TY - JOUR A1 - Cooper, R. A1 - Bruno, Giovanni A1 - Shyam, A. A1 - Watkins, T. A1 - Pandey, A. A1 - Wheeler, M. T1 - Effect of microcracking on the uniaxial tensile response of beta-eucryptite ceramics: Experiments and constitutive model N2 - A constitutive model for the nonlinear or “pseudoplastic” mechanical behavior in a linear-elastic solid with thermally induced microcracks is developed and applied to experimental results. The model is termed strain dependent microcrack density approximation (SDMDA) and is an extension of the modified differential scheme that describes the slope of the stress-strain curves of microcracked solids. SDMDA allows a continuous variation in the microcrack density with tensile loading. Experimental uniaxial tensile response of β-eucryptite glass and ceramics with controlled levels of microcracking is reported. It is demonstrated that SDMDA can well describe the extent of non-linearity in the experimental uniaxial tensile response of β-eucryptite with varying levels of microcracking. The advantages of the SDMDA are discussed in regard to tensile loading. KW - Microcracking KW - β-eucryptite KW - Young's modulus KW - Modeling KW - Tensile behavior PY - 2017 DO - https://doi.org/10.1016/j.actamat.2017.06.033 SN - 1359-6454 SN - 1873-2453 VL - 135 SP - 361 EP - 371 PB - Elsevier Ltd. AN - OPUS4-40859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fedelich, Bernard A1 - Kühn, Hans-Joachim A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Experimental and analytical investigation of the TMF-HCF lifetime behavior of two cast iron alloys N2 - The combined loading Thermomechanical Fatigue (TMF) with High Cycle Fatigue (HCF) has been experimentally investigated for two cast iron alloys. Both alloys contain globular graphite nodules but the first one has a ferritic structure while the second one has an austenitic crystal structure. In particular, the influences of the HCF frequency, of the HCF loading amplitude and of the location of the superposed HCF cycles have been investigated. It was observed that the HCF frequency has a limited impact on the fatigue life. On the other side, the HCF-strain amplitude has a highly non-linear influence on the fatigue life. The experimental results can be understood in terms of a fracture mechanics based damage mechanism: Cracks quickly initiate due to the TMF loading and the growth of the cracks up to a few mm controls the fatigue life. If HCF-loading cycles are superposed, cyclic crack propagation dramatically accelerates after a threshold has been reached. This threshold is regarded as controlling the fatigue life reduction. The previous ideas have been expressed in a model that can be very simply applied to estimate the fatigue life reduction ratio due to the superposed HCF cycles. It only contains two adjustable parameters and can be combined with any TMF life assessment model. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Thermomechanical Fatigue (TMF) KW - High Cycle Fatigue (HCF) KW - Cast iron KW - Fatigue assessment PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2016.11.013 SN - 0142-1123 SN - 1879-3452 VL - 99 IS - 2 (Special issue: Recent developments in thermo-mechanical fatigue) SP - 266 EP - 278 PB - Elsevier CY - Oxford AN - OPUS4-39810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Pourmand, P. A1 - Wolff, Dietmar A1 - Gedde, U.W. T1 - Influence of ageing on sealability of elastomeric O-rings N2 - At BAM, which is the federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes the assessment of the service lifetime of elastomeric seals that are part of the container lid system with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) up to 1.5 years. In order to assess sealability, O-rings are aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings are aged as well. Further methods characterising seal performance are compression stress relaxation (CSR) reflecting the loss of sealing force of a compressed seal over time, and compression set (CS) which represents the recovery behaviour of a seal after release from compression. Additionally, hardness is measured for information about the change of mechanical properties. The experimental results indicate that while hardness, CSR and CS show considerable degradation effects, the leakage rate stays relatively constant or even decreases until shrinkage combined with the loss of resilience of the aged seal leads to leakage. This demonstrates that static leakage rate, which is the only available direct seal performance criterion, has only limited sensitivity towards the degradation of the seal material. CS data is extrapolated using time-temperature shifts and Arrhenius graphs. An exemplary CS of 50 % would be reached after approx. 1.2, 17 and 29 years at 60 °C for HNBR, EPDM and FKM respectively. T2 - PolymerTec 2016 CY - Merseburg, Germany DA - 15.06.2016 KW - Compression KW - Leakage KW - Degradation KW - Rubber KW - Lifetime PY - 2017 DO - https://doi.org/10.1002/masy.201600157 SN - 1022-1360 SN - 1521-3900 VL - 373 IS - 1 SP - UNSP 1600157, 1 EP - 10 PB - WILEY-V C H VERLAG GMBH CY - Weinheim AN - OPUS4-40958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Palasse, L. A1 - Häusler, Ines A1 - Dirscherl, K. A1 - Oswald, F. A1 - Narbey, S. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - Characterization of the inner structure of porous TiO2 nanoparticle films in dye sensitive solar cells (DSSC) by focused ion beam (FIB) tomography and transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) N2 - A combined methodical approach is tested for the first time with respect to the characterization of the inner structure of porous TiO2 layers infiltrated with ruthenium molecular sensitizer as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area ‘offered’ by the pore Network to the dye. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles (NPs) on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). While the first method results in the visualization of the 3D pore network within the TiO2 layer, the second one can be successfully applied to analyze the crystal orientation of grains (i.e. NPs in our case) in nanometer resolution. Moreover, size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - Transmission Kikuchi diffraction KW - Focused ion beam tomography KW - Titanium dioxide KW - Nanoparticles KW - Porosity KW - Particle size KW - DSSC PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.06.030 SN - 1044-5803 SN - 1873-4189 VL - 131 SP - 39 EP - 48 PB - Elsevier AN - OPUS4-40875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Chatzigiannakis, E. A1 - Beckmann, Jörg A1 - Wachtendorf, Volker A1 - von der Ehe, Kerstin A1 - Braun, Ulrike A1 - Jaunich, Matthias A1 - Schade, U. A1 - Wolff, Dietmar T1 - Discoloration Effects of High-Dose gamma-Irradiation and Long-Term Thermal Aging of (U) HMW-PE N2 - Two polyethylene types with ultra-high (UHMWPE) and high molecular weight (HMW-PE) used as neutron radiation shielding materials in casks for radioactive waste were irradiated with doses up to 600 kGy using a 60Co gammasource. Subsequently, thermal aging at 125∘C was applied for up to one year. Degradation effects in the materials were characterized using colorimetry, UV-Visspectroscopy, IR spectroscopy, and DSC. Both materials exhibited a yellowing upon irradiation.The discoloration of UHMW-PE disappeared again after thermal aging.Therefore, the yellowing is assumed to originate fromannealable color centers in the formof free radicals that are trapped in the crystalline regions of the polymer and recombine at elevated temperatures. For the antioxidantcontaining HMWPE, yellowing was observed after both irradiation and thermal aging. The color change was correlated mainly to decomposition products of the antioxidant in addition to trapped radicals as in UHMW-PE. Additionally, black spots appeared after thermal aging of HMW-PE. KW - Irradiation KW - UHMWPE KW - Colour center KW - Yellowness index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-423992 DO - https://doi.org/10.1155/2017/1362491 SN - 1687-9422 VL - 2017 IS - Article ID 1362491 SP - 1 EP - 10 PB - Hindawi AN - OPUS4-42399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Cabeza, Sandra A1 - Artzt, Katia A1 - Haubrich, J. A1 - Klaus, M. A1 - Genzel, Ch. A1 - Requena, G. A1 - Bruno, Giovanni T1 - An Assessment of Subsurface Residual Stress Analysis in SLM Ti-6Al-4V N2 - Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment. KW - Selective laser melting KW - Additive manufacturing KW - Heat treatment KW - Ti-6Al-4V KW - Synchrotron X-ray diffraction KW - Residual stress PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395759 DO - https://doi.org/10.3390/ma10040348 SN - 1996-1944 VL - 10 IS - 4 SP - Article 348, 1 EP - 14 AN - OPUS4-39575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obaton, A-F. A1 - Fain, J. A1 - Djemaï, M. A1 - Meinel, Dietmar A1 - Léonard, Fabien A1 - Mahé, E. A1 - Lécuelle, B. A1 - Fouchet, J-J. A1 - Bruno, Giovanni T1 - In vivo XCT bone characterization of lattice structured implants fabricated by additive manufacturing N2 - Several cylindrical specimens and dental implants, presenting diagonal lattice structures with different cell sizes (600, 900 and 1200 µm) were additively manufactured by selective laser melting process. Then they were implanted for two months in a sheep. After removal, they were studied by Archimedes’ method as well as X-ray computed tomography in order to assess the penetration of bone into the lattice. We observed that the additive manufactured parts were geometrically conform to the theoretical specifications. However, several particles were left adhering to the surface of the lattice, thereby partly or entirely obstructing the cells. Nevertheless, bone penetration was clearly visible. We conclude that the 900 µm lattice cell size is more favourable to bone penetration than the 1200 µm lattice cell size, as the bone penetration is 84 % for 900 µm against 54 % for 1200 µm cell structures. The lower bone penetration value for the 1200 µm lattice cell could possibly be attributed to the short residence time in the sheep. Our results lead to the conclusion that lattice implants additively manufactured by selective laser melting enable better bone integration. KW - Biomedical engineering KW - Dentistry KW - Medical imaging KW - X-ray computer tomography PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418648 DO - https://doi.org/10.1016/j.heliyon.2017.e00374 SN - 2405-8440 IS - 3 SP - Article e00374, 1 EP - 21 PB - Elsevier Limited CY - 125 London Wall London, EC2Y 5AS United Kingdom AN - OPUS4-41864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Häusler, Ines A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Palasse, L. A1 - Dirscherl, K. T1 - Characterization of porous, TiO2 nanoparticle films using on-axis TKD in SEM – a new nano-analysis tool for a large-scale application N2 - A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - TiO2 KW - TKD KW - Particle size distribution KW - Nanoparticles KW - Porous film PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/8A8B29335A2F4D0CB6922F6F5A19C5DC/S1431927617003397a.pdf/characterization_of_porous_tio2_nanoparticle_films_using_onaxis_tkd_in_sem_a_new_nanoanalysis_tool_for_a_largescale_application.pdf DO - https://doi.org/10.1017/S1431927617003397 VL - 23 IS - S1 (July) SP - 542 EP - 543 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rehmer, Birgit A1 - Skrotzki, Birgit A1 - Glaubitz, Steffen T1 - Influence of casting skin on fatigue lifetime of ferritic ductile cast iron N2 - The fatigue behaviour of cast iron is usually investigated on machined specimens. Components of cast iron, however, have a casting skin; therefore the investigation of the influence of the casting skin on the lifetime is of interest. To study this influence isothermal fatigue tests were carried out on heat-resisting spheroidal graphite cast iron EN GJS SiMo 4.05 in 4–point-bending set-up at 400 °C. Specimens with and without casting skin were investigated comparatively. The number of cycles to failure was significantly lower for specimens with casting skin. Metallographic investigations underline the reduction of lifetime caused by casting skin. KW - Cast iron KW - Casting skin KW - Fatigue KW - Lifetime PY - 2017 SN - 0025-5300 VL - 59 IS - 1 SP - 5 EP - 10 PB - Carl Hanser Verlag CY - München AN - OPUS4-38929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Lyamkin, V. A1 - Bruno, Giovanni A1 - Pittner, Andreas A1 - Wimpory, Robert A1 - Boin, M. A1 - Kreutzbruck, Marc T1 - Residual stress characterization of steel TIG welds by neutron diffraction and by residual magnetic stray field mappings N2 - The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth. KW - GMR KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - TIG-welding PY - 2017 DO - https://doi.org/10.1016/j.jmmm.2016.11.102 SN - 0304-8853 SN - 1873-4766 VL - 426 SP - 580 EP - 587 PB - Elsevier CY - Amsterdam AN - OPUS4-38678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabeza, Sandra A1 - Garces, G. A1 - Adeva, Paloma A1 - Kabra, S. A1 - Gan, W. T1 - Effect of Extrusion Temperature on the Plastic Deformation of an Mg-Y-Zn Alloy Containing LPSO Phase Using In Situ Neutron Diffraction N2 - The evolution of the internal strains during in situ tension and compression tests has been measured in an MgY2Zn1 alloy containing long-period stacking ordered (LPSO) phase using neutron diffraction. The alloy was extruded at two different temperatures to study the influence of the microstructure and texture of the magnesium and the LPSO phases on the deformation mechanisms. The alloy extruded at 623 K (350 °C) exhibits a strong fiber texture with the basal plane parallel to the extrusion direction due to the presence of areas of coarse non-recrystallised grains. However, at 723 K (450 °C), the magnesium phase is fully recrystallised with grains randomly oriented. On the other hand, at the two extrusion temperatures, the LPSO phase orients their basal plane parallel to the extrusion direction. Yield stress is always slightly higher in compression than in tension. Independently on the stress sign and the extrusion temperature, the beginning of plasticity is controlled by the activation of the basal slip system in the dynamic recrystallized grains. Therefore, the elongated fiber-shaped LPSO phase which behaves as the reinforcement in a metal matrix composite is responsible for this tension–compression asymmetry. KW - Mg-Y-Zn Alloy KW - LPSO Phase KW - Neutron Diffraction PY - 2017 DO - https://doi.org/10.1007/s11661-017-4284-6 VL - 48A IS - 11 SP - 5332 EP - 5343 PB - Spinger AN - OPUS4-42935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klingelhöffer, Hellmuth A1 - Affeldt, E. E. A1 - Bache, M. A1 - Bartsch, M. A1 - Beck, T. A1 - Christ, H. J. A1 - Fedelich, Bernard A1 - Hähner, P. A1 - Holdsworth, S. R. A1 - Lang, K.-H. A1 - McGaw, M. A1 - Olbricht, Jürgen A1 - Remy, L. A1 - Skrotzki, Birgit A1 - Stekovich, S. T1 - Editorial - Special issue: Recent developments in thermo-mechanical fatigue N2 - Components in the Aerospace, Power and Automotive engineering sectors are frequently subjected to cyclic stresses induced by thermal fluctuations and mechanical loads. For the design of such components, reliable material property data are required which need to be acquired using well accepted and reproducible test procedures for thermo-mechanical fatigue (TMF) loading. There is limited availability of proven TMF data indicating there is need for further research and testing. The TMF behaviour of materials is often desired to be simulated in models which describe the cyclic stress-strain behaviour, the fatigue life and the cyclic crack growth behaviour. There is a continuous need for the development and amendment of such models. Models can be validated by using materials in industrial applications which are subjected to TMF loading. The 3rd Workshop on Thermo-Mechanical Fatigue was held on 27–29 April 2016 at BAM, Berlin, Germany. The workshop was attended by 90 attendees coming from 17 countries in the world. 38 presentations including five poster presentations were held. The following topics were covered by the workshop: – TMF of materials coated with Thermal Barrier Coatings. – Thermal Gradient Mechanical Fatigue. – TMF crack growth. – TMF + High Cycle Fatigue. – TMF Modelling and Lifetime Prediction. – TMF Properties of steels, cast iron, Al-, Mg- and Ni-alloys – Advanced TMF Testing Techniques. – Industrial Applications. A panel discussion was held regarding the present state of TMF testing standards (ISO and ASTM) and their potential for improvement. The discussion and contributions were summarized and forwarded to the standard committees. The 3rd TMF-Workshop ensured the continuation of international exchange of knowledge providing a forum to present and discuss all recent developments in the field of thermo-mechanical fatigue. The current special issue publishes eleven selected papers of the 3rd TMF-Workshop 2016. The papers were peer reviewed by a number of experts in the Thermo-Mechanical Fatigue sector. I hope you will enjoy reading papers of this special issue. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Fatigue damage KW - Thermo-mechanical fatigue KW - Fatigue life time KW - Life time prediction KW - TMF PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2017.02.002 SN - 0142-1123 VL - 99 IS - 2 SP - 215 PB - Elsevier CY - Oxford AN - OPUS4-40895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Garces, G. A1 - Requena, G. A1 - Bruno, Giovanni A1 - Sevostianov, I. T1 - Stress-induced damage evolution in cast AlSi12CuMgNi alloy with one- and two ceramic reinforcements N2 - Two composites, consisting of an as-cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 short fibres and with 7%vol. Al2O3 short fibres + 15%vol. SiC particles were studied. Synchrotron computed tomography disclosed distribution, orientation, and volume fraction of the different phases. In-situ compression tests during neutron diffraction in direction parallel to the fibres plane revealed the load partition between phases. Internal damage (fragmentation) of the Si phase and Al2O3 fibres was directly observed in CT reconstructions. Significant debonding between Al-matrix and SiC particles was also found. Finally, based on the Maxwell scheme, a micro-mechanical model was utilized for the new composite with two ceramic reinforcements; it rationalizes the experimental data, and predicts the evolution of all internal stress components in each phase. KW - Computed tomography KW - Metal matrix composite KW - Load partition KW - Neutron diffraction PY - 2017 DO - https://doi.org/10.1007/s10853-017-1182-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 17 SP - 10198 EP - 10216 PB - Springer AN - OPUS4-40572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shashev, Yury A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Osenberg, Markus A1 - Manke, Ingo A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni T1 - Optimizing the visibility of X-ray phase grating interferometry N2 - The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup. KW - Synchrotron, BAMline KW - Talbot-Lau interferometer KW - X-ray imaging KW - X-ray refraction KW - Grating interferometry KW - X-ray phase contrast PY - 2017 DO - https://doi.org/10.3139/120.111097 SN - 0025-5300 VL - 59 IS - 11-12 SP - 974 EP - 980 PB - Hanser Verlag AN - OPUS4-42955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Bruno, Giovanni T1 - Microstructure Characterization of Ceramics via 2D and 3D X-Ray Refraction Techniques N2 - 3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. KW - X-ray refraction KW - Porosity KW - Specific surface KW - Crack detection KW - Composites PY - 2017 DO - https://doi.org/10.1016/j.jeurceramsoc.2016.12.031 SN - 0955-2219 SN - 1873-619X VL - 37 IS - 5 SP - 1879 EP - 1889 PB - Elsevier CY - Amsterdam AN - OPUS4-39094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Léonard, Fabien A1 - Oesch, Tyler A1 - Meinel, Dietmar A1 - Bruno, Giovanni A1 - Rachmatulin, Natalia A1 - Fontana, Patrick A1 - Sevostianov, I. T1 - Evaluation of fiber orientation in a composite and its effect on material behavior N2 - The reinforcement of concrete with polymer fibers provides resistance to crack formation. The orientation distribution of these fibers has a significant influence on the mechanical behavior of the material. To optimize material performance, micromechanical models that are capable of making accurate predictions of the mechanical behavior of composite materials are needed. These models must be calibrated using experimental results from microstructural characterization. For the fiber orientation distribution analysis in the present study, computed tomography (CT) data were used to evaluate the properties of a fiber-reinforced cement mortar. The results have indicated that the fibers in this material have highly anisotropic orientation characteristics and that there is a clear tendency for the polymer fibers to agglomerate during mixing and casting. The incorporation of this experimental data into micromechanical models will increase the accuracy of those models for material simulation and optimization. T2 - 7th Conference on Industrial Computed Tomography (iCT 2017) CY - Leuven, Belgium DA - 07.02.2017 KW - Orientation distribution KW - Fiber-reinforced concrete KW - Computed tomography PY - 2017 UR - http://www.ndt.net/?id=20818 SN - 1435-4934 VL - 22 IS - 3 SP - 1 EP - 7 PB - NDT.net CY - Kirchwald AN - OPUS4-39338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosu, Dana-Maria A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas ED - Hertwig, Andreas ED - Hinrichs, K. ED - Beck, Uwe ED - Esser, N. T1 - Ellipsometric porosimetry on pore-controlled TiO2 layers N2 - The practical performance of surface coatings in applications like catalysis, water splitting or batteries depends critically on the coating materials’ porosity. Determining the porosity in a fast and nondestructive way is still an unsolved problem for industrial thin-films technology. As a contribution to calibrated, non-destructive, optical layer characterisation, we present a multi-method comparison study on porous TiO2 films deposited by sol-gel synthesis on Si wafers. The ellipsometric data were collected on a range of samples with different TiO2 layer thickness and different porosity values. These samples were produced by templated sol-gel synthesis resulting in layers with a well-defined pore size and pore density. The ellipsometry measurement data were analysed by means of a Bruggeman effective medium approximation (BEMA), with the aim to determine the mixture ratio of void and matrix material by a multi-sample analysis strategy. This analysis yielded porosities and layer thicknesses for all samples as well as the dielectric function for the matrix material. Following the idea of multi-method techniques in metrology, the data was referenced to imaging by electron microscopy (SEM) and to a new EPMA (electron probe microanalysis) porosity approach for thin film analysis. This work might lead to a better metrological understanding of optical porosimetry and also to better-qualified characterisation methods for nano-porous layer systems. 1. IntroductionPorous materials, especially porous thin films play an importantrole in chemical and physical technology in every case where thecontact area between two media has to be maximised. From cataly-sis to photochemistry and photovoltaics, the applications of porouslayer materials are diverse and numerous [1–6].The accurate and non-destructive characterisation of porousfilms for layered systems poses a challenge. This applies especiallyfor the key parameter of porous films, their porosity, i.e. the mix-ing ratio between the Matrix of the film (host material) and thepore volume which is empty or filled with a fluid medium (inclu-sions). This parameter influences most of the physical and chemicalproperties of a porous thin film and is therefore essential for theunderstanding as well as the optimisation of this class of materials. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsometry KW - Porous materials KW - Porosimetry KW - Multi-sample analysis KW - Thin film metrology PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.055 SN - 0169-4332 SN - 1873-5584 VL - 421 IS - Part B SP - 487 EP - 493 PB - Elsevier B.V. AN - OPUS4-42517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias T1 - Editorial: Shape memory polymers N2 - In this editorial the focus lies on the testing of shape memory materials. KW - Shape memory polymer KW - Testing PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.08.019 SN - 0142-9418 VL - 62 SP - A1 PB - Elsevier CY - Oxford AN - OPUS4-41714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Rangelov, V. T1 - In situ shrinkage measurement during pressure-assisted sintering of low temperature co-fired ceramic panels N2 - Shrinkage measurements of miniaturized low temperature co-fired ceramics (LTCC) samples under load typically lead to collapsing of the samples, which hampers the characterization of shrinkage up to full densification. In this paper, a measurement setup is presented, which allows for in situ shrinkage measurements of practical, large LTCC panels during pressure-assisted sintering in a sintering press. The shrinkage behavior of two commercial LTCC systems (GreenTape 951 and Ceramtape GC) has been measured under loads of up to 1 MPa. No crushing of the specimens was observed and reproducible characterization of shrinkage up to full densification has been performed. Based on comparisons to thermomechanical analyzer measurements in this and other studies, it was found that the in situ approach is much better suited for shrinkage characterization of LTCC under load. Reproducibility and accuracy of the method are discussed and practical as well as more academic applications are proposed. KW - Shrinkage KW - Low temperature KW - Sinter/sintering PY - 2017 DO - https://doi.org/10.1111/ijac.12634 SN - 1546-542X SN - 1744-7402 VL - 14 IS - 2 SP - 245 EP - 251 AN - OPUS4-39327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wessig, P. A1 - Schulze, T. A1 - Pfennig, A. A1 - Weidner, Steffen A1 - Prentzel, S. A1 - Schlaad, H. T1 - Thiol–ene polymerization of oligospiroketal rods N2 - The nucleophilic thiol–ene (thia-Michael) reaction between molecular rods bearing terminal thiols and bis-maleimides was investigated. The molecular rods have oligospiroketal (OSK) and oligospirothioketal (OSTK) backbones. Contrary to the expectations, cyclic oligomers were always obtained instead of linear rigid-rod polymers. Replacing the OS(T)K rods with a flexible chain yielded polymeric products, suggesting that the OS(T)K structure is responsible for the formation of cyclic products. The reason for the preferred formation of cyclic products is due to the presence of folded conformations, which have already been described for articulated rods. KW - Oligospiroketals KW - Polymerization KW - MALDI-TOF MS PY - 2017 DO - https://doi.org/10.1039/C7PY01569K SN - 1759-9954 SN - 1759-9962 VL - 8 IS - 44 SP - 6879 EP - 6885 PB - Royal Society of Chemistry AN - OPUS4-42685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -