prevent the execution of DCB and DCDC measurements. Here we present an approach that is based on a statistical analysis of Vickers induced radial cracks. For this purpose more than 150 single radial cracks were analyzed. The cracks were generated in a commercial soda-lime silicate glass. The experiments were performed in a glovebox purged with dry nitrogen gas to minimize the influence of atmospheric water on crack growth. The temporally resolved evolution of the radial cracks was monitored in-situ using an inverted microscope equipped with a camera system directly below the Vickers indenter. An automated image analysis software was used to determine the crack length over time. The data show that the crack propagation and thereby the crack velocities are not uniformly but statistically distributed. These findings allow, using the statistical mean value of the distributions in combination with DCB data, a precise formulation of KI for each measured crack length. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Crack growth KW - Soda-lime silicate glass KW - Vickers PY - 2018 AN - OPUS4-45703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Deubener, J. A1 - Waurischk, Tina A1 - Balzer, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. T1 - Subcritical crack growth in water bearing soda-lime silicate glasses N2 - The presence of water in the surrounding atmosphere of a propagating crack has a major influence on the subcritical crack growth. While these external phenomena are well understood, there is still a lack of knowledge on the influence of structurally bound water on crack propagation. Thus, our recent study aims on the analysis of crack propagation in water bearing soda-lime silicate glasses with up to 8 wt.% water. The samples were synthesized in an internally heated pressure vessel at 0.5 GPa. Since this preparation route limits the sample sizes, standard test geometries allowing for the determination of stress intensity factors, such as double cantilever beam, are not feasible. Thus, radial cracks in the hydrous glasses were initiated by Vickers indentation and crack growth was simultaneously captured with a camera system. An automated image analysis algorithm was used for the analysis of the crack length of each single video frame. To minimize influences by atmospheric water, all experiments were conducted in a glovebox purged with dry N2. About 150 cracks per glass composition were analyzed to provide statistical significance of the Vickers-induced SCCG. The results show that structurally bound water has a major influence on SCCG by means of crack lengths, growth rates and time of crack initiation. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Water speciation KW - Soda-lime silicate glass KW - Crack growth KW - Vickers PY - 2018 AN - OPUS4-45704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Goedecke, Caroline A1 - Sojref, Regine T1 - Transformation of the antidiabetic drug metformin N2 - For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide. Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents. In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS. T2 - SPEA 10 CY - Almeria, Spain DA - 04.06.2018 KW - Metformin KW - Photocatalysis PY - 2018 AN - OPUS4-47030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker A1 - Kraus, David A1 - Kübler, Stefan A1 - Eisermann, René T1 - Multiaxial fatigue damage of glass fiber reinforced polymers N2 - Fiber reinforced polymers (FRPs) are a well established material in lightweight applications, e.g. in automotive, aerospace or wind energy. The FRP components are subjected to multiaxial mechanical as well as hygrothermal loads. Common operation temperatures are in the range of 213 K and 373 K (-60 °C and 100 °C) at a relative humidity of 10% to 90%. In spacecraft applications, the environmental conditions are even more extreme. However, the correlation between multiaxial mechanical loading and harsh environment conditions have to-date not been investigated in detail. The project aims to investigate the fatigue behavior of FRPs dependent on multiaxial mechanical loading, temperature, and humidity. Extensive experimental testing is performed on flat plate and cylindrical tube specimens, accompanied by numerical and analytical calculations. T2 - 24. Nationales SAMPE Symposium CY - Dresden, Germany DA - 06.02.2019 KW - Composite KW - Fatigue KW - Thermomechanics KW - Distributed fiber optic sensors PY - 2019 AN - OPUS4-47335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Welter, T. A1 - Deubener, J. A1 - Reinsch, Stefan A1 - Marzok, Ulrich A1 - Müller, Ralf T1 - Glass structures with low H2-diffusity N2 - Effective hydrogen storage capacities are prerequisite for an efficient energy provision using fuel cells. Since glass has low intrinsic hydrogen permeability, it is a promising material for hydrogen storage containers as well as hydrogen diffusion barriers. Previous studies on oxidic glasses suggest a correlation between the glass composition and hydrogen permeation that was derived mainly from silica glass. In the present study, we concentrate on the relationship between thermodynamic (i.e., configurational entropy) and topologic (i.e., free volume, network polymerization) parameters. Experimental data were gathered well below the glass transition temperature, excluding significant effects caused by structural relaxation and chemical dissolution of hydrogen. The results of seven analysed glasses on the SiO2-NaAlO2 joint showed that the hydrogen permeability in fully polymerized glasses cannot solely be derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen solubility and diffusion. Additionally, the results indicate that the configurational heat capacity ΔCp at Tg affects the hydrogen permeability of the investigated glasses. T2 - 92. Glastechnische Tagung der DGG CY - Bayreuth, Germany DA - 28.05.2018 KW - Hydrogen permeability KW - Atomic packing factor KW - Glass composition KW - Diffusion coefficient PY - 2018 AN - OPUS4-45900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grelle, Tobias A1 - Probst, Ulrich A1 - Jaunich, Matthias A1 - Skrotzki, Birgit A1 - Wolff, Dietmar T1 - Creep Investigations on Aluminum Seals for Application in Radioactive Waste Containers N2 - In Germany spent nuclear fuel (SNF) and high level radioactive waste (HLW) are stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. Being licensed for up to 40 years of interim storage the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads. T2 - International Conference on Aluminum Alloys CY - Montreal, Canada DA - 17.06.2018 KW - Metal seal KW - Creep KW - Long-term behavior PY - 2018 AN - OPUS4-45843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -