TY - JOUR A1 - Baer, Wolfram A1 - Wossidlo, Peter T1 - Validation of a low blow specimen technique for R-curve determination using a drop tower N2 - Fracture mechanics based component design requires appropriate fracture mechanics toughness data with respect to both, loading rate as well as test temperature. Taking high-rate loading into account such as with accidental scenarios, different standards such as ASTM E 1820 or BS 7448-3 provide some information on dynamic fracture mechanics testing. Nevertheless, the designations differ so that a validation of the own material specific test method used for dynamic R-curve determination is mandatory. In order to address this for ductile cast iron materials an experimental method for the reliable determination of dynamic J-integral crack resistance curves at -40 °C following the multiple specimen approach has been established and validated. The experimental concept offers some additional valuable features. Single values of dynamic crack initiation toughness can be determined using a single specimen technique based on crack sensors. Furthermore, an experimentally independent method is provided according to which CTOD δ5 R-curves can be established. The focus of the present paper is on the validation of the experimental low blow technique using a drop tower test system. A drop tower test system was developed and set up to perform low blow tests at temperatures down to -40 °C. The system allows for a variation of the impact mass and height and was optimized for testing of ductile cast iron at stress intensity rates from approximately 5∙10⁴ to 3∙10⁵ MPa√ms⁻¹. This range of loading rate is characteristic for instance with crash scenarios of heavy sectioned DCI casks for radioactive materials. In order to address characteristic challenges of impact tests (test duration of microseconds up to milliseconds, inertial effects, signal oscillations), an appropriate full bridge strain gage method for the measurement of force directly on the specimen as well as a non-contact measurement of load line displacement using an optical extensometer have been developed and validated. The low blow test requires either to prevent bouncing strikes of the hammer by using the stop block technique or to catch the hammer after its first strike. Both options are not part of the experimental concept and setup which have been realized here. The paper describes investigations which have been performed in order to make sure that bouncing strikes of the hammer do not cause additional crack extension in the specimen. This is necessary to ensure a unique relation between the work done and the achieved crack extension. The investigations covered the analysis of limit loads of the specimen with respect to the measured force. The measured stiffness of the specimen was assessed and signals of crack sensors were analyzed. Furthermore, an analysis of the mechanical behavior of the loading system and the specimen by optical observation was performed. Corresponding results are discussed in the paper. It had finally been proven that additional crack extension in the specimen due to bouncing strikes of the hammer is not to be expected under the given conditions of test setup, material and loading. It can be seen as a major experimental advantage that the striker does not have to be catched after the low blow test. T2 - XXIV Italian Group of Fracture Conference CY - Urbino, Italy DA - 01.03.2017 KW - Dynamic fracture mechanics KW - R-curve KW - Low blow KW - Ductile cast iron PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-437686 DO - https://doi.org/10.1016/j.prostr.2017.04.005 SN - 2452-3216 VL - 3 SP - 25 EP - 32 AN - OPUS4-43768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Göbenli, G. A1 - Eggeler, G. ED - Göken, M. T1 - Transmission electron microscopy study of the microstructural evolution during high-temperature and low-stress (011) [01-1] shear creep deformation of the superalloy single crystal LEK 94 N2 - The present work describes the shear creep behavior of the superalloy LEK 94 at temperatures between 980 and 1050 °C and shear stresses between 50 and 140 MPa for loading on the macroscopic crystallographic shear system (MCSS) (011)[01-1]. The strain rate versus strain curves show short primary and extended secondary creep regimes. We find an apparent activation energy for creep of Qapp = 466 kJ/mol and a Norton-law stress exponent of n = 6. With scanning transmission electron microscopy, we characterize three material states that differ in temperature, applied stress, and accumulated strain/time. Rafting develops perpendicular to the maximum principal stress direction, gamma channels fill with dislocations, superdislocations cut gamma' particles, and dislocation networks form at gamma/gamma' interfaces. Our findings are in agreement with previous results for high-temperature and low-stress [001] and [110] tensile creep testing, and for shear creep testing of the superalloys CMSX-4 and CMSX-6 on the MCSSs (111)[01-1] and (001)[100]. The parameters that characterize the evolving gamma/gamma' microstructure and the evolving dislocation substructures depend on creep temperature, stress, strain, and time. KW - Dislocations KW - Microstructure KW - Scanning transmission electron microscopy (STEM) KW - Creep KW - Shear test PY - 2017 DO - https://doi.org/10.1557/jmr.2017.336 SN - 0884-2914 SN - 2044-5326 VL - 32 IS - 24 SP - 4491 EP - 4502 PB - Cambridge University Press CY - Cambrigde AN - OPUS4-43756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Revealing hidden spectral information of chlorine and sulfur in data of a mobile Laser-induced Breakdown Spectroscopy system using chemometrics N2 - For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation. KW - LIBS KW - Chemometrics KW - Building materials PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.04.001 SN - 0584-8547 VL - 132 SP - 43 EP - 49 PB - Elsevier B.V. AN - OPUS4-40066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weltschev, Margit T1 - Auswahl eines Kennwertes für den Vergleich des mechanischen Leistungsniveaus von Polyethylenformstoffen für Gefahrgutverpackungen T1 - Parameter selection for the comparison of the mechanical level of performance of polyethylene molding materials for packagings of dangerous goods N2 - Zum Vergleich der Polyethylenformstoffe für eine Bauart von Gefahrgutverpackungen und IBC wurden die Materialkennwerte: Schmelze-Massefließrate MFR, Dichte D, Kerbschlag-zähigkeit acN bei -30 °C, Spannungsrissbeständigkeit (bestimmt mit dem Full Notch Creep Test) und Beständigkeit gegen oxidativen Abbau Ox (bestimmt durch den prozentualen Anstieg des MFR in Salpetersäure) in der DIN EN 15507 – Verpackung – Verpackungen zur Beförderung gefährlicher Güter – Vergleichende Werkstoffprüfung von Polyethylensorten ausgewählt. Das Ziel der Untersuchungen war die Auswahl eines Kennwertes für die Bestimmung des mechanischen Leistungsniveaus von Polyethylenformstoffen, da unter Druck Verpackungen beulen oder knicken. Zur Auswahl standen drei Prüfverfahren: a) Bestimmung der Biegesteifigkeit S nach DIN 53 350 (Prinzip von Ohlsen). b) Bestimmung der Biegefestigkeit σfM und Biegedehnung ɛfM nach DIN EN ISO 178 c) Bestimmung der Druckkraft Fmax und Verformung dL bei Fmax nach DIN EN ISO 604. Die Prüfmethode zur Bestimmung der Biegesteifigkeit nach DIN 53 350 eignet sich zum Vergleich des mechanischen Leistungsniveaus der Formstoffe. Zur Verbesserung der Reproduzierbarkeit der Ergebnisse sollte der Skalierungsbereich der Prüfapparatur erweitert wer-den, um genauere Messergebnisse zu erzielen. Der Dreipunktbiegeversuch nach DIN EN ISO 178 eignet sich bei verformungsfähigen Kunststoffen, wie dem Polyethylen, zur Bestimmung der Biegefestigkeit σfM. Dieser Ver-such besitzt den Nachteil, dass am Ort des maximalen Biegemoments in der Randschicht, wo auch die maximale Biegespannung erzeugt wird, zusätzlich der Biegestempel angreift. Die Messergebnisse haben gezeigt, dass die Druckprüfung nach DIN EN ISO 604 sich sehr gut zur Bewertung des mechanischen Verhaltens der Polyethylenformstoffe unter Druckbelastung (Stapeldruckprüfung der Verpackungen) eignet. KW - Gefahrgutverpackung KW - Polyethylen KW - Biegesteifigkeit KW - Biegefestigkeit KW - Druckkraft PY - 2017 DO - https://doi.org/10.3139/120.111025 SN - 0025-5300 VL - 59 IS - 5 SP - 466 EP - 471 PB - Carl Hanser Verlag GmbH & Co.KG CY - München AN - OPUS4-40145 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Joester, Maike A1 - Seifert, Stephan A1 - Emmerling, Franziska A1 - Kneipp, Janina T1 - Physiological influence of silica on germinating pollen as shown by Raman spectroscopy N2 - The process of silicification in plants and the biochemical effects of silica in plant tissues are largely unknown. To study the molecular changes occurring in growing cells that are exposed to higher than normal concentration of silicic acid, Raman spectra of germinating pollen grains of three species (Pinus nigra, Picea omorika, and Camellia japonica) were analyzed in a multivariate classification approach that takes into account the variation of biochemical composition due to species, plant tissue structure, and germination condition. The results of principal component analyses of the Raman spectra indicate differences in the utilization of stored lipids, a changed mobilization of storage carbohydrates in the pollen grain bodies, and altered composition and/or structure of cellulose of the developing pollen tube cell walls. These biochemical changes vary in the different species. KW - Silica KW - Raman spectroscopy KW - Principal component analysis PY - 2017 DO - https://doi.org/10.1002/jbio.201600011 SN - 1864-063X SN - 1864-0648 VL - 10 IS - 4 SP - 542 EP - 552 AN - OPUS4-40090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, P. A1 - Bogart, L.K. A1 - Posth, O. A1 - Szczerba, Wojciech A1 - Rogers, S.E. A1 - Castro, A. A1 - Nilsson, L. A1 - Zeng, L. J. A1 - Sugunan, A. A1 - Sommertune, J. A1 - Fornara, A. A1 - Gonzales-Alonso, D. A1 - Fernandez Barquin, L. A1 - Johansson, C. T1 - Structural and magnetic properties of multi-core nanoparticles analysed using a generalised numerical inversion method N2 - The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions. KW - Numerical inversion KW - Magnetic nanoparticles KW - Iron oxides KW - Magnetic properties KW - Structural properties PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400952 DO - https://doi.org/10.1038/srep45990 SN - 2045-2322 VL - 7 SP - Article 45990, 1 EP - 14 AN - OPUS4-40095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, A.C.P. A1 - Österle, Werner A1 - Gradt, Thomas A1 - Azevedo, César Roberto de Farias T1 - Impact of copper nanoparticles on tribofilm formation determined by pin-on-disc tests with powder supply: Addition of artificial third body consisting of Fe3O4, Cu and graphite N2 - Copper, magnetite and graphite particles were mixed in order to observe their impact on the coefficient of friction (CoF) during pin-on-disc tests and on the tribofilm formation after testing. Pure magnetite powder provided a value of CoF of 0.4. Magnetite-copper mixtures tested at 400 °C revealed lower CoF values (~0.4) than those at room temperature (~0.6). Magnetite-graphite and magnetite-graphite-copper mixtures presented lower CoF values (~0.3). All systems formed a magnetite-based tribofilm and patches of metallic copper were found on the tribosurfaces of the mixtures containing copper. Carbon layers and graphite nanoinclusions were observed in the graphite mixtures. The incorporation of zirconia particles, a by-product of ball milling mixing, prevented the selective transfer of graphite and copper to the tribosurfaces of some of the samples. KW - Brake pad materials KW - Sliding friction KW - Transfer layer KW - Surface analysis KW - Model friction tests PY - 2017 DO - https://doi.org/10.1016/j.triboint.2017.02.014 SN - 0301-679X VL - 110 SP - 103 EP - 112 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-40104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Joseph, A. A1 - Bernardes, C. E. S. A1 - Druzhinina, A. I. A1 - Varushchenko, R. M. A1 - Nguyen, Thi Yen A1 - Emmerling, Franziska A1 - Yuan, L. A1 - Dupray, V. A1 - Coquerel, G. A1 - Minas da Piedade, M. E. T1 - Polymorphic phase transition in 4′-hydroxyacetophenone: Equilibrium temperature, kinetic barrier, and the relative stability of Z′=1 and Z′=2 forms N2 - Particularly relevant in the context of polymorphism is understanding how structural, thermodynamic, and kinetic factors dictate the stability domains of polymorphs, their tendency to interconvert through phase transitions, or their possibility to exist in metastable states. These three aspects were investigated here for two 4′-hydroxyacetophenone (HAP) polymorphs, differing in crystal system, space group, and number and conformation of molecules in the asymmetric unit. The results led to a ΔfGm°-T phase diagram highlighting the enantiotropic nature of the system and the fact that the Z′=1 polymorph is not necessarily more stable than its Z′=2 counterpart. It was also shown that the form II → form I transition is entropy driven and is likely to occur through a nucleation and growth mechanism, which does not involve intermediate phases, and is characterized by a high activation energy. Finally, although it has been noted that conflicts between hydrogen bond formation and close packing are usually behind exceptions from the hypothesis of Z′=1 forms being more stable than their higher Z′ analogues, in this case, the HAP polymorph with stronger hydrogen bonds (Z′=2) is also the one with higher density. KW - Polymorphism KW - Polymorphic transition KW - 4'-hydroxyacetophenone PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01876 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 4 SP - 1918 EP - 1932 PB - ACS AN - OPUS4-40167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Jan P. A1 - Götschel, S. A1 - Maierhofer, Christiane A1 - Weiser, M. T1 - Determining the Material Parameters for the Reconstruction of Defects in Carbon Fiber Reinforced Polymers from Data Measured by Flash Thermography N2 - Flash thermography is a fast and reliable non-destructive testing method for the investigation of defects in carbon fiber reinforced polymer (CFRP) materials. In this paper numerical simulations of transient thermography data are presented, calculated for a quasi-isotropic flat bottom hole sample. They are compared to experimental data. These simulations are one important step towards the quantitative reconstruction of a flaw by assessing thermographic data. The applied numerical model is based on the finite-element method, extended by a semi-analytical treatment of the boundary of the sample, which is heated by the flash light. A crucial part for a reliable numerical model is the prior determination of the material parameters of the specimen as well as of the experimental parameters of the set-up. The material parameters in plane and in depth diffusivity are measured using laser line excitation. In addition, the absorption and heat transfer process of the first layers is investigated using an IR microscopic lens. The performance of the two distinct components of CFRP during heating – epoxy resin and carbon fibers – is examined. Finally, the material parameters are optimized by variation and comparison of the simulation results to the experimental data. The optimized parameters are compared to the measured ones and further methods to ensure precise material parameter measurements are discussed. T2 - 43rd Review of Progress in Quantitative Nondestructive Evaluation CY - Atlanta, GA, USA DA - 17.07.2016 KW - Aktive Thermografie KW - Thermische Diffusivität KW - Zerstörungsfreie Prüfung KW - Kohlenstofffaserverstärkter Kunststoff KW - CFK KW - Active thermography KW - Thermal diffusivity KW - Non-Destructive testing KW - Carbon fiber reinforced polymer KW - CFRP PY - 2017 SN - 978-0-7354-1474-7 DO - https://doi.org/10.1063/1.4974671 SN - 0094-243X VL - 1806 IS - 1 SP - UNSP 100006-1 EP - 11 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-39332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Billing, Mark A1 - Gräfe, Christine A1 - Saal, Adrian A1 - Biehl, Philip A1 - Clement, Joachim A1 - Dutz, silvio A1 - Weidner, Steffen A1 - Schacher, Felix T1 - Zwitterionic Iron Oxide (γ-Fe2O3) Nanoparticles Based on P(2VP-grad-AA) Copolymers N2 - This study presents the synthesis and characterization of zwitterionic core–shell hybrid nanoparticles consisting of a core of iron oxide multicore nanoparticles (MCNPs, γ-Fe2O3) and a shell of sultonated poly(2-vinylpyridine-grad-acrylic acid) copolymers. The gradient copolymers are prepared by reversible addition fragmentation chain transfer polymerization of 2-vinylpyridine (2VP), followed by the addition of tert-butyl acrylate and subsequent hydrolysis. Grafting of P(2VP-grad-AA) onto MCNP results in P(2VP-grad-AA)@MCNP, followed by quaternization using 1,3-propanesultone-leading to P(2VPS-grad-AA)@MCNP with a zwitterionic shell. The resulting particles are characterized by transmission electron microscopy, dynamic light scattering, and thermogravimetric analysis measurements, showing particle diameters of ≈70–90 nm and an overall content of the copolymer shell of ≈10%. Turbidity measurements indicate increased stability toward secondary aggregation after coating if compared to the pristine MCNP and additional cytotoxicity tests do not reveal any significant influence on cell viability. KW - Blockcopolymer KW - Controlled radical polymerization KW - Hybrid nanoparticles KW - Iron oxide nanoparticles KW - Sulfobetaines PY - 2017 DO - https://doi.org/10.1002/marc.201600637 SN - 1022-1336 SN - 1521-3927 VL - 38 IS - 4 SP - 1600637-1 EP - 1600637-8 PB - Wiley-VCH AN - OPUS4-39339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babutzka, Martin A1 - Heyn, A. T1 - Dynamic tafel factor adaption for the evaluation of instantaneous corrosion rates on zinc by using gel-type electrolytes N2 - The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Gel-type electrolytes KW - Gelartige Elektrolyte KW - Zinc KW - Zink KW - Stern Geary constant KW - Stern-Geary-Konstante PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394324 UR - http://iopscience.iop.org/article/10.1088/1757-899X/181/1/012021/pdf DO - https://doi.org/10.1088/1757-899X/181/1/012021 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012021, 1 EP - 11 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Kent, B. A1 - Bertin, Annabelle T1 - Phase transition and aggregation behaviour of an UCST-type copolymer poly(acrylamide-coacrylonitrile) in water: effect of acrylonitrile content, concentration in solution, copolymer chain length and presence of electrolyte N2 - An UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its temperature-induced phase transition and aggregation behaviour studied by turbidimetry, static and dynamic light scattering, small angle neutron scattering (SANS) and cryo-transmission electron microscopy (cryo-TEM) measurements. The phase transition temperature was found to increase with increasing AN content in the copolymer, concentration of the solutions and copolymer chain length. A significant effect was observed onto the phase transition temperature by addition of different electrolytes into the copolymer solution. The copolymer chains were aggregated below the phase transition temperature and disaggregated above it. The size of the aggregates increases with increasing AN contents and concentration of the copolymer solutions below the phase transition temperature. The copolymer chains were expanded and weekly associated in solution above the phase transition temperature. A model is proposed to explain such association–aggregation behaviour of poly(AAm-co-AN) copolymers depending on AN contents and concentration of the copolymer solutions as a function of temperature. KW - Thermoresponsive polymers KW - UCST-type copolymer PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394636 DO - https://doi.org/10.1039/c6sm02262f SN - 1744-683X SN - 1744-6848 VL - 13 IS - 3 SP - 658 EP - 669 PB - RSC AN - OPUS4-39463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philippen, Jan A1 - Guguschev, Christo A1 - Klimm, Detlef ED - Kuech, Thomas F. ED - Feigelson, Robert R. ED - Nakajima, K. ED - Stringfellow, G.B. T1 - Single crystal fiber growth of cerium doped strontium yttrate, SrY2O4:Ce3+ N2 - First single crystal fibers of cerium doped Strontium yttrate were fabricated using the laser-heated pedestal growth technique. Through thermodynamic Equilibrium calculations and by high-temperature mass spectrometry suitable growth conditions could be determined. The atmosphere played an important role during crystallization. It affected the composition shift, on the one hand, and the valence state of cerium, on the other hand. These dependencies can be explained by combining X-ray diffraction, elemental analysis, and optical spectroscopy. Crystallization in slightly reducing nitrogen atmosphere proved to be a reasonable choice, because evaporation is suppressed and trivalent cerium is stabilized. Strong green emission that depends on the Oxygen fugacity during crystallization could be excited using UV light. Optical properties of SrY2O4:Ce3+ were measured for the first time. KW - Laser heated pedestal growth KW - Oxides KW - Strontium yttrate KW - Single crystal fiber KW - LED phosphors PY - 2017 DO - https://doi.org/10.1016/j.jcrysgro.2016.11.033 SN - 0022-0248 SN - 1873-5002 VL - 459 SP - 17 EP - 22 PB - Elsevier CY - Amsterdam AN - OPUS4-39496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maenz, S. A1 - Brinkmann, O. A1 - Kunisch, E. A1 - Horbert, V. A1 - Gunella, F. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Xin, L. A1 - Günster, Jens A1 - Illerhaus, Bernhard A1 - Jandt, K. D. A1 - Bossert, J. A1 - Kinne, R. W. A1 - Bungartz, M. T1 - Enhanced bone formation in sheep vertebral bodies after minimally invasive treatment with a novel, PLGA fiber-reinforced brushite cement. N2 - Injectable, brushite-forming calcium phosphate cements (CPC) show potential for bone replacement, but they exhibit low mechanical strength. This study tested a CPC reinforced with poly(l-lactide-co-glycolide) acid (PLGA) fibers in a minimally invasive, sheep lumbar vertebroplasty model. The study aimed to test the in vivo biocompatibility and osteogenic potential of a PLGA fiber-reinforced, brushite-forming CPC in a sheep large animal model. KW - µCT KW - Vertebral KW - PLGA cement PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S152994301631066X DO - https://doi.org/10.1016/j.spinee.2016.11.006 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 5 SP - 709 EP - 719 PB - Elsevier Science direct AN - OPUS4-40462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Kilinc, Y. A1 - Nadar, G. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Top-down technique for scaling to nano in silicon MEMS N2 - Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales. KW - Nanowires KW - Silicon KW - Top-down KW - MEMS PY - 2017 DO - https://doi.org/10.1116/1.4978047 SN - 1071-1023 VL - 35 IS - 2 SP - 022001-1 EP - 022001-7 PB - America Vacuum Society AN - OPUS4-39370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seuthe, T. A1 - Mermillod-Blondin, A. A1 - Grehn, M. A1 - Bonse, Jörn A1 - Wondraczek, L. A1 - Eberstein, M. T1 - Structural relaxation phenomena in silicate glasses modifed by irradiation with femtosecond laser pulses N2 - Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility. KW - Femtosecond laser KW - Silicate glasses KW - Raman spectroscopy KW - Structural relaxation KW - Refractive index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393045 DO - https://doi.org/10.1038/srep43815 SN - 2045-2322 VL - 7 SP - 43815, 1 EP - 43815, 10 PB - Nature Publishing Group CY - London, UK AN - OPUS4-39304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Lohse, V. A1 - Negendank, D. A1 - Kormunda, M. A1 - Esser, N. T1 - Thin SnOx films for surface plasmon resonance enhanced ellipsometric gas sensing (SPREE) N2 - Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept Shows promising results to solve the problems of cross sensitivity of the MOS concept. Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the Diffusion into the layer instead of adsorption on the surface. Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors. KW - Doped tin oxide KW - Ellipsometry KW - Gas sensing KW - Surface plasmon KW - Resonance KW - Thin films KW - Transparent conductive oxides PY - 2017 DO - https://doi.org/10.3762/bjnano.8.56 SN - 2190-4286 VL - 8 SP - 522 EP - 529 AN - OPUS4-39391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Knowing When To Stop-Trapping Metastable Polymorphs in Mechanochemical Reactions N2 - The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods. KW - Mechanochemistry KW - Polymorphs KW - Metastable KW - In situ PXRD KW - Cocrystal KW - Pyrazinamide PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01572 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 3 SP - 1190 EP - 1196 AN - OPUS4-39420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, S. G. A1 - Vleugels, J. A1 - Mohrbacher, H. A1 - Woydt, Mathias T1 - Microstructure and tribological performance of NbC-Ni cermets modified by VC and Mo2C N2 - The current study reports on the influence of the Addition of 5–15 vol% VC or/and Mo2C carbide on the microstructure and mechanical properties of nickel bonded NbC cermets, which are compared to cobalt bonded NbC cermets. The NbC, Ni and secondary carbides powder mixtures were liquid phase sintered for 1 h at 1420 °C in vacuum. The fully densified cermets are composed of a cubic NbC grains matrix and an evenly distributed fcc Ni binder. NbC grain growth was significantly inhibited and a homogeneous NbC grain size distribution was obtained in the cermets with VC/Mo2C additions. The mechanical properties of the NbC-Ni matrix cermets are strongly dependent on the carbide and Ni binder content and are directly compared to their NbC-Co equivalents. The liquid phase sintered NbC-12 vol% Ni cermet had a modest Vickers hardness (HV30) of 1077 ± 22 kg/mm2 and an indentation toughness of 9.1 ± 0.5 MPa·m1/2. With the addition of 10–15 vol% VC, the hardness increased to 1359 ± 15 kg/mm2, whereas the toughness increased to 11.3 ± 0.1 MPa·m1/2. Addition of 5 and 10 vol% Mo2C into a NbC-12 vol% Ni mixtures generated the same values in HV30 and KIC when compared to VC additions. A maximum flexural strength of 1899 ± 77 MPa was obtained in the cermet with 20 vol% Ni binder and 4 vol% VC+4 vol% Mo2C addition, exhibiting a high fracture toughness of 15.0 ± 0.5 MPa·m1/2, but associated with a loss in hardness due to the high Ni content. The dry sliding wear behaviour was established at room temperature and 400 °C from 0.1 to 10 m/s. KW - Cermet KW - Liquid phase sintering KW - Grain growth KW - Wear KW - Niobium carbide PY - 2017 DO - https://doi.org/10.1016/j.ijrmhm.2017.03.012 SN - 0263-4368 VL - 66 SP - 188 EP - 197 AN - OPUS4-40505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Kirner, Sabrina A1 - Koter, Robert A1 - Pentzien, Simone A1 - Spaltmann, Dirk A1 - Krüger, Jörg T1 - Femtosecond laser-induced periodic surface structures on titanium nitride coatings for tribological applications N2 - Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser ablation KW - Titanium nitride films KW - Friction KW - Wear PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0169433216322486 DO - https://doi.org/10.1016/j.apsusc.2016.10.132 SN - 0169-4332 SN - 1873-5584 VL - 418 IS - Part B SP - 572 EP - 579 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-40507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -