TY - JOUR A1 - Faghani, A. A1 - Gholami, M. F. A1 - Trunk, M. A1 - Müller, J. A1 - Pachfule, P. A1 - Vogl, S. A1 - Donskyi, Ievgen A1 - Li, M. A1 - Nickl, Philip A1 - Shao, J. A1 - Huang, M. R. S. A1 - Unger, Wolfgang A1 - Arenal, R. A1 - Koch, C. T. A1 - Paulus, B. A1 - Rabe, J. P. A1 - Thomas, A. A1 - Haag, R. A1 - Adeli, M. T1 - Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale N2 - Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation. KW - XPS KW - Triazine KW - 2D PY - 2020 DO - https://doi.org/10.1021/jacs.0c02399 VL - 142 IS - 30 SP - 12976 EP - 12986 PB - ACS American Chemical Society AN - OPUS4-51203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abou-Ras, D. A1 - Caballero, R. A1 - Fischer, C.-H. A1 - Kaufmann, C.A. A1 - Lauermann, I. A1 - Mainz, R. A1 - Mönig, H. A1 - Schöpke, A. A1 - Stephan, C. A1 - Streeck, C. A1 - Schorr, S. A1 - Eicke, A. A1 - Döbeli, M. A1 - Gade, B. A1 - Hinrichs, J. A1 - Nunney, T. A1 - Dijkstra, H. A1 - Hoffmann, V. A1 - Klemm, D. A1 - Efimova, V. A1 - Bergmaier, A. A1 - Dollinger, G. A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Rockett, A.A. A1 - Perez-Rodriguez, A. A1 - Alvarez-Garcia, J. A1 - Izquierdo-Roca, V. A1 - Schmid, T. A1 - Choi, P.-P. A1 - Müller, M. A1 - Bertram, F. A1 - Christen, J. A1 - Khatri, H. A1 - Collins, R.W. A1 - Marsillac, S. A1 - Kötschau, I. T1 - Comprehensive comparison of various techniques for the analysis of elemental distributions in thin films N2 - The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits. KW - Elemental distributions KW - Comparison KW - Depth profiling KW - Chemical mapping KW - Thin films KW - Solar cells KW - Chalcopyrite-type KW - Cu(In,Ga)Se2 PY - 2011 DO - https://doi.org/10.1017/S1431927611000523 SN - 1431-9276 SN - 1435-8115 VL - 17 IS - 5 SP - 728 EP - 751 PB - Cambridge University Press CY - New York, NY AN - OPUS4-24506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kasper, J. A1 - Hermanns, M. A1 - Bantz, C. A1 - Maskos, Michael A1 - Stauber, R. A1 - Pohl, C. A1 - Unger, R. E. A1 - Kirkpatrick, J.C. T1 - Inflammatory and cytotoxic responses of an alveolar-capillary coculture model to silica nanoparticles: comparison with conventional monocultures N2 - To date silica nanoparticles (SNPs) play an important role in modern technology and nanomedicine. SNPs are present in various materials (tyres, electrical and thermal insulation material, photovoltaic facilities). They are also used in products that are directly exposed to humans such as cosmetics or toothpaste. For that reason it is of great concern to evaluate the possible hazards of these engineered particles for human health. Attention should primarily be focussed on SNP effects on biological barriers. Accidentally released SNP could, for example, encounter the alveolar-capillary barrier by inhalation. In this study we examined the inflammatory and cytotoxic responses of monodisperse amorphous silica nanoparticles (aSNPs) of 30 nm in size on an in vitro coculture model mimicking the alveolar-capillary barrier and compared these to conventional monocultures. Methods Thus, the epithelial cell line, H441, and the endothelial cell line, ISO-HAS-1, were used in monoculture and in coculture on opposite sides of a filter membrane. Cytotoxicity was evaluated by the MTS assay, detection of membrane integrity (LDH release), and TER (Transepithelial Electrical Resistance) measurement. Additionally, parameters of inflammation (sICAM-1, IL-6 and IL-8 release) and apoptosis markers were investigated. Results Regarding toxic effects (viability, membrane integrity, TER) the coculture model was less sensitive to apical aSNP exposure than the conventional monocultures of the appropriate cells. On the other hand, the in vitro coculture model responded with the release of inflammatory markers in a much more sensitive fashion than the conventional monoculture. At concentrations that were 10-100fold less than the toxic concentrations the apically exposed coculture showed a release of IL-6 and IL-8 to the basolateral side. This may mimic the early inflammatory events that take place in the pulmonary alveoli after aSNP inhalation. Furthermore, a number of apoptosis markers belonging to the intrinsic pathway were upregulated in the coculture following aSNP treatment. Analysis of the individual markers indicated that the cells suffered from DNA damage, hypoxia and ER-stress. Conclusion We present evidence that our in vitro coculture model of the alveolar-capillary barrier is clearly advantageous compared to conventional monocultures in evaluating the extent of damage caused by hazardous material encountering the principle biological barrier in the lower respiratory tract. KW - Silica nanoparticles KW - Alveolar-capillary coculture model KW - Cytotoxicity PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254217 DO - https://doi.org/10.1186/1743-8977-8-6 SN - 1743-8977 VL - 8 IS - 6 SP - 1 EP - 16(?) PB - BioMed Central CY - London AN - OPUS4-25421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moritz, W. A1 - Werner, R. A1 - Tausche, A. A1 - Cherkaschinin, G. A1 - Molajew, R. A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Linke, S. T1 - Alloys for gas sensors investigated using the continuous gradient-high throughput screening macroscope CG-HTSM N2 - Ternary alloys have been studied as the gate metal of chemical sensors based on the field effect in silicon. The investigation of reduced poisoning of hydrogen sensors by H2S is presented in the alloy system PdxNiyCo1-x-y. A new method in high throughput screening of alloys is applied. Not singular sample compositions but a continuous gradient in alloy concentrations was produced on a semiconductor sample. A laser scanning system produces a photo current in the semiconductor to map the sensor signal and provide a quasi continuous alloy characterization. The new system is therefore called Continuous Gradient—High Throughput Screening Macroscope (CG-HTSM). Typically 625 alloys are characterized in 15 minutes. The resolution of our set-up allows distinguishing 100.000 alloy compositions. KW - Alloy KW - Sensor KW - High throughput screening KW - Macroscope PY - 2011 DO - https://doi.org/10.1166/sl.2011.1586 SN - 1546-198X SN - 1546-1971 VL - 9 IS - 2 SP - 662 EP - 664 PB - American Scientific Publishers (ASP) CY - Stevenson Ranch, CA, USA AN - OPUS4-24504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rouquerol, J. A1 - Baron, G. A1 - Denoyel, R. A1 - Giesche, H. A1 - Groen, J. A1 - Klobes, Peter A1 - Levitz, P. A1 - Neimark, A.V. A1 - Rigby, S. A1 - Skudas, R. A1 - Sing, K. A1 - Thommes, M. A1 - Unger, K. T1 - Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC technical report) N2 - This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 µm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion–extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed and evaluated. The reliability of mercury porosimetry is discussed in the first part of the report along with the conditions required for its safe use. Other procedures for macropore size analysis, which are critically examined, include the intrusion of other non-wetting liquids and certain wetting liquids, capillary condensation, liquid permeation, imaging, and image analysis. The statistical reconstruction of porous materials and the use of macroporous reference materials (RMs) are also examined. Finally, the future of macropore analysis is discussed. KW - Capillary condensation KW - Image analysis KW - IUPAC physical and biophysical chemistry division KW - Liquid intrusion KW - Macroporous materials KW - Mercury prorsimetry KW - Permeation KW - Pore size characterization KW - Reference porous materials KW - Statistical reconstruction of porous solids PY - 2012 DO - https://doi.org/10.1351/PAC-REP-10-11-19 SN - 0033-4545 SN - 1365-3075 VL - 84 IS - 1 SP - 107 EP - 136 PB - Union CY - Research Triangle Park, NC AN - OPUS4-26109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, R. A1 - Vaishampayan, A. A1 - Cuellar-Camacho, J. L. A1 - Wight, D. J. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Grohmann, E. A1 - Haag, R. A1 - Wagner, O. T1 - Multivalent Bacteria Binding by Flexible Polycationic Microsheets Matching Their Surface Charge Density N2 - Aiming at the overall negative surface charge of bacteria, a new strategy of antibacterial agents based on large polymer-modified graphene oxide (GO) sheets is assessed. The presented flexible, polycationic Sheets match the size and charge density of the Escherichia coli surface charge density (2 × 1014 cm−2). These matching parameters create an unspecific but very strong bacteria adsorber by multivalent, electrostatic attraction. Their interaction with bacteria is visualized via atomic force and confocal microscopy and shows that they effectively bind and wrap around E. coli cells, and thereby immobilize them. The incubation of Gram-negative and -positive bacteria (E. coli and methicillin-resistant Staphylococcus aureus, MRSA) with these polycationic sheets leads to the inhibition of proliferation and a reduction of the colony forming bacteria over time. This new type of antibacterial agent acts in a different mode of Action than classical biocides and could potentially be employed in medicinal, technical, or agriculture applications. The presented microsheets and their unspecific binding of cell interfaces could further be employed as adsorber material for bacterial filtration or immobilization for imaging, analysis, or sensor technologies. KW - Surface charge KW - Bacteria KW - Graphene oxide KW - Escherichia coli KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509651 DO - https://doi.org/10.1002/admi.201902066 VL - 7 IS - 15 SP - 1902066 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K.J. A1 - Jang, J. S. A1 - Kim, A. S. A1 - Suh, J.K. A1 - Chung, Y.-D. A1 - Hodoroaba, Vasile-Dan A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Kang, H. J. A1 - Popov, O. A1 - Popov, I. A1 - Kuselman, I. A1 - Lee, Y. H. A1 - Sykes, D. E. A1 - Wang, M. A1 - Wang, H. A1 - Ogiwara, T. A1 - Nishio, M. A1 - Tanuma, S. A1 - Simons, D. A1 - Szakal, C. A1 - Osborn, W. A1 - Terauchi, S. A1 - Ito, M. A1 - Kurokawa, A. A1 - Fujiimoto, T. A1 - Jordaan, W. A1 - Jeong, C. S. A1 - Havelund, R. A1 - Spencer, S. A1 - Shard, A. A1 - Streeck, C. A1 - Beckhoff, B. A1 - Eicke, A. A1 - Terborg, R. T1 - CCQM pilot study P-140: Quantitative surface analysis of multi-element alloy films N2 - A pilot study for the quantitative surface analysis of multi-element alloy films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this pilot study is to ensure the equivalency in the measurement capability of national metrology institutes for the quantification of multi-element alloy films. A Cu(In,Ga)Se2 (CIGS) film with non-uniform depth distribution was chosen as a representative multi-element alloy film. The atomic fractions of the reference and the test CIGS films were certified by isotope dilution - inductively coupled plasma/mass spectrometry. A total number counting (TNC) method was used as a method to determine the signal intensities of the constituent elements, which are compared with their certified atomic fractions. The atomic fractions of the CIGS films were measured by various methods, such as Secondary Ion Mass Spectrometry (SIMS), Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), X-Ray Fluorescence (XRF) analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). Fifteen laboratories from eight National Metrology Institutes (NMIs), one Designated Institute (DI) and six non-NMIs participated in this pilot study. Although the average atomic fractions of 18 data sets showed rather poor relative standard deviations of about 5.5 % to 6.8 %, they were greatly improved to about 1.5 % to 2.2 % by excluding 5 strongly deviating data sets from the average atomic fractions. In this pilot study, the average expanded uncertainties of SIMS, XPS, AES, XRF and EPMA were 3.84%, 3.68%, 3.81%, 2.88% and 2.90%, respectively. These values are much better than those in the key comparison K-67 for composition of a Fe-Ni alloy film. As a result, the quantification of CIGS films using the TNC method was found to be a good candidate as a subject for a CCQM key comparison. KW - CCQM KW - Pilot study KW - Surface analysis KW - Alloy films KW - CIGS PY - 2015 DO - https://doi.org/10.1088/0026-1394/52/1A/08017 SN - 0026-1394 SN - 1681-7575 VL - 52 IS - Technical Supplement SP - Article 08017 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-35306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzweber, Markus A1 - Lippitz, Andreas A1 - Hesse, R. A1 - Denecke, R. A1 - Werner, W. A1 - Unger, Wolfgang T1 - The use of ionic liquids for the determination of the spectrometer transmission function in X-ray photoelectron spectroscopy (XPS) N2 - The uncertainty of measurement in quantitative XPS analysis can be reduced by using a calibrated spectrometer transmission function T (E), which is usually determined by taking spectra from Au, Ag, Cu and Ge elemental reference materials. However, this approach is quite time-consuming due to required sample preparation steps like sputter cleaning etc., and the relatively big number of samples to be measured. This contribution proposes the use of the ionic liquids [C2C1im][NTf2] and [C3C1im][NTf2] as reference materials for a determination of T(E). These multi-elemental samples deliver five intensive photoemission peaks, F 1s, O 1s, N 1s, C 1s and S 2p, in an energy window from 160 eV to 700 eV which is of specific interest for applications of quantitative XPS for surface chemical analysis of soft matter, one of the major applications of XPS. KW - Quantitative XPS KW - Ionic liquid KW - Transmission function PY - 2019 DO - https://doi.org/10.1016/j.elspec.2019.03.008 VL - 233 SP - 51 EP - 56 PB - Elsevier B.V. AN - OPUS4-48019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, R. A1 - Braun, Ulrike A1 - Fankhänel, J. A1 - Daum, B. A1 - Arash, B. A1 - Rolfes, R. T1 - Molecular modelling of epoxy resin crosslinking experimentally validated by near-infrared spectroscopy N2 - Reliable simulation of polymers on an atomistic length scale requires a realistic representation of the cured material. A molecular modelling method for the curing of epoxy systems is presented, which is developed with respect to efficiency while maintaining a well equilibrated system. The main criterion for bond formation is the distance between reactive groups and no specific reaction probability is prescribed. The molecular modelling is studied for three different mixing ratios with respect to the curing evolution of reactive Groups and the final curing stage. For the first time, the evolution of reactive groups during the curing process predicted by the molecular modelling is validated with near-infrared spectroscopy data, showing a good agreement between simulation results and experimental measurements. With the proposed method, deeper insights into the curing mechanism of epoxy systems can be gained and it allows us to provide reliable input data for molecular Dynamics simulations of material properties. KW - Epoxy KW - NIR spectroscopy KW - Modelling PY - 2019 DO - https://doi.org/10.1016/j.commatsci.2019.01.054 SN - 0927-0256 VL - 161 SP - 223 EP - 235 PB - Elsevier AN - OPUS4-47431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tu, Z. A1 - Donskyi, Ievgen A1 - Qiao, H. A1 - Zhu, Z. A1 - Unger, Wolfgang A1 - Hackenberger, C. P. R. A1 - Chen, W. A1 - Adeli, M. A1 - Haag, R. T1 - Graphene Oxide-Cyclic R10 Peptide Nuclear Translocation Nanoplatforms for the Surmounting of Multiple-Drug Resistance N2 - Multidrug resistance resulting from a variety of defensive pathways in Cancer has become a global concern with a considerable impact on the mortality associated with the failure of traditional chemotherapy. Therefore, further research and new therapies are required to overcome this challenge. In this work, a cyclic R10 peptide (cR10) is conjugated to polyglycerol-covered nanographene oxide to engineer a nanoplatform for the surmounting of multidrug resistance. The nuclear translocation of the nanoplatform, facilitated by cR10 peptide, and subsequently, a laser-triggered release of the loaded doxorubicin result in efficient anticancer activity confirmed by both in vitro and in vivo experiments. The synthesized nanoplatform with a combination of different features, including active nucleus-targeting, highloading capacity, controlled release of cargo, and photothermal property, provides a new strategy for circumventing multidrug resistant cancers. KW - Graphen Oxide KW - Nanoplatform KW - Cancer PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510061 DO - https://doi.org/10.1002/adfm.202000933 VL - 30 IS - 35 SP - 2000933 PB - Wiley VCH AN - OPUS4-51006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leach, R.K. A1 - Boyd, R. A1 - Burke, T. A1 - Danzebrink, H.-U. A1 - Dirscherl, K. A1 - Dziomba, T. A1 - Gee, M. A1 - Koenders, L. A1 - Morazzani, V. A1 - Pidduck, A. A1 - Roy, D. A1 - Unger, Wolfgang A1 - Yacoot, A. T1 - The European nanometrology landscape N2 - This review paper summarizes the European nanometrology landscape from a technical perspective. Dimensional and chemical nanometrology are discussed first as they underpin many of the developments in other areas of nanometrology. Applications for the measurement of thin film parameters are followed by two of the most widely relevant families of functional properties: measurement of mechanical and electrical properties at the nanoscale. Nanostructured materials and surfaces, which are seen as key materials areas having specific metrology challenges, are covered next. The final section describes biological nanometrology, which is perhaps the most interdisciplinary applications area, and presents unique challenges. Within each area, a review is provided of current status, the capabilities and limitations of current techniques and instruments, and future directions being driven by emerging industrial measurement requirements. Issues of traceability, standardization, national and international programmes, regulation and skills development will be discussed in a future paper. KW - Nanotechnology KW - Metrology KW - Chemistry KW - Surface analysis PY - 2011 DO - https://doi.org/10.1088/0957-4484/22/6/062001 SN - 0957-4484 SN - 1361-6528 VL - 22 IS - 6 SP - 062001-1 - 062001-15 PB - IOP Publishing Ltd. CY - Bristol AN - OPUS4-23259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Pelster, A. A1 - Tyler, B.J. A1 - Kösgen, M. A1 - Kassenböhmer, R. A1 - Peterson, R.E. A1 - Stöver, M. A1 - Arlinghaus, H. F. T1 - Improved 3D-imaging of a sirolimus/probucol eluting stent coating using laser postionization secondary neutral mass spectrometry and time-of-flight secondary ion mass spectrometry N2 - Implantable drug delivery systems that provide controlled and sustained release of a therapeutic agent are used in a wide variety of applications. Drug eluting stents, which are used to treat coronary artery disease, are among the most widespread of these devices, with an estimated 3x10⁶ implants annually worldwide. Controlling the rate of drug release from these devices relies on precise control of the three dimensional (3D)-distribution of the drug, so methods for measuring this distribution are of great importance. The aims of this work were to determine how 3D-imaging of polymer-free sirolimus/probucol drug eluting stent coatings could be improved through the use of laser postionization secondary neutral mass spectrometry (Laser- SNMS) and Ar cluster sputtering with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and to optimize conditions for this analysis. In this study, 3D-imaging of a sirolimus/probucol dual drug eluting stent has been investigated using Laser-SNMS and ToF-SIMS. Laser-SNMS studies of pure sirolimus and probucol were undertaken using 30 keV Bi₃⁺ primary Ions and a 157 nm excimer postionization laser. Under optimal conditions, a greater than 100-fold increase in detected ion yield was observed for Laser-SNMS when compared to ToF-SIMS, although ToF-SIMS provided equal or greater yields for higher mass characteristic ions. Although the optimal laser power density for detecting probucol (5x10⁶W/cm²) was significantly lower than the optimum for sirolimus(7x10⁷W/cm²), an intermediate laser power density of 1x10⁷W/cm² was sufficient to allow imaging of both drugs. Using individual selected ion signals, ToF-SIMS and Laser-SNMS produced similar images of the two drug species. When using, however, a multivariate approach (Maximum autocorrelation factors), Laser-SNMS provided significant improvements in image contrast and small area detection when compared to ToF-SIMS. Following optimization of the technique, 3D-images of the dual drug eluting stent coating were obtained using 10 keV Ar₂₀₀₀⁺ cluster ions for sputtering and 30 keV Bi₃⁺ cluster ions for Analysis for both ToF-SIMS and Laser-SNMS. This work demonstrates the advantages of Laser-SNMS for 3D-imaging of pharmaceutical devices, which has not been previously published. Both ToF-SIMS and Laser-SNMS revealed that the outermost surface of the drug eluting coating contained pure sirolimus to a depth of a few tens of nanometers, with a few channels of sirolimus extending to a depth of around 1 lm. Below about 1 lm, the two drugs were uniformly mixed. Using the 10 keV Ar₂₀₀₀⁺ sputter beam, the authors were able to sputter through the complete drug coating (~6 μm) without observing any accumulated damage in the organic layer. The two techniques showed complementary strengths: ToF-SIMS offers faster data collection and better detected ion yield for larger characteristic ions than Laser-SNMS, and Laser-SNMS offers significantly enhanced detected ion yield for smaller fragment ions, allowing for improved Image contrast and Resolution of smaller features. KW - Imaging ToF SIMS KW - Eluting stent PY - 2016 DO - https://doi.org/10.1116/1.4964687 SN - 1934-8630 SN - 1559-4106 VL - 11 IS - 4 SP - 041001-1 EP - 041001-10 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-38272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kasper, J. A1 - Hermanns, M.I. A1 - Bantz, C. A1 - Koshkina, Olga A1 - Lang, Thomas A1 - Maskos, Michael A1 - Pohl, C. A1 - Unger, R. E. A1 - Kirkpatrick, C.J. T1 - Interactions of silica nanoparticles with lung epithelial cells and the association to flotillins N2 - Amorphous silica nanoparticles (aSNPs) gain increasing popularity for industrial and therapeutic claims. The lung with its surface area of 1006#8211;140 m² displays an ideal target for therapeutic approaches, but it represents also a serious area of attack for harmful nanomaterials. The exact nature of the cytotoxic effects of NPs is still unknown. Furthermore, cellular pathways and the destiny of internalized NPs are still poorly understood. Therefore, we examined the cytotoxicity (MTS, LDH) and inflammatory responses (IL-8) for different-sized aSNPs (30, 70, 300 nm) on our lung epithelial cells line NCI H441 and endothelial cell line ISO-HAS-1. Additionally, colocalization studies have been conducted via immunofluorescence staining for flotillin-1- and flotillin-2-bearing endocytic vesicles. Subsequently, the relevance of flotillins concerning the viability of aSNP-exposed epithelial cells has been evaluated using flotillin-1/2 depleted cells (siRNA). This study reveals the relevance of the nanoparticle size regarding cytotoxicity (MTS, LDH) and inflammatory responses (IL-8), whereat the smaller the size of the nanoparticle is, the more harmful are the effects. All different aSNP sizes have been incorporated in flotillin-1- and flotillin-2-labelled vesicles in lung epithelial and endothelial cells, which display a marker for late endosomal or lysosomal structures and appear to exhibit a clathrin- or caveolae-independent mode of endocytosis. Flotillin-depleted H441 showed a clearly decreased uptake of aSNPs. Additionally, the viability of aSNP-exposed cells was reduced in these cells. These findings indicate a contribution of flotillins in as yet unknown (clathrin or caveolae-independent) endocytosis mechanisms and (or) endosomal storage. KW - Silica nanoparticles KW - Alveolar-capillary barrier KW - Lung epithelial cells KW - Endothelial cells KW - Endocytosis KW - Flotillin-1 KW - Flotillin-2 KW - Cytotoxicity KW - Inflammatory response PY - 2012 UR - http://link.springer.com/content/pdf/10.1007%2Fs00204-012-0876-5 DO - https://doi.org/10.1007/s00204-012-0876-5 SN - 0340-5761 SN - 1432-0738 SP - 1 EP - 13(?) PB - Springer CY - Berlin ; Heidelberg [u.a.] AN - OPUS4-26195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kasper, J. A1 - Herrmanns, M.I. A1 - Bantz, C. A1 - Utech, S. A1 - Koshkina, Olga A1 - Maskos, Michael A1 - Brochhausen, C. A1 - Pohl, C. A1 - Fuchs, S. A1 - Unger, R. E. A1 - Kirkpatrick, C.J. T1 - Flotillin-involved uptake of silica nanoparticles and responses of an alveolar-capillary barrier in vitro N2 - Drug and gene delivery via nanoparticles across biological barriers such as the alveolar-capillary barrier of the lung constitutes an interesting and increasingly relevant field in nanomedicine. Nevertheless, potential hazardous effects of nanoparticles (NPs) as well as their cellular and systemic fate should be thoroughly examined. Hence, this study was designed to evaluate the effects of amorphous silica NPs (Sicastar) and (poly)organosiloxane NPs (AmOrSil) on the viability and the inflammatory response as well as on the cellular uptake mechanisms and fate in cells of the alveolar barrier. For this purpose, the alveolar epithelial cell line (NCI H441) and microvascular endothelial cell line (ISO-HAS-1) were used in an experimental set up resembling the alveolar-capillary barrier of the lung. In terms of IL-8 and sICAM Sicastar resulted in harmful effects at higher concentrations (60 µg/ml) in conventional monocultures but not in the coculture, whereas AmOrSil showed no significant effects. Immunofluorescence counterstaining of endosomal structures in NP-incubated cells showed no evidence for a clathrin- or caveolae-mediated uptake mechanism. However, NPs were enclosed in flotillin-1 and -2 marked vesicles in both cell types. Flotillins appear to play a role in cellular uptake or trafficking mechanisms of NPs and are discussed as indicators for clathrin- or caveolae-independent uptake mechanisms. In addition, we examined the transport of NPs across this in vitro model of the alveolar-capillary barrier forming a tight barrier with a transepithelial electrical resistance of 560 ± 8 Ω cm². H441 in coculture with endothelial cells took up much less NPs compared to monocultures. Moreover, coculturing prevented the transport of NP from the epithelial compartment to the endothelial layer on the bottom of the filter insert. This supports the relevance of coculture models, which favour a differentiated and polarised epithelial layer as in vitro test systems for nanoparticle uptake. KW - Silica nanoparticles KW - Alveolar-capillary barrier KW - NP uptake KW - NP-transport KW - Endocytosis KW - Flotillin-1/-2-dependent uptake/trafficking PY - 2013 DO - https://doi.org/10.1016/j.ejpb.2012.10.011 SN - 0939-6411 SN - 1873-3441 VL - 84 IS - 2 SP - 275 EP - 287 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-28841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Horlacher, T. A1 - Girard-Lauriault, Pierre-Luc A1 - Gross, Thomas A1 - Lippitz, Andreas A1 - Min, Hyegeun A1 - Wirth, Thomas A1 - Castelli, R. A1 - Seeberger, P. A1 - Unger, Wolfgang T1 - Multimethod chemical characterization of carbohydrate-functionalized surfaces N2 - A combined XPS, NEXAFS, and ToF-SIMS chemical surface characterization of carbohydrate-functionalized gold and glass surfaces is presented. Spot shape and chemical composition across a spot surface are provided by surface-sensitive methods as ToF-SIMS and XPS, used in their imaging modes. Moreover, the feasibility of this multimethod approach to control relevant production steps of a carbohydrate microarray prototype is demonstrated. KW - Carbohydrates KW - Microarrays KW - Self-assembled monolayers KW - XPS KW - NEXAFS KW - ToF-SIMS PY - 2011 DO - https://doi.org/10.1080/07328303.2011.615181 SN - 0732-8303 VL - 30 IS - 4-6 SP - 361 EP - 372 PB - Taylor & Francis CY - London [u.a.] AN - OPUS4-24874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Girard-Lauriault, Pierre-Luc A1 - Illgen, René A1 - Ruiz, J.-C. A1 - Wertheimer, M. R. A1 - Unger, Wolfgang T1 - Surface functionalization of graphite and carbon nanotubes by vacuum-ultraviolet photochemical reactions N2 - Graphite and multiwall carbon nanotube surfaces were functionalized by vacuum-ultraviolet induced photochemistry in NH3 or O2, in order to introduce amino- (NH2) or hydroxyl (OH) functionalities, respectively. Modified surfaces were characterized by X-ray photoelectron spectroscopy (XPS), which showed significant incorporation of nitrogen (N) and oxygen (O) at the materials’ surface. While high-resolution XP spectra did not yield much specific information about the incorporated functional groups, chemical derivatization with 4-trifluoromethyl benzaldehyde and trifluoroacetic anhydride accompanied by XPS enabled quantification of NH2 and OH groups, respectively. Using near edge X-ray absorption fine structure spectroscopy, we assessed the conservation of the aromatic structure following functionalization treatments. KW - Carbon nanotubes KW - Graphite KW - Vacuum ultraviolet photochemistry KW - Surface functionalization KW - Amino groups KW - Hydroxyl KW - Derivatization PY - 2012 DO - https://doi.org/10.1016/j.apsusc.2012.03.012 SN - 0169-4332 SN - 1873-5584 VL - 258 IS - 22 SP - 8448 EP - 8454 PB - North-Holland CY - Amsterdam AN - OPUS4-26233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Girard-Lauriault, P.-L. A1 - Wertheimer, M. R. A1 - Lippitz, Andreas A1 - Unger, Wolfgang T1 - NEXAFS Surface Chemical Characterisation of Atmospheric Pressure deposited N-rich Plasma-Polymer Films for Tissue Engineering KW - Synchrotron KW - NEXAFS KW - Plasma-Polymer KW - Tissue Engineering PY - 2007 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annual_report_2006.pdf#page=248 SN - 0179-4159 SP - 248 EP - 250 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-17453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Truica-Marasescu, F. A1 - Girard-Lauriault, P.-L. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Wertheimer, M. R. T1 - Nitrogen-rich plasma polymers: Comparison of films deposited in atmospheric- and low-pressure plasmas N2 - Low- and atmospheric-pressure plasma co-polymerisations of binary gas mixtures of C2H4 and NH3 or N2, respectively, were investigated for depositing N-rich plasma polymer coatings for biomedical applications. Deposition kinetics and relevant surface characteristics of resulting plasma polymerised ethylene enriched with nitrogen, “PPE:N”, coatings were investigated as a function of the gas mixture ratio, X = NH3(N2)/C2H4. Physico-chemical properties of the coatings were determined using a combination of complementary surface-sensitive techniques: for example, total nitrogen concentrations, [N], up to 40 at.% were measured by X-ray Photoelectron Spectroscopy, XPS, while those of primary amines, [–NH2], were determined by performing chemical derivatisation followed by XPS analyses. PPE:N films were further characterised by UV–VIS Ellipsometry, Near Edge X-ray Absorption Fine Structure Spectroscopy, IR Spectroscopy and by Contact Angle Goniometry measurements. The stability of the coatings was tested, both in terms of water solubility and of “ageing” in ambient atmosphere. For the latter, selected samples were stored in the laboratory for different durations, in order to assess possible changes in their chemical structures. KW - Aging KW - Deposition process KW - Ethylene KW - Fourier transform infrared spectroscopy (FTIR) KW - Glow discharge KW - Plasma polymers KW - Surface chemistry KW - Surface energy PY - 2008 DO - https://doi.org/10.1016/j.tsf.2008.02.033 SN - 0040-6090 VL - 516 IS - 21 SP - 7406 EP - 7417 PB - Elsevier CY - Amsterdam AN - OPUS4-18279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Senoner, Mathias A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Österle, Werner A1 - Kaiander, I. A1 - Sellin, R. L. A1 - Bimberg, D. ED - Wilkening, G. ED - Koenders, L. T1 - Testing the Lateral Resolution in the Nanometre Range with a New Type of Certified Reference Material T2 - NanoScale 2004 Seminar ; 6th Seminar on Quantitative Microscopy ; 2nd Seminar on Nanoscale Calibration Standards and Methods CY - Braunschweig, Germany DA - 2004-03-25 KW - Laterale Auflösung KW - Nanometrologie KW - Nanotechnologie KW - Oberflächenanalytik KW - Zertifiziertes Referenzmaterial PY - 2004 SN - 3-527-40502-X DO - https://doi.org/10.1002/3527606661.ch21 SP - 282 EP - 294 PB - Wiley-VCH CY - Weinheim AN - OPUS4-7541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Girard-Lauriault, P.-L. A1 - Desjardins, P. A1 - Unger, Wolfgang A1 - Lippitz, Andreas A1 - Wertheimer, M. R. T1 - Chemical characterisation of nitrogen-rich plasma-polymer films deposited in dielectric barrier discharges at atmospheric pressure N2 - We have used an atmospheric pressure DBD apparatus to deposit novel families of N-rich plasma polymers (PP:N), using mixtures of three different hydrocarbon precursors in nitrogen at varying respective gas flow ratios. This research focuses on the overall chemical characterisation of those materials, with specific attention to (semi)-quantitative analysis of functional groups. Well-established and some lesser-known analytical techniques have been combined to provide the best possible chemical and structural characterisations of these three families of PP:N thin films, namely XPS, NEXAFS and FT-IR spectroscopy. KW - NEXAFS KW - XPS KW - DBD-plasma KW - Plasma polymerization PY - 2008 DO - https://doi.org/10.1002/ppap.200800054 SN - 1612-8850 SN - 1612-8869 VL - 5 IS - 7 SP - 631 EP - 644 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-17820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -