TY - JOUR A1 - Resch-Genger, Ute A1 - Gorris, H.H. T1 - Perspectives and challenges of photon-upconversion nanoparticles - Part I: routes to brighter particles and quantitative spectroscopic studies N2 - Lanthanide-doped photon-upconversion nanoparticles (UCNPs) have been the Focus of many Research activities in materials and life sciences in the last 15 years because of their potential to convert light between different spectral regions and their unique photophysical properties. To fully exploit the application potential of These facinating nanomaterials, a number of challenges have to be overcome, such as the low brightness, particularly of small UCNPs, and the reliable quantification of the excitation-power-density-dependent upconversion luminescence. In this series of critical Reviews, recent developments in the design, Synthesis, optical-spectroscopic characterization, and application of UCNPs are presented with Special Focus on bioanalysis and the life sciences. Here we guide the reader from the Synthesis of UCNPs to different concepts to enhance their luminescence, including the required optical-spectroscopic assessment to quantify material Performance; surface modification strategies and bioanalytical applications as well as selected examples of the use of UCNPs as reporters in different Assay formats are addressed in part II. Future Trends and challenges in the field of upconversion are discussed with Special emphasis on UCNP Synthesis and material characterization, particularly quantitative luminescence studies. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield PY - 2017 DO - https://doi.org/10.1007/s00216-017-0499-z SN - 1618-2650 SN - 1618-2642 VL - 409 IS - 25 SP - 5855 EP - 5874 PB - Springer AN - OPUS4-41665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudenko, A. A1 - Colombier, J.-P. A1 - Höhm, S. A1 - Rosenfeld, A. A1 - Krüger, Jörg A1 - Bonse, Jörn A1 - Itina, T.E. T1 - Spontaneous periodic ordering on the surface and in the bulk of dielectrics irradiated by ultrafast laser: a shared electromagnetic origin N2 - Periodic self-organization of matter beyond the diffraction limit is a puzzling phenomenon, typical both for surface and bulk ultrashort laser processing. Here we compare the mechanisms of periodic nanostructure formation on the surface and in the bulk of fused silica. We show that volume nanogratings and surface nanoripples having subwavelength periodicity and oriented perpendicular to the laser polarization share the same electromagnetic origin. The nanostructure orientation is defined by the near-field local enhancement in the vicinity of the inhomogeneous scattering centers. The periodicity is attributed to the coherent superposition of the waves scattered at inhomogeneities. Numerical calculations also support the multipulse accumulation nature of nanogratings formation on the surface and inside fused silica. Laser surface processing by multiple laser pulses promotes the transition from the high spatial frequency perpendicularly oriented nanoripples to the low spatial frequency ripples, parallel or perpendicular to the laser polarization. The latter structures also share the electromagnetic origin, but are related to the incident field interference with the scattered far-field of rough non-metallic or transiently metallic surfaces. The characteristic ripple appearances are predicted by combined electromagnetic and thermo-mechanical approaches and supported by SEM images of the final surface morphology and by time-resolved pump-probe diffraction measurements. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser KW - Nanostructures KW - Dielectrics KW - Electromagnetic scattering PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-421747 UR - https://www.nature.com/articles/s41598-017-12502-4 DO - https://doi.org/10.1038/s41598-017-12502-4 SN - 2045-2322 VL - 7 SP - Article 12306, 1 EP - 14 PB - Springer Nature AN - OPUS4-42174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klingelhöffer, Hellmuth A1 - Aegerter, J. A1 - Scherm, T. A1 - Schenuit, E. A1 - Sotheran, S. A1 - Loveday, M. A1 - Bosch, P. A1 - Bloching, H. A1 - Olbricht, Jürgen A1 - McEnteggart, I. T1 - Discussion on “Analysis on the issues in ISO 6892-1 and TENSTAND WP4 report based on the data of confirm tests by 21 laboratories” by H. Li, X. Zhou, J. Shen, and D. Luo. The regular article was published in journal of Testing and Evaluation, Vol. 45, No. 3, 2017, pp. 723–731, doi:10.1520/ JTE20150479. ISSN 0090-3973 N2 - The authors, Li et al., of the paper entitled “Analysis on the Issues in ISO 6892-1 and TENSTAND WP4 Report Based on Data to Confirm Tests by 21 Laboratories” (J. Test. Eval. DOI: 10.1520/JTE20150479 (online only)) have expressed views that the authors of this rebuttal believe to be based on fundamental misunderstandings and misinterpretations of the tensile testing standard ISO 6892-1:2009, ISO 6892-1:2016, and its former versions, thus leading to erroneous conclusions. This refutation is intended to clarify the understanding of ISO 6892-1 and to address the misunderstandings and the misinterpretations of the authors of the paper. The present standard ISO 6892-1:2016 has a long history dating back to the 1970s. At that time, the tensile testing procedure was standardized on the National and International scale in parallel. To understand the present standard, the knowledge of the history helps to understand the background of details of the testing procedure implemented today. The history of the tensile testing standard has been discussed extensively during the annual international standardization meeting of ISO committee TC 164 SC1 for the last few years, at which some of the authors of the Li et al. paper attended. The authors continue to disagree with facts that were agreed by the consortium of the European research project TENSTAND and by the present international experts involved in ISO TC 164 SC1. It appears that the principal objective of the authors regarding their present publication was to increase the testing speed during tensile testing. However, the international standardization community has previously declined similar proposals by some of the authors. Many Arguments presented by Li et al. were thus refuted. The conclusions of their paper are misleading and the international standardization community for tensile testing refused to revise the present standard, ISO 6892-1 (2016), according the authors’ proposals. KW - Tnsile testing KW - ISO 6892-1 KW - TENSTAND WP4 Report PY - 2017 UR - www.astm.org DO - https://doi.org/10.1520/JTE20160526 SN - 0090-3973 VL - 45 IS - 3 SP - 1105 EP - 1114 PB - ASTM CY - West Conshohocken, PA, USA AN - OPUS4-46690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grohmann, Maria A1 - Müller, Sabine A1 - Niederleithinger, Ernst A1 - Sieber, S. T1 - Reverse time migration: introducing a new imaging technique for ultrasonic measurements in civil engineering N2 - Ultrasonic echo testing is widely used in non-destructive testing in civil engineering to investigate concrete structures, to measure thickness, and to locate and characterise built-in components or inhomogeneities. Currently, synthetic aperture focusing techniques are mostly used for imaging. These algorithms are highly developed but have some limitations. For example, it is not possible to image the lower boundary of built-in components like tendon ducts or vertical reflectors. We adopted reverse time migration for non-destructive testing in civil engineering in order to improve the imaging of complicated structures in concrete. By using the entire wavefield, including waves reflected more than once, there are fewer limitations compared to synthetic aperture focusing technique algorithms. As a drawback, the required computation is significantly higher than that for the techniques currently used. Simulations for polyamide and concrete structures showed the potential for non-destructive testing. The simulations were followed by experiments at a polyamide specimen. Here, having acquired almost noise-free measurement data to test the algorithm, we were able to determine the shape and size of boreholes with sufficient accuracy. After these successful tests, we performed experiments at a reinforced concrete foundation slab. We obtained information from the data by reverse time migration, which was not accessible by traditional imaging. The imaging of the location and structure of the lower boundary of the concrete foundation slab was improved. Furthermore, vertical reflectors inside the slab were imaged clearly, and more flaws were found. It has been shown that reverse time migration is a step forward in ultrasonic testing in civil engineering. KW - Ultrasonic echo technique KW - Reverse time migration PY - 2017 DO - https://doi.org/10.3997/1873-0604.2017006 SN - 1569-4445 SN - 1873-0604 VL - 15 IS - 3 SP - 242 EP - 258 PB - Wiley AN - OPUS4-41921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu 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 - Maierhofer, Christiane A1 - Krankenhagen, Rainer A1 - Röllig, Mathias A1 - Rehmer, Birgit A1 - Gower, M. A1 - Baker, G. A1 - Lodeiro, M. A1 - Aktas, A. A1 - Monte, C. A1 - Adibekyan, A. A1 - Gutschwager, B. T1 - Defect characterisation of tensile loaded CFRP and GFRP laminates used in energy applications by means of infrared thermography N2 - The increased use of fibre reinforced plastic (FRP) composites for improved efficiency and reliability in energy related applications, e.g. wind and marine turbine blades, nacelles, oil and gas flexible risers, also increases the demand for innovative non-destructive testing technologies. In this contribution, results concerning the characterisation of CFRP and GFRP during and after quasi-static tensile loading are presented. It includes the measurement of optical properties in the infrared spectral range, tensile loading tests with the observation of the temperature distribution at one or both sides of the specimens using an infrared camera for the preparation and monitoring of intended natural defects, and active thermography inspections after tensile loading. It is shown that the defect preparation was successful. Thermographic monitoring during and active thermography testing after tensile loading enable the detection of the lateral extend of the generated defects. Differences between CFRP and GFRP materials are discussed. KW - Tensile loading KW - Fibre reinforced composites KW - Active and passive thermography KW - Emissivity PY - 2017 DO - https://doi.org/10.1080/17686733.2017.1334312 SN - 1768-6733 SN - 2116-7176 VL - 15 IS - 1 SP - 17 EP - 36 PB - Taylor and Francis CY - London AN - OPUS4-40968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadammal, Naresh A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Thiede, Tobias A1 - Kromm, Arne A1 - Seyfert, Christoph A1 - Farahbod, Lena A1 - Haberland, Christoph A1 - Schneider, Judith Ann A1 - Portella, Pedro Dolabella A1 - Bruno, Giovanni T1 - Effect of hatch length on the development of microstructure, texture and residual stresses in selective laser melted superalloy Inconel 718 N2 - In the present study, samples fabricated by varying the deposition hatch length during selective laser melting of nickel based superalloy Inconel 718 were investigated. Microstructure and texture of these samples was characterized using scanning electron microscopy, combined with electron back-scattered diffraction, and residual stress assessment, using neutron diffraction method. Textured columnar grains oriented along the sample building direction were observed in the shorter hatch length processed sample. A ten-fold increase in the hatch length reduced the texture intensity by a factor of two attributed to the formation of finer grains in the longer hatch length sample. Larger gradients of transverse residual stress in the longer hatch length sample were also observed. Along the build direction, compressive stresses in the shorter hatch length and negligible stresses for the longer hatch length specimen were observed. Changes to the temperature gradient (G) in response to the hatch length variation, influenced the G to growth rate (R) ratio and the product G × R, in agreement with the microstructures and textures formed. For the residual stress development, geometry of the part also played an important role. In summary, tailored isotropy could be induced in Inconel 718 by a careful selection of parameters during selective laser melting. KW - Additive manufacturing KW - Nickel-based superalloy KW - Microstructure and texture KW - Residual stress KW - Electron back-scattered diffraction KW - Neutron diffraction PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0264127517308018 DO - https://doi.org/10.1016/j.matdes.2017.08.049 SN - 0264-1275 VL - 134 SP - 139 EP - 150 PB - Elsevier CY - Oxford, UK AN - OPUS4-41606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Jörg F. A1 - Kindrachuk, Vitaliy T1 - A Fourier transformation-based temporal integration scheme for viscoplastic solids subjected to fatigue deterioration N2 - Using continuum damage mechanics (CDM) for lifetime prediction requires numerical integration of evolving damage until the onset of failure. The primary challenge for the simulation of structural fatigue failure is caused by the enormous computational costs due to cycle-by-cycle temporal integration throughout the whole loading history, which is in the order of 103–107 cycles. As a consequence, most approaches circumvent this problem and use empirical methods such as Wöhler curves. They are well suited for approximating the lifetime, but they are not capable to capture a realistic degradation of the material including redistribution of stresses. The main objective of the paper is to provide a technique for finite element (FE) simulations of structures under fatigue loading while reducing computational costs. A Fourier transformation-based temporal integration (FTTI) scheme is proposed, which adapts the conventional FE method for modeling the viscoplastic deterioration in a structure subjected to cyclic loading. The response fields are represented by a Fourier series which assumes a temporal scale separation: a microchronological (short time) scale arises from the oscillatory loading and a macrochronological (long time) scale is due to the slow material relaxation resulting from yielding and damage evolution. The original dynamic boundary value problem (BVP) is approximated by the stationary BVP on the microchronological scale. Alternation of the displacement field on the macrochronological scale is correlated with evolution of the history variables by means of a high order adaptive cycle jump method. Performance and significant acceleration of the FE simulations is demonstrated at different loading scenarios for a constitutive damage model where the progressive damage accumulation is driven by viscoplastic yielding. KW - Fatigue KW - Accelerated time integration KW - Continuum damage mechanics KW - Fourier series PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2017.03.015 SN - 0142-1123 SN - 1879-3452 VL - 100 IS - 1 SP - 215 EP - 228 PB - Elsevier Ltd. AN - OPUS4-39616 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 - Scheuerlein, C. A1 - Uhlemann, Patrick A1 - Finn, Monika A1 - Lackner, F. A1 - Savary, F. T1 - Mechanical properties of the HL-LHC 11 T Nb3Sn magnet constituent materials N2 - A test campaign was launched to determine the mechanical properties of the High Luminosity-Large HadronCollider (HL-LHC) 11 T Nb3Sn magnet components. The results can be used to accurately represent the mechanical properties in finite elementmodels that predict the stress and strain distribution in these magnets. Particular attention is paid to anisotropic mechanical behavior of the different magnet materials. Static and dynamic test methods have been applied for determining elastic materials’ behavior, and highly accurate Young’s moduli are obtained with the nondestructive dynamic methods resonance and impulse excitation at ambient temperature and during in situ heat cycles. KW - Superconducting magnets KW - Young’s modulus KW - Resonance testing KW - Stress-strain behavior PY - 2017 DO - https://doi.org/10.1109/TASC.2016.2638046 SN - 1051-8223 SN - 1558-2515 VL - 27 IS - 4 SP - 1 EP - 7 PB - IEEE AN - OPUS4-39219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kühn, Hans-Joachim A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Thermomechanical fatigue of heat-resistant austenitic cast iron EN-GJSA-XNiSiCr35-5-2 (Ni-Resist D-5S) N2 - TMF tests were carried out on EN-GJSA-XNiSiCr35-5-2 at constant minimum temperature (400 °C) and varying maximum temperatures (Tmax = 700 °C, 800 °C, 900 °C) with hold times of 180 s at Tmax and two phase angles (in-phase (IP), 180° out-of-phase (OP)). The results showed a comparable strength under OP- and IP-TMF loading. At Tmax = 700 °C and 900 °C, the lifetime in IP-tests was slightly longer than that of OP-tests, while it is vice versa at Tmax = 800 °C. The IP-tests at Tmax = 900 °C showed a similar lifetime as OP-tests at Tmax = 700 °C and 800 °C, which was unexpected for such a high testing temperature. All IP-tests at Tmax = 900 °C showed a continuous cyclic softening from the beginning on, which was different from all other testing conditions. Complementary metallographic investigations indicated that under this test condition, intergranular creep damage is present in the volume of the test pieces. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Cast iron KW - Cracks KW - Cyclic softening KW - Microscopy KW - Thermomechanical fatigue PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2017.01.009 SN - 0142-1123 SN - 1879-3452 VL - 99 IS - 2 (Special issue: Recent developments in thermo-mechanical fatigue) SP - 295 EP - 302 PB - Elsevier CY - Oxford AN - OPUS4-39680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Omara, Shereen Shabaan A1 - Turky, G. A1 - Ghoneim, A. A1 - Thünemann, Andreas A1 - Abdel Rehim, M. H. A1 - Schönhals, Andreas T1 - Hyperbranched poly(amidoamine)/kaolinite nanocomposites: Structure and charge carrier dynamics N2 - An ex-situ approach was applied to prepare nanocomposites from hyperbranched poly(amidoamine) and modified kaolinite (Ka-DCA). The structure of the polymer and the corresponding nanocomposites was investigated by FTIR, DSC, SAXS and TEM. SAXS might suggest a partly exfoliated structure of the nanocomposites, which was supported by TEM. The molecular dynamics was studied by means of broadband dielectric spectroscopy (BDS). The dielectric spectra are dominated by a conductivity contribution at higher temperatures for all samples investigated. The obtained results further indicated that DC conductivity is increased by 4 orders of magnitude with increasing concentration of Ka-DCA nanofiller. Further, a significant separation between the conductivity relaxation time and that of segmental dynamics was observed. The decoupling phenomenon and the conductivity mechanism were discussed in detail. This study provides insights about the influence of the nanofiller on the structure and the conductivity contribution of nanocomposites of hyperbranched polymers including the decoupling phenomenon and fragility. KW - Hyperbranched polymers KW - Nanocomposites KW - Conductivity PY - 2017 DO - https://doi.org/10.1016/j.polymer.2017.06.017 SN - 0032-3861 VL - 121 SP - 64 EP - 74 PB - Elsevier Ltd. AN - OPUS4-40648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Juling, S. A1 - Niedzwiecka, A. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Selve, S. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Krause, E. A1 - Lampen, A. T1 - Protein Corona Analysis of Silver Nanoparticles Links to Their Cellular Effects N2 - The breadth of applications of nanoparticles and the access to food-associated consumer products containing nanosized materials lead to oral human exposure to such particles. In biological fluids nanoparticles dynamically interact with biomolecules and form a protein corona. Knowledge about the protein corona is of great interest for understanding the molecular effects of particles as well as their fate inside the human body. We used a mass spectrometry-based toxicoproteomics approach to elucidate mechanisms of toxicity of silver nanoparticles and to comprehensively characterize the protein corona formed around silver nanoparticles in Caco-2 human intestinal epithelial cells. Results were compared with respect to the cellular function of proteins either affected by exposure to nanoparticles or present in the protein corona. A transcriptomic data set was included in the analyses in order to obtain a combined multiomics view of nanoparticle-affected cellular processes. A relationship between corona proteins and the proteomic or transcriptomic responses was revealed, showing that differentially regulated proteins or transcripts were engaged in the same cellular signaling pathways. Protein corona analyses of nanoparticles in cells might therefore help in obtaining information about the molecular consequences of nanoparticle treatment. KW - Silver nanoparticles KW - Protein KW - Small-angle X-ray scattering KW - SAXS PY - 2017 DO - https://doi.org/10.1021/acs.jproteome.7b00412 SN - 1535-3893 SN - 1535-3907 VL - 16 IS - 11 SP - 4020 EP - 4034 PB - Americal Chemical Society AN - OPUS4-42688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lichtenstein, D. A1 - Meyer, T. A1 - Böhmert, L. A1 - Juling, S. A1 - Fahrenson, C. A1 - Selve, S. A1 - Thünemann, Andreas A1 - Meijer, J. A1 - Estrela-Lopis, I. A1 - Braeuning, A. A1 - Lampen, A. T1 - Dosimetric quantification of coating-related uptake of silver nanoparticles N2 - The elucidation of mechanisms underlying the cellular uptake of nanoparticles (NPs) is an important topic in nanotoxicological research. Most studies dealing with silver NP uptake provide only qualitative data about internalization efficiency and do not consider NP-specific dosimetry. Therefore, we performed a comprehensive comparison of the cellular uptake of differently coated silver NPs of comparable size in different human intestinal Caco-2 cell-derived models to cover also the influence of the intestinal mucus barrier and uptake-specialized M-cells. We used a combination of the Transwell system, transmission electron microscopy, atomic absorption spectroscopy, and ion beam microscopy techniques. The computational in vitro sedimentation, diffusion, and dosimetry (ISDD) model was used to determine the effective dose of the particles in vitro based on their individual physicochemical characteristics. Data indicate that silver NPs with a similar size and shape show coating-dependent differences in their uptake into Caco-2 cells. The internalization of silver NPs was enhanced in uptake-specialized M-cells while the mucus did not provide a substantial barrier for NP internalization. ISDD modeling revealed a fivefold underestimation of dose–response relationships of NPs in in vitro assays. In summary, the present study provides dosimetry-adjusted quantitative data about the influence of NP coating materials in cellular uptake into human intestinal cells. Underestimation of particle effects in vitro might be prevented by using dosimetry models and by considering cell models with greater proximity to the in vivo situation, such as the M-cell model. KW - Silver nanoparticles KW - Small-angle X-ray scattering KW - Saxs PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.7b01851 SN - 0743-7463 VL - 33 IS - 45 SP - 13087 EP - 13097 PB - Americal Chemical Society AN - OPUS4-42875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Kang, Nianjun A1 - Wang, De-Yi A1 - Falkenhagen, Jana A1 - Thünemann, Andreas A1 - Schönhals, Andreas T1 - Structure–Property Relationships of Nanocomposites Based on Polylactide and Layered Double Hydroxides – Comparison of MgAl and NiAl LDH as Nanofiller N2 - Nanocomposites based on poly(L-lactide) (PLA) and organically modified Ni/Al layered double hydroxides (NiAl/LDHs) are prepared by melt blending and investigated by a combination of size exclusion chromatography, differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), wide-angle X-ray scattering, and broadband dielectric spectroscopy. A detailed comparison to the behavior of the corresponding MgAl/LDH–PLA nanocomposites is made. SAXS investigations show that the morphology of the NiAl/LDH–PLA nanocomposites is more intercalated compared to the MgAl/LDH based PLA nanocomposite, which is more exfoliated. The DSC investigation gives a different dependence of the degree of crystallization on the concentration of LDH for NiAl/LDH–PLA than for MgAl/LDH–PLA nanocomposite system. These differences are discussed taking the differences of the morphologies of both systems into account. Broadband dielectric spectroscopy reveals information about the molecular dynamics where essential differences are observed for all relaxation processes taking place in both systems which were related to the different morphologies. KW - Nanocomposites KW - Polylactide PY - 2017 DO - https://doi.org/10.1002/macp.201700232 SN - 1022-1352 SN - 1521-3935 VL - 218 IS - 20 SP - Article 1700232, 1 EP - 12 PB - Wiley-VCH Verlag AN - OPUS4-42597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieg, H. A1 - Kästner, Claudia A1 - Krause, B. A1 - Meyer, T. A1 - Burel, A. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Jungnickel, H. A1 - Tentschert, J. A1 - Laux, P. A1 - Braeuning, A. A1 - Estreal-Lopis, I. A1 - Gauffre, F. A1 - Fessard, V. A1 - Meijer, J. A1 - Luch, A. A1 - Thünemann, Andreas A1 - Lampen, A. T1 - Impact of an artificial digestion procedure on aluminum-containing nanomaterials N2 - Aluminum has gathered toxicological Attention based on relevant human exposure and its suspected hazardous potential. Nanoparticles from food supplements or Food contact materials may reach the human gastrointestinal tract. Here, we monitored the physicochemical fate of aluminum containing nanoparticles and aluminum ions when passaging an in vitro model of the human gastrointestinal tract. Smallangle X-ray scattering (SAXS), transmission electron microscopy (TEM), ion beam microscopy (IBM), secondary ion beam mass spectrometry (TOF-SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) in the singleparticle mode were employed to characterize two aluminumcontaining nanomaterials with different particle core materials (Al0, γAl2O3) and soluble AlCl3. Particle size and shape remained unchanged in saliva, whereas strong Agglomeration of both aluminum nanoparticle species was observed at low pH in gastric fluid together with an increased ion release. The levels of free aluminum ions decreased in intestinal fluid and the particles deagglomerated, thus liberating primary particles again. Dissolution of nanoparticles was limited and substantial changes of their shape and size were not detected. The amounts of particle-associated phosphorus, chlorine, potassium, and calcium increased in intestinal fluid, as compared to nanoparticles in standard dispersion. Interestingly, nanoparticles were found in the intestinal fluid after addition of ionic aluminum. We provide a comprehensive characterization of the fate of aluminum nanoparticles in simulated gastrointestinal fluids, demonstrating that orally ingested nanoparticles probably reach the intestinal epithelium. The balance between dissolution and de novo complex formation should be considered when evaluating nanotoxicological experiments. KW - Small-angle X-ray scattering KW - SAXS KW - Nanoparticle PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.7b02729 SN - 1520-5827 SN - 0743-7463 VL - 33 IS - 40 SP - 10726 EP - 10735 PB - Americal Chemical Society AN - OPUS4-42438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lichtenstein, D. A1 - Ebmeyer, J. A1 - Meyer, T. A1 - Behr, A.-C. A1 - Kästner, Claudia A1 - Böhmert, L. A1 - Juling, J. A1 - Niemann, B. A1 - Fahrenson, C. A1 - Selve, S. A1 - Thünemann, Andreas A1 - Meijer, J. A1 - Estrela-Lopis, I. A1 - Bräuning, A. A1 - Lampen, A. T1 - It takes more than a coating to get nanoparticles through the intestinal barrier in vitro N2 - Size and shape are crucial parameters which have impact on the potential of nanoparticles to penetrate cell membranes and epithelial barriers. Current research in nanotoxicology additionally focuses on particle coating. To distinguish between core- and coating-related effects in nanoparticle uptake and translocation, two nanoparticles equal in size, coating and charge but different in core material were investigated. Silver and iron oxide nanoparticles coated with poly(acrylic acid) were chosen and extensively characterized by small-angle x-ray scattering, nanoparticle tracing analysis and transmission electron microscopy (TEM). Uptake and transport were studied in the intestinal Caco-2 model in a Transwell System with subsequent elemental analysis. TEM and ion beam microscopy were conducted for particle visualization. Although equal in size, charge and coating, the behavior of the two particles in Caco-2 cells was different: while the internalized amount was comparable, only iron oxide nanoparticles additionally passed the epithelium. Our findings suggest that the coating material influenced only the uptake of the nanoparticles whereas the translocation was determined by the core material. Knowledge about the different roles of the particle coating and core materials in crossing biological barriers will facilitate toxicological risk assessment of nanoparticles and contribute to the optimization of pharmacokinetic properties of nano-scaled pharmaceuticals. KW - Silver KW - Nanoparticle KW - Polymer KW - Polyacrylic acid PY - 2017 DO - https://doi.org/10.1016/j.ejpb.2016.12.004 SN - 0939-6411 SN - 1873-3441 VL - 118 SP - 21 EP - 29 PB - Elsevier AN - OPUS4-41170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, P A1 - Balceris, C. A1 - Ludwig, F A1 - Posth, O A1 - Bogart, L. K. A1 - Szczerba, Wojciech A1 - Castro, A A1 - Nilsson, L A1 - Costo, R A1 - Gavilan, H A1 - Gonzalez-Alonso, D A1 - de Pedro, I A1 - Barquin, L. F. A1 - Johansson, C T1 - Distribution functions of magnetic nanoparticles determined by a numerical inversion method N2 - In the present study, we applied a regularized inversion method to extract the particle size, magnetic moment and relaxation-time distribution of magnetic nanoparticles from small-angle x-ray scattering (SAXS), DC magnetization (DCM) and AC susceptibility (ACS) measurements. For the measurements the particles were colloidally dispersed in water. At first approximation the particles could be assumed to be spherically shaped and homogeneously magnetized single-domain particles. As model functions for the inversion, we used the particle form factor of a sphere (SAXS), the Langevin function (DCM) and the Debye model (ACS). The extracted distributions exhibited features/peaks that could be distinctly attributed to the individually dispersed and non-interacting nanoparticles. Further analysis of these peaks enabled, in combination with a prior characterization of the particle ensemble by electron microscopy and dynamic light scattering, a detailed structural and magnetic characterization of the particles. Additionally, all three extracted distributions featured peaks, which indicated deviations of the scattering (SAXS), magnetization (DCM) or relaxation (ACS) behavior from the one expected for individually dispersed, homogeneously magnetized nanoparticles. These deviations could be mainly attributed to partial agglomeration (SAXS, DCM, ACS), uncorrelated surface spins (DCM) and/or intra-well relaxation processes (ACS). The main advantage of the numerical inversion method is that no ad hoc assumptions regarding the line shape of the extracted distribution functions are required, which enabled the detection of these contributions. We highlighted this by comparing the results with the results obtained by standard model fits, where the functional form of the distributions was a priori assumed to be log-normal shaped. KW - SAXS KW - Small-angle X-ray scattering KW - Nanoparticle PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-429373 DO - https://doi.org/10.1088/1367-2630/aa73b4 SN - 1367-2630 VL - 19 SP - 073012, 1 EP - 073012, 19 PB - IOP Publ. Ltd. AN - OPUS4-42937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Terril, N. J. A1 - Thünemann, Andreas T1 - The modular small-angle X-ray scattering data correction sequence N2 - Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors. KW - Small-angle X-ray scattering KW - SAXS KW - Accuracy KW - Methodology KW - Data correction PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432114 DO - https://doi.org/10.1107/S1600576717015096 SN - 1600-5767 VL - 50 IS - 6 SP - 1800 EP - 1811 PB - International Union of Crystallography AN - OPUS4-43211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -