TY - JOUR A1 - Woydt, Mathias A1 - Scholz, C. A1 - Burbank, J. A1 - Spaltmann, Dirk T1 - Slip-rolling resistant steel alloys up to P0max of 3,920 MPa N2 - Downsizing (power-to-weight ratio) and higher speeds lead to a rise in Hertzian contact pressures in combination with an increase in surface or oil temperatures. Under such conditions, commonly used bearing steels, such as 100Cr6, reach their limits, creating a demand for alternative slip-rolling resistant steel alloys. The present work therefore compares the slip-rolling performance of various steel types with Maraging- and PM-type steel alloys such as e.g. CSS-42L™, ASP2012, BIMAX42+, in the Hertzian contact pressure range up to P0max of 4 GPa. Through-hardened 100Cr6H (AISI 52100), case-hardened 20MnCr5 (AISI 5120H) and nitrogen alloyed Croni-dur30 (AMS 5898) still compete in terms of slip-rolling and wear resistance and load carrying capacity, whereas Maraging- and PM-type steel alloys offer superior strength and toughness properties. KW - Steel KW - Alloy KW - Slip-rolling KW - Friction KW - Wear rate KW - Contact pressure KW - 100Cr6 KW - BIMAX42 KW - CSS-42L KW - ASP20212 PY - 2012 DO - https://doi.org/10.1016/j.wear.2021.203707 VL - 474-475 SP - 203707 PB - Elsevier B.V. AN - OPUS4-52549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallstabe, Ronald T1 - Laser-assisted surface modification of alumina and its tribological behavior N2 - High performance friction systems, e.g., dry clutches and brakes, require a good wear resistance and a friction coefficient that is nearly independent from sliding velocity and environmental conditions. Organic-based friction materials have reached their limitations regarding higher power densities. Engineering ceramics such as alumina (Al2O3) or silicon carbide (SiC) offer a great potential since remarkably higher thermal and mechanical loading is possible. However, the tribological performance of these monolithic ceramics is still insufficient. The aim of the present study was to assess the potential of a laser-assisted surface modification process in order to improve the tribological performance with regard to the application in dry friction systems. Therefore, commercially available alumina was modified using a newly developed laser-assisted preheating process and subsequent melting of the ceramic’s surface using a CO2-laser and modification by additives such as TiC, TiN, B4C, WC, ZrB2, Cr, Ni, Cu, and Ti. A systematic variation of additives and process parameters led to different multiphase microstructures. Subsequently, these were characterized using scanning electron microscopy and surface analysis methods (wavelength dispersive X-ray spectroscopy, energy dispersive X-ray spectroscopy). Finally, the tribological properties were investigated using a laboratory tribometer. The surface-modified ceramics were tested in unidirectional sliding motion against steel disks. The tribological results of the surface-modified ceramics were compared to those of monolithic Al2O3 and SiC ceramics and showed a reduced dependence of friction coefficient on sliding velocity. Moreover, the multi-phase ceramics possessed a higher wear resistance than the monolithic ones. KW - Alumina KW - Ceramics KW - Ceramic matrix composites KW - Dry sliding KW - Laser-assisted surface modification KW - Steel KW - Tribology KW - Wear resistance PY - 2012 DO - https://doi.org/10.1007/s11665-012-0215-2 SN - 1059-9495 SN - 1544-1024 SP - 1 EP - 13(?) PB - ASM international CY - Materials Park, Ohio AN - OPUS4-25842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallstabe, Ronald A1 - Klinger, Christian T1 - Cause of an implant fracture: material- or fabrication failure? N2 - Intramedullary hip screws (IMHSs) are implanted for the fixture of pertrochanteric femoral fractures (thigh bone). The present work investigates the failure of an IMHS implant after the rehabilitation period which required a revision surgery where the upper femur had to be replaced by a hip endoprosthesis. Due to litigation the corresponding failure analysis was conducted at BAM Federal Institute for Materials Research and Testing and is the subject of this article. By order of the customer failure causes due to material and fabrication failures should be particularly investigated. Therefore, thorough fractographic, chemical as well as metallographic investigations were carried out. In order to assess possible fabrication failures selected dimensions of the components were compared with the technical drawings and the surface topography was analysed. The investigation revealed several causes for the fracture of the lag screw which is the implant component intended to fix the position of the femoral head. These are in descending order of relevance: (1) the screw was placed incorrectly and therefore had a smaller bending stiffness, (2) the femoral fracture zone was not stable, i.e., the lag screw 'moved out' of its proper position and (3) the laser marking on the lag screw was relatively large and led to a metallurgical notch at the now, because of the above mentioned points, severely stressed region. A material- or fabrication failure was not the root cause for the fracture of the lag screw. It was mainly due to its incorrect placement during surgery and the instability of the bone fracture. Furthermore, the implant geometry with 130° was not well-suited for the patient's anatomy. A 135°-IMHS might have been biomechanically preferable. Based on the determined failure causes and influences a relative lifetime estimation led to about 10% of the lifetime of a correctly placed 135°-IMHS assuming a sufficiently stable bone fracture zone. KW - Implant fracture KW - Intramedullary hip screw (IMHS) KW - Austenitic steel KW - Laser-marking KW - Implant placement PY - 2012 DO - https://doi.org/10.1016/j.engfailanal.2012.05.010 SN - 1350-6307 SN - 1873-1961 VL - 25 SP - 261 EP - 270 PB - Elsevier Science Publ. CY - Oxford AN - OPUS4-26238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, Gert A1 - Brauser, Stephan A1 - Gaul, Holger A1 - Rethmeier, Michael T1 - Study of fatigue behavior for spot welded tensile shear specimens of advanced high strength steels N2 - For automotive body-in-white applications the influence of manufacture-related gaps between the steel sheets and also of manufacture-related surface cracks on the fatigue behavior of tensile shear specimens for spot welded TRIP steel was analyzed. It was shown that gaps between the steel sheets reduce the fatigue strength, whereas the fatigue behavior is neither influenced by cracks in the electrode indentation area nor in the heat effected zone. KW - Automotive manufacteuring KW - Fatigue behavior KW - TRIP Steel HCT690T PY - 2012 DO - https://doi.org/10.1002/srin.201100286 SN - 1611-3683 SN - 0177-4832 VL - 83 IS - 10 SP - 988 EP - 994 PB - Verl. Stahleisen CY - Düsseldorf AN - OPUS4-27632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiermann, Raphael A1 - Mueller, W. A1 - Montesinos-Castellanos, A. A1 - Metzke, D. A1 - Löb, P. A1 - Hessel, V. A1 - Maskos, Michael T1 - Size controlled polymersomes by continous self-assembly in micromixers N2 - The formation of vesicles based on the self-assembly of amphiphilic poly(butadiene)-b-poly(ethylene oxide) (PB130-b-PEO66) block copolymer in water has been studied using THF as co-solvent. To obtain a highly controlled mixing process for the polymer/THF- and the water-phase, we employed micro mixers with different mixing geometries. The high impact of this preparation method on the self-assembling process was verified by TEM and DLS characterization of the obtained structures. Spherical micelles, vesicles and worm-like micelles were found depending on the parameters of mixing. By additional parameter adjustment in the vesicle regime, the size of the assembled vesicles was controlled between 45 and 100 nm. This demonstrates the continuous preparation of narrowly distributed vesicle structures with controlled sizes. KW - Vesicles KW - Polymersomes KW - Micromixers PY - 2012 DO - https://doi.org/10.1016/j.polymer.2012.03.058 SN - 0032-3861 SN - 1873-2291 VL - 53 IS - 11 SP - 2205 EP - 2210 PB - Springer CY - Berlin AN - OPUS4-25884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H.R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Poly(Epsilon-caprolactone) by combined ring-opening polymerization and azeotropic polycondensation - the role of cyclization and equilibration N2 - Using three different catalysts, water-initiated polymerizations of ε-caprolactone were conducted in bulk with variation of the monomer/water ratio. The resulting CH2OH and CO2H- terminated polylactones were subjected in situ to azeotropic polycondensations. With Bi-triflate and temperatures, the polycondensations were not much successful and involved side reactions. With ZnCl2, and especially SnCl2, considerably higher molar masses were achieved. The substitution of toluene for chlorobenzene for refluxing gave better results. The polycondensations broadened the molar mass distribution of the ROP-based prepolymers, and polydispersities between 1.4–1.8 were obtained. The MALDI–TOF mass spectra revealed that the polycondensations significantly enhanced the fraction of rings due to efficient 'end-biting' reactions. By comparison with copolymerization experiments and Sn methoxide-initiated polymerizations, it was demonstrated that equilibration reactions, such as the formation of rings by 'back-biting,' did not occur. KW - Ring-opening polymerization KW - Epsilon-caprolactone (e-CL) KW - Cyclization KW - MALDI-TOF mass spectrometry KW - Polycondensation KW - Polyesters PY - 2012 DO - https://doi.org/10.1002/pola.26222 SN - 0360-6376 SN - 0887-624X VL - 50 IS - 20 SP - 4206 EP - 4214 PB - Wiley CY - Hoboken, NJ AN - OPUS4-26500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Symietz, Christian A1 - Lehmann, Erhard A1 - Gildenhaar, Renate A1 - Hackbarth, Andreas A1 - Berger, Georg A1 - Krüger, Jörg T1 - Mechanical stability of Ti6Al4V implant material after femtosecond laser irradiation N2 - The surface of a titanium alloy (Ti6Al4V) implant material was covered with a bioactive calcium alkali phosphate ceramic with the aim to accelerate the healing and to form a stronger bond to living bone tissue. To fix the ceramic powder we used a femtosecond laser, which causes a thin surface melting of the metal. It is a requirement to prove that the laser irradiation would not reduce the lifetime of implants. Here we present the results of mechanical stability tests, determined by the rotating bending fatigue strength of sample rods. After describing the sample surfaces and their modifications caused by the laser treatment we give evidence for an unchanged mechanical stability. This applies not only to the ceramic fixation but also to a comparatively strong laser ablation. KW - Aluminium alloys KW - Bending strength KW - Bioceramics KW - Bone KW - Calcium compounds KW - Fatigue KW - Fatigue testing KW - High-speed optical techniques KW - Laser ablation KW - Melting KW - Orthopaedics KW - Prosthetics KW - Rods (structures) KW - Surface treatment KW - Titanium alloys KW - Vanadium alloys PY - 2012 DO - https://doi.org/10.1063/1.4737576 SN - 0021-8979 SN - 1089-7550 VL - 112 IS - 2 SP - 1 EP - 5 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-26200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vöse, Markus A1 - Fedelich, Bernard A1 - Owen, J. T1 - A simplified model for creep induced grain boundary cavitation validated by multiple cavity growth simulations N2 - Simulations of cavitation processes on a grain boundary under creep conditions have been carried out, taking into account nucleation, growth, coalescence and sintering of multiple cavities. Cavity growth rates have been calculated through a resolution procedure based on the use of holomorphic complex functions. Three dimensionless parameters have been identified that are responsible for the cavitation development. Parameter studies have been carried out in order to characterise the mechanisms that are responsible for the cavitation development. These studies have been used to develop a physically motivated, simplified model in order to describe the cavitation development of the simulations in terms of global state variables. The simplified model is able to reproduce the cavitation development for all considered combinations of the dimensionless parameters and allows the description of the thickening behaviour of a cavitating grain boundary. KW - Creep damage KW - Grain boundary diffusion KW - Cavitation KW - Simulation PY - 2012 DO - https://doi.org/10.1016/j.commatsci.2012.01.033 SN - 0927-0256 VL - 58 SP - 201 EP - 213 PB - Elsevier CY - Amsterdam AN - OPUS4-25630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hussung, D. R. A1 - Kurz, J. H. A1 - Stoppel, Markus T1 - Automatisierte, zerstörungsfreie Prüftechnik für großflächige Stahlbetontragwerke - Ein Anwendungsbeispiel T1 - Automated non-destructive inspection techniques for large reinforced concrete constructions - An example of use N2 - Eine Vielzahl zerstörungsfreier Prüfverfahren hat in den letzten Jahren Einzug in die Bauwerksuntersuchung gehalten. Um die Aussagekraft der Einzelverfahren zu erhöhen und den wirtschaftlichen Einsatz weiter voranzubringen, lag es nahe, die Verfahren kombiniert auf einer automatisierten Plattform zu montieren. Zu diesem Zweck wurde das BetoScan-System entwickelt. Um weitere Erfahrungen mit dem BetoScan-System zu erhalten, wurde ein langjährig genutztes Parkhaus aus Stahlbeton mit Gussasphaltfahrbahn als Untersuchungsobjekt ausgewählt. Bei der experimentellen Bauwerksuntersuchung wurden die Verfahren Wirbelstrom, Radar, Ultraschall und Mikrowelle zum Einsatz gebracht. Von der Anwendung des Systems und der Auswertung der Ergebnisse wird in diesem Beitrag berichtet. N2 - In recent years a variety of non-destructive evaluation methods are more and more used for the inspection of constructions. Increasing the information value of inspections and the economic aspects of applications leads to a combination of methods on an automated system. Therefore, the BetoScan robot was developed. Gaining more experience in applications was realized with the inspection of a car park which was unused for several years. The building was made of reinforced concrete with melted asphalt as floor coating. Within the frame of the inspections eddy current, radar, ultrasound and microwaves were used. The application of the BetoScan system and the results are presented in this article. KW - Automatisierte zerstörungsfreie Prüfung KW - Bauwesen KW - Kombination KW - Verfahren KW - Bauwerksüberwachung KW - BetoScan-System KW - Dauerhaftigkeit KW - Gussasphalt KW - Instandsetzung KW - Lebensdauer KW - Mikrowelle KW - Nachhaltigkeit KW - Qualitätssicherung KW - Radar KW - Ultraschall-Prüfung KW - ZfP-Verfahren KW - Bauwerkserhaltung/Sanierung KW - Allgemeines PY - 2012 DO - https://doi.org/10.1002/best.201200048 SN - 0005-9900 SN - 1437-1006 VL - 107 IS - 12 SP - 794 EP - 804 PB - Ernst CY - Berlin AN - OPUS4-27588 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stoppel, Markus A1 - Taffe, Alexander A1 - Wiggenhauser, Herbert A1 - Kurz, J. H. A1 - Boller, C. ED - Grantham, M. ED - Mechtcherine, V. ED - Schneck, U. T1 - Automated multi-sensor systems in civil engineering for condition assessment of concrete structures N2 - Infrastructure is subject to continuous ageing. This has given life cycle management of infrastructure an important role. Therefore an increasing demand for reliable inspection and monitoring tools is noticeable. A combination of different non-destructive test methods is often necessary to receive reliable results for material characterization, flaw detection and the determination of component specific geometry Parameters. Regarding concrete structures thickness measurements are combined with flaw detection and additional Information about reinforcement and tendon ducts is required. Therefore, a multi-sensor measurement approach is necessary with a high degree of automation. Otherwise a time consuming succession of manual measurements has to be performed which would prevent practical applications. A modular control and data acquisition approach is described and the application of two different automated measurement devices is shown. The BetoScan System consists of a self-navigating mobile robot. The System is especially designed for the Investigation of reinforced concrete floors exposed to de-icing salts. The data acquisition of the OSSCAR System, a multi-sensor Scanner, is similar to the robot approach. These different applications are based on a similar kernel allowing the modular use of different contact and non-contact sensors. The described general concept of multi-sensor data acquisition and data analysis presented here is not limited to the field of civil engineering applications. T2 - Concrete Solutions 2011 - 4th International Conference on Concrete Repair CY - Dresden, Germany DA - 26.09.2011 KW - Multi sensor KW - Data aquisition KW - Assessment of concrete structures KW - Scanner KW - NDT PY - 2012 SN - 978-0-415-61-622-5 SP - 397 EP - 403 PB - Taylor & Francis CY - London AN - OPUS4-24659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andrade, M. A. B. A1 - Stindt, Arne A1 - Panne, Ulrich A1 - Riedel, Jens A1 - Adamowski, J. C. T1 - Numerical and experimental determination of the sound pressure distribution in single-axis acoustic levitators N2 - This paper presents a numerical and an experimental procedure to obtain the pressure field in single-axis acoustic levitators. Numerically, the pressure field is determined by a matrix method based on the Rayleigh integral that take into account the multiple wave reflections that occur between the transducer and the reflector. The numerical pressure field is compared with the acoustic pressure measured by an earplug microphone, that is connected to a hollow needle. The tip of the needle is moved by a µm translation stage through the field and the signal is recorded using a lock-in amplifier locked to the levitator frequency. The pressure field obtained numerically show good agreement with that obtained experimentally. T2 - 2012 IEEE International Ultrasonics Symposium (IUS) CY - Dresden, Germany DA - 07.10.2012 KW - Acoustic levitation KW - Matrix method KW - Pressure field PY - 2012 SN - 978-1-4673-4562-0 DO - https://doi.org/10.1109/ULTSYM.2012.0690 SP - 2754 EP - 2757 PB - Institute of Electrical and Electronics Engineers (IEEE) CY - Piscataway, NJ AN - OPUS4-32587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waegner, M. A1 - Schröder, M. A1 - Suchaneck, G. A1 - Sturm, Heinz A1 - Weimann, Christiane A1 - Eng, L. M. A1 - Gerlach, G. T1 - Enhanced piezoelectric response in nano-patterned lead zirconate titanate thin films N2 - In this work, Pb(Zr,Ti)O3 thin films were used to fabricate well-ordered nanodot arrays by means of nanosphere lithography. This technique is based on a two-step etch process that enables excellent control of the fabrication of ordered nanodisc arrays of defined height, diameter, and pitch. Piezoresponse force microscopy was used to investigate both non-patterned and patterned films. The topography and both the out-of-plane and the in-plane polarization were deduced in this mode. Grains of nanodots with a low aspect ratio form domain structures comparable to domains in non-patterned two-dimensional films. In contrast, nanodots with a higher aspect ratio form particular structures like bi-sectioned domain assemblies, c-shaped domains or multi-domains surrounding a center domain. The patterning of the ferroelectric material was shown to affect the formation of ferroelectric domains. The initial polycrystalline films with random polarization orientation re-orient upon patterning and then show domain structures dependent on the nanodisc diameter and aspect ratio. KW - Nanostructures KW - Ferroelectric KW - Nanodots PY - 2012 DO - https://doi.org/10.1143/JJAP.51.11PG04 SN - 0021-4922 VL - 51 SP - 1 EP - 5 PB - IOP Publ. CY - Bristol AN - OPUS4-27697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sturm, Heinz A1 - Schröter, Maria-Astrid A1 - Weimann, Christiane T1 - Imaging method for vibrating scanning force microscopy cantilevers for the analysis of mode shapes and nonlinear harmonic motion N2 - A specially designed scanning force microscope (SFM, atomic force microscope – AFM) was incorporated into the chamber of a commercial scanning electron microscope (SEM) to investigate vibrating SFM cantilevers at their resonance. Inherently, the spatial resolution of electron microscopy is higher than that of optical methods. In this paper we present vibration modes (eigenmodes) of two different SFM cantilevers. Their nonlinear behavior is also explored in order to depict their 2nd harmonics (twice the fundamental frequency). Imaging of the local vibration is performed by measuring the frequency- and phase-selective responses of the SE signal at different X and Y positions of the scanned electron beam. KW - Electron microscopy KW - Scanning force microscopy KW - Motion detection KW - Cantilever KW - Eigenmode KW - Harmonic KW - Nonlinearity KW - Harmonix cantilever PY - 2012 DO - https://doi.org/10.1016/j.mee.2012.07.088 SN - 0167-9317 SN - 1873-5568 VL - 98 SP - 492 EP - 496 PB - Elsevier Science CY - Amsterdam, Netherlands AN - OPUS4-26431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Schulz, Ulrich A1 - Geburtig, Anja A1 - Stephan, Ina T1 - Mildew growth on automotive coatings influencing the results of outdoor weathering N2 - As the results of a 14 weeks outdoor exposure of a series of automotive coatings in South Florida, the panels were found to be overgrown with an almost closed layer of mildew. Pinholes remained as permanent surface damage after removing the mildew mycelium. The extent of the damage differed in dependence of the kind of the coating. By tracing the images and profiles of the coating surfaces systematically over all phases of weathering and the subsequent cleaning procedure, a connection between formation of pinholes and mildew growth could be found. Outdoor weathering tests in other regions of Florida as well as in Europe and Australia showed that pinholes caused by mildew attack could also be found in all other locations, but always to a lower extent than in South Florida. The standardised mildew tests EN ISO 846 and MIL-STD 810F for laboratory exposure failed to reproduce the formation of pinholes. KW - Coatings KW - Mildew KW - Weathering KW - South Florida PY - 2012 DO - https://doi.org/10.1002/maco.201005784 SN - 0947-5117 SN - 1521-4176 VL - 63 IS - 2 SP - 140 EP - 147 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-25467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröter, Maria-Astrid A1 - Holschneider, M. A1 - Sturm, Heinz T1 - Analytical and numerical analysis of imaging mechanism of dynamic scanning electron microscopy N2 - The direct observation of small oscillating structures with the help of a scanning electron beam is a new approach to study the vibrational dynamics of cantilevers and microelectromechanical systems. In the scanning electron microscope, the conventional signal of secondary electrons (SE, dc part) is separated from the signal response of the SE detector, which is correlated to the respective excitation frequency for vibration by means of a lock-in amplifier. The dynamic response is separated either into images of amplitude and phase shift or into real and imaginary parts. Spatial resolution is limited to the diameter of the electron beam. The sensitivity limit to vibrational motion is estimated to be sub-nanometer for high integration times. Due to complex imaging mechanisms, a theoretical model was developed for the interpretation of the obtained measurements, relating cantilever shapes to interaction processes consisting of incident electron beam, electron–lever interaction, emitted electrons and detector response. Conclusions drawn from this new model are compared with numerical results based on the Euler–Bernoulli equation. KW - Electron microscopy KW - Scanning force microscopy KW - Cantilever motion KW - Modes KW - Harmonics KW - Mathematical model KW - Imaging theory PY - 2012 DO - https://doi.org/10.1088/0957-4484/23/43/435501 SN - 0957-4484 SN - 1361-6528 VL - 23 IS - 43 SP - 1 EP - 10 PB - IOP Publishing Ltd. CY - Bristol AN - OPUS4-27642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sturm, Heinz A1 - Schartel, Bernhard A1 - Weiß, André A1 - Braun, Ulrike T1 - SEM/EDX: Advanced investigation of structured fire residues and residue formation N2 - Heterogeneous, gradual or structured morphology of fire residues plays an important role in fire retardancy of polymers. A scanning electron microscope with an attached energy dispersive X-ray spectrometer (SEM/EDX) is highlighted as a powerful tool for the advanced characterization of such complex fire residues, since it offers high resolution in combination with both good depth of field and analysis of chemical composition. Two examples are presented: First, comprehensive SEM/EDX investigation on a complex structured fire residue of glass fibre reinforced polyamide 6,6 (PA 66-GF) flame retarded by diethylaluminium phosphinate, melamine polyphosphate and some zinc borate. A multilayered surface crust (thickness ~ 24 µm) covers a rather hollow area stabilized by GF glued together. The resulting efficient thermal insulation results in self-extinguishing before pyrolysis is completed, even under forced-flaming combustion. Second, sophisticated, quasi online SEM/EDX imaging of the formation of residual protection layer in layered silicate epoxy resin nanocomposites (LSEC). Burning specimens were quenched in liquid nitrogen for subsequent analyses. Different zones were distinguished in the condensed phase characterized by distinct processes such as melting and ablation of organic material, as well as agglomeration, depletion, exfoliation and reorientation of the LS. KW - Fire residue KW - SEM/EDX KW - Fire retardancy KW - PA 66 KW - Layered silicate KW - Diethylaluminium phosphinate PY - 2012 DO - https://doi.org/10.1016/j.polymertesting.2012.03.005 SN - 0142-9418 VL - 31 IS - 5 SP - 606 EP - 619 PB - Elsevier CY - Amsterdam AN - OPUS4-25802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Razzaq, M. Y. A1 - Behl, M. A1 - Frank, U. A1 - Koetz, J. A1 - Szczerba, Wojciech A1 - Lendlein, A. T1 - Oligo(omega-pentadecalactone) decorated magnetic nanoparticles N2 - Hybrid magnetic nanoparticles (mgNP) with a magnetite core diameter of 10 ± 1 nm surface functionalized with oligo(ω-pentadecalactone) (OPDL) oligomers with Mn between 1300 and 3300 g mol-1 could be successfully prepared having OPDL grafted from 200 mg g-1 to 2170 mg g-1. The particles are dispersible in chloroform resulting in stable suspensions. Magnetic response against an external magnetic field proved the superparamagnetic nature of the particles with a low coercivity (Bc) value of 297 µT. The combination of the advantageous superparamagnetism of the mgNP with the exceptional stability of OPDL makes these novel hybrid mgNP promising candidates as multifunctional building blocks for magnetic nanocomposites with tunable physical properties. KW - PPDL KW - OPDL KW - Magnetic core-shell nanoparticles PY - 2012 DO - https://doi.org/10.1039/c2jm16146j SN - 0959-9428 SN - 1364-5501 VL - 22 IS - 18 SP - 9237 EP - 9243 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-25741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mandel, K. A1 - Szczerba, Wojciech A1 - Thünemann, Andreas A1 - Riesemeier, Heinrich A1 - Girod, Matthias A1 - Sextl, G. T1 - Nitric acid-stabilized superparamagnetic iron oxide nanoparticles studied with X-rays N2 - Agglomerated superparamagnetic iron oxide nanoparticles can easily and in large scale be precipitated from iron salt solutions. Although the process is well known, it is ambiguously either assumed that magnetite or maghemite is obtained. The first part of our study clarifies this question using X-ray absorption spectroscopy. For further processing of the nanoparticles, i.e., for giving them a surface functionality or incorporating them into composites, it is important to break the agglomerates and individualize the particles at first. This can effectively be done with nitric acid treatment. The influence of this process on the particles chemistry and structure was analyzed in great detail using X-ray diffraction, X-ray absorption, and smallangle X-ray scattering. In contrast to our expectation, no oxidation from magnetite (Fe3O4) to maghemite (γ- Fe2O3) was found; the formal valence of the particles in any case is magnetite (Fe3O4). Instead, an increase in the particles' surface disorder was discovered from X-ray absorption analyses and high-resolution transmission electron microscopy. The acid treatment roughens and distorts the surface of the nanoparticles which is connected with an increased spin disorder. KW - XANES KW - EXAFS KW - SAXS KW - Coprecipitation KW - Iron oxide spectra KW - Ferrofluid PY - 2012 DO - https://doi.org/10.1007/s11051-012-1066-3 SN - 1388-0764 SN - 1572-896X VL - 14 IS - 8 SP - 1 EP - 9 PB - Kluwer CY - Dordrecht AN - OPUS4-26357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiegner, Katharina A1 - Hahn, Oliver A1 - Horn, Wolfgang A1 - Farke, M. A1 - Kalus, Sabine A1 - Nohr, Michael A1 - Jann, Oliver T1 - Determination of formic and acetic acid emissions in indoor air or from building products N2 - Several construction and building materials, including wood, glue and coatings, are possible sources of very volatile organic compounds (VVOCs) and volatile organic compounds (VOCs) like formic and acetic acid. Due to very high air tightness and very low air exchange rates in new buildings concentrations of these harmful substances can increase considerably. To minimize the risk, emissions from building products should be identified and quantified. With the common standard method, this means Tenax® sampling followed by thermal desorption and GC-MS analysis, these acids could not be detected sufficiently. The aim oft this study is the comparison of two different methods for the determination of acetic and formic acid. The sampling of method one, which is usually used for identification and quantification of VOCs, is done in accordance with ISO 16000-6 and ISO 16017-1 on Carbotrap® 202 multi-bed thermal desorption tube by subsequent identification and quantification with GC-MS. Method two is based on sampling on 2,4-dinitrophenylhydrazine (DNPH) cartridges, derivatisation, elution, identification and quantification of the derivatives with LC-MS/MS (liquid chromatography – mass spectrometry/mass spectrometry). N2 - Viele Konstruktions- und Baumaterialien, wie Holz, Kleber und Anstriche, sind mögliche Quellen für leicht flüchtige organische Verbindungen (VVOC) und flüchtige organische Verbindungen (VOC), wie Ameisen- und Essigsäure. Bedingt durch die hohe Dichtigkeit und den damit verbundenen niedrigen Luftwechsel in neuen Gebäuden können die Konzentrationen dieser gesundheitsgefährdenden Substanzen beträchtlich ansteigen. Um das Risiko zu minimieren, sollen Emissionen aus Bauprodukten identifiziert und quantifiziert werden. Mit der üblichen Standardmethode, die auf einer Luftprobenahme auf Tenax® und anschließender Analyse mittels GC-MS basiert, können diese Säuren nicht ausreichend detektiert werden. Ziel dieser Arbeit ist der Vergleich von zwei unterschiedlichen Methoden zur Bestimmung von Essig- und Ameisensäure. Die Luftprobenahme der ersten Methode, die üblicherweise zur Identifizierung und Quantifizierung von VOC genutzt wird, wurde gemäß ISO 16000-6 and ISO 16017-1 auf Carbotrap® 202, ein mit mehreren Adsorbentien gepacktes Thermodesorptionsrohr, mit anschließender Identifikation und Quantifizierung mittels GC-MS durchgeführt. Die zweite Methode basiert auf einer Luftprobenahme mittels 2,4-Dinitrophenylhydrazin-(DNPH)-Kartuschen, Derivatisierung, Elution, Identifikation und Quantifizierung der Derivate mit LC-MS/MS (Flüssigkeitschromatographie – Massenspektometrie/Massenspektometrie). KW - Formic acid KW - Acetic acid KW - VVOCs KW - Air sampling KW - DNPH PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-255911 UR - http://www.gefahrstoffe.de/gest/article.php?data[article_id]=65887 SN - 0949-8036 SN - 0039-0771 SN - 1436-4891 VL - 72 IS - 3 SP - 84 EP - 88 PB - Springer-VDI-Verlag CY - Düsseldorf AN - OPUS4-25591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard T1 - Towards evidence-based development of flame retarded polymers N2 - Competence in polymer research and development is founded not only on technical/methodical components such as know-how, knowledge and communication, but also on scientific components. According to many sources the latter can be identified as a) identifying topics, tasks, opportunities, challenges, etc. b) describing /understanding phenomena and c) using evidence. Accepting this Basic background, this contribution demonstrates how a, b and c can be fulfilled in the development of flame retarded polymeric materials. Based on different examples of our work over the last 10 years, it is shown that innovation and co-operation are used to tackle actualtasks and opportunities, and that multi-methodical approaches and key experiments are sufficient to generate a deep understanding of phenomena as well as systematic investigations and comprehensive assessments. What is more, the examples shown demonstrate how guidelines are deduced for future material developments, which is, of course, the ultimate benefit of using evidence in applied polymer Science and engineering. T2 - 243rd National ACS meeting - Spring 2012 CY - San Diego, CA, USA DA - 25.03.2012 KW - Flame retardancy KW - Halogen-free KW - Flame retardancy mechanism KW - Fire property assessment PY - 2012 SN - 978-0-8412-2727-9 SN - 1550-6703 N1 - Serientitel: PMSE Preprints – Series title: PMSE Preprints VL - 243 SP - 38-PMSE PB - Amer Chemical SOC CY - Washington, USA AN - OPUS4-26381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schartel, Bernhard A1 - Richter, K. H. A1 - Böhning, Martin ED - Morgan, A. B. ED - Wilkie, C. A. ED - Nelson, G. L. T1 - Synergistic use of talc in halogen-free flame retarded polycarbonate/Acrylonitrile-butadiene-styrene blends N2 - Pyrolysis, flammability, fire behavior, melt viscosity, and gas diffusion of bisphenol A polycarbonate/acrylonitrile-butadiene-styrene (PC/ABS) were investigated, with bisphenol A bis(diphenyl phosphate) (BDP), with 10 wt.% talc and with BDP in combination with 5, 10 and 20 wt.% talc, respectively. Compared to PC/ABS, PC/ABS + BDP results in an increased decomposition temperature of PC, a higher char yield, a significantly increased LOI, a V-0 classification in UL 94, a reduced peak heat release rate (pHRR), and a reduced total heat release (THR) in the cone calorimeter. This efficient flame retardancy is due to mechanisms in both the gas and condensed phases. PC/ABS + 10 wt.% talc shows a decrease in the PC decomposition temperature. The fire behavior is improved in part compared to PC/ABS, with an increased LOI and reduced pHRR. PC/ABS + BDP + 10 wt.% talc shows a strong synergism in LOI, a V-0 classification, and a decrease in pHRR, whereas THR is slightly increased compared to PC/ABS + BDP. Talc decreases the gas diffusion and enhances the flow limit for low shear rates, both of which influence the pyrolysis and flammability results. Further, talc improves the protection properties of the fire residues. Nevertheless it also partly suppresses flame inhibition and the charring effect of BDP. The synergism between BDP and talc in LOI is obtained even for low talc loadings in PC/ABS + BDP + talc, whereas for higher loadings saturation is observed. KW - Flame retardancy KW - PC/ABS KW - Aryl phosphate KW - Talc PY - 2012 SN - 978-0-8412-2780-4 DO - https://doi.org/10.1021/bk-2012-1118.ch002 N1 - Serientitel: ACS Symposium Series – Series title: ACS Symposium Series VL - 1118 IS - Chapter 2 SP - 15 EP - 36 PB - Oxford University Press AN - OPUS4-27563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brice, H. A1 - Theiler, Geraldine A1 - Gradt, Thomas T1 - Frictional behavior of material couples in superconducting MRI magnet systems at 4.2 K N2 - Windings in superconducting magnets operating at 4.2 K are highly susceptible to quenching caused by small frictional heat inputs. Small movements in the magnet system are inevitable during ramping due to the increasing electromagnetic forces. Friction pairs of polymer based materials have been investigated at 4.2 K to gain an understanding of their sliding behavior in conditions representative of superconducting MRI systems. The results indicate that polymer-polymer pairs experience unstable sliding behavior with repeated stick-slip whereas polymer-aluminum couples have stable sliding behavior up to high contact pressures of 20 MPa. KW - Cryotribology KW - Friction KW - MRI magnets KW - Stick-slip PY - 2012 DO - https://doi.org/10.1109/TASC.2011.2175683 SN - 1051-8223 VL - 22 IS - 3 SP - 4400204-1 EP - 4400204-4 PB - IEEE CY - New York, NY AN - OPUS4-26384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sterthaus, Jens A1 - Ballheimer, Viktor A1 - Kuschke, Christian A1 - Wille, Frank T1 - Numerical analysis of bolted trunnion systems of packages for radioactive materials N2 - Packages for the transport of radioactive material are generally equipped with particular components for crane operations and supporting the package during transport. As an example of such components the bolted trunnion system of heavy packages are analysed in this paper. According to the German guideline BAM-GGR 012 created by the BAM Federal Institute for Materials Research and Testing for analysis and assessment of bolted lid and trunnion Systems, the finite element (FE) method is to be used preferably in the analysis of such kind of structures to obtain more accurate and detailed Information about their stressing. The FE model of a trunnion System should include the trunnion itself, the bolts and an appropriate part of the packaging wall with necessary contact conditions on all interfaces between these components. The use of solid finite elements, which is generally recommended in the BAM-GGR 012 guideline, leads to local stress and strain fields as a result of the calculation. The modelling strategy, e.g. the way of modelling interaction between the components of the trunnion System, has an essential impact on these local values. The effect of different assumptions in a FE model is demonstrated in this paper using the calculation results for a reference trunnion System. The approaches for preparation and Interpretation of results in connection with local or nominal assessment criteria are discussed as well. T2 - ASME 2012 Pressure Vessels and Piping Division Conference - PVP 2012 CY - Toronto, Ontario, Canada DA - 15.07.2012 KW - Bolted trunnion KW - German guideline BAM-GGR 012 KW - Local stress and strain fields KW - Local and nominal assessment criteria PY - 2012 SP - 1 EP - 6 PB - American Society of Mechanical Engineers (ASME) CY - New York, NY AN - OPUS4-26835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - Bohmeyer, W. A1 - Lange, K. T1 - Investigation of the crosslinking behaviour of ehtylene vinyl acetate (EVA) for solar cell encapsulation by rheology and ultrasound N2 - EVA is a widely used material for the encapsulation of photovoltaic modules. It melts at elevated temperatures, and seals the module before it is crosslinked at temperatures above 130 °C by a peroxide-initiated crosslinking reaction. EVA has good optical properties necessary for application in solar modules. For process optimization and quality management, a method for the quick and reliable characterization of EVA crosslinking behaviour is of great value. Here, the practicability of ultrasound for online crosslinking monitoring is demonstrated. A sound velocity increase of about 8 m/s during the crosslinking reaction is found. The ultrasound results are compared with rheometer measurements performed with a curemeter typically used for the investigation of rubber crosslinking. KW - Ethylene vinyl acetate KW - EVA KW - Crosslinking KW - Ultrasound KW - Rheology KW - Curemeter KW - DSC PY - 2012 DO - https://doi.org/10.1016/j.polymertesting.2012.07.004 SN - 0142-9418 VL - 31 IS - 7 SP - 904 EP - 908 PB - Elsevier CY - Amsterdam AN - OPUS4-26291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Bressler, I. T1 - Copolymer composition determined by LC-MALDI-TOF MS coupling and 'MassChrom2D' data analysis N2 - The MALDI-TOF MS analysis of copolymers very often results in complex spectra. A chromatographic separation/fractionation prior to the MALDI investigation can be advantageous since the MALDI mass spectra of fractions very often reveal well-resolved peaks of distinguishable copolymer series. For this purpose, different modes of chromatography have been applied. Chromatographic runs were transferred to MALDI targets utilizing a combined air/electrospray deposition device. Using the new MassChrom2D software, fraction-dependent 2D copolymer compositions plots were obtained providing additional information on the chromatographic mode, and enabling fast modification of conditions to increase separation. KW - Copolymer composition KW - Chromatography KW - Coupling KW - MALDI-TOF mass spectrometry PY - 2012 DO - https://doi.org/10.1002/macp.201200169 SN - 1022-1352 SN - 1521-3935 VL - 213 IS - 22 SP - 2404 EP - 2411 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-27270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -