TY - JOUR A1 - Kim, K.J. A1 - Unger, Wolfgang A1 - Kim, J.W. A1 - Moon, D.W. A1 - Gross, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Dieter A1 - Wirth, Thomas A1 - Jordaan, W. A1 - van Staden, M. A1 - Prins, S. A1 - Zhang, L. A1 - Fujimoto, T. A1 - Song, X.P. A1 - Wang, H. T1 - Inter-laboratory comparison: quantitative surface analysis of thin Fe-Ni alloy films N2 - An international interlaboratory comparison of the measurement capabilities of four National Metrology Institutes (NMIs) and one Designated Institute (DI) in the determination of the chemical composition of thin Fe-Ni alloy films was conducted via a key comparison (K-67) of the Surface Analysis Working Group of the Consultative Committee for Amount of Substance. This comparison was made using XPS (four laboratories) and AES (one laboratory) measurements. The uncertainty budget of the measured chemical composition of a thin alloy film was dominated by the uncertainty of the certified composition of a reference specimen which had been determined by inductively coupled plasma mass spectrometry using the isotope dilution method. Pilot study P-98 showed that the quantification using relative sensitivity factors (RSFs) of Fe and Ni derived from an alloy reference sample results in much more accurate result in comparison to an approach using RSFs derived from pure Fe and Ni films. The individual expanded uncertainties of the participants in the K-67 comparison were found to be between 2.88 and 3.40 atomic %. The uncertainty of the key comparison reference value (KCRV) calculated from individual standard deviations and a coverage factor (k) of 2 was 1.23 atomic %. KW - Quantification KW - Fe-Ni alloy KW - Uncertainty KW - Key comparison KW - Traceability PY - 2012 DO - https://doi.org/10.1002/sia.3795 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 2 SP - 192 EP - 199 PB - Wiley CY - Chichester AN - OPUS4-24505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wittig, Günther A1 - Thomas, Hans-Martin A1 - Maser, Dieter A1 - Hennig, P. T1 - Application of the pulsed-eddy-current techniques for the inspection of the austenitic cladding in a thermal shock loaded nozzle of a pressure vessel T2 - 6th International Conference on NDE in the Nuclear Industry and Equipment CY - Zürich, Switzerland DA - 1983-11-28 PY - 1984 SN - 0-87170-192-8 SP - 665 EP - 674 PB - American Society for Metals CY - Metals Park, Ohio AN - OPUS4-34232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Puthiyaveettil, N. A1 - Thomas, K. R. A1 - Myrach, Philipp A1 - Ziegler, Mathias A1 - Rajagopal, P. A1 - Balasubramaniamam, K. T1 - Defect detection in steel bars up to 600 °C using laser line thermography N2 - Crack detection in steel bars at high surface temperatures is a critical problem in any manufacturing industry. Surface breaking cracks are the major problems during the billet casting. Many NDT techniques are proven its capability in crack detection at room temperature. Here, we are demonstrating the possibility of exposure of cracks using laser line thermography at higher surface temperatures (up to 600 °C). A continuous-wave (CW) laser is used to excite the sample kept at higher surface temperatures. The temperature distribution over the sample due to the laser line scanning is captured using a temperature calibrated infrared (IR) thermal camera. The response of the sample temperature in crack detection is investigated using a validated FE model. The impact of the oxide layer in crack detection is investigated by using two types of samples; one without any oxide layer and the second is with the oxide layer. The influence of laser power in the detection of defects at high temperatures is studied. 3D numerical models were developed for the cases; when the sample is with oxide layer and without any oxide layer for a better understanding of physics. The surface temperature rise due to laser heating is higher for the scaled sample compared to the no-scale sample. The presence of the oxide layer above the parent metal will reduce the reflectivity of the surface. Lower reflectivity will lead to increased absorption of incident energy so that the surface temperature rise will be higher than the surface with no scale. Thermal contrast linearly depends on laser power, which means higher laser power will increase the defect detectability even at a higher surface temperature. KW - Laser thermography KW - High temperature KW - Modeling KW - Surface cracks KW - Non-destructive testing PY - 2020 DO - https://doi.org/10.1016/j.infrared.2020.103565 SN - 1350-4495 VL - 111 SP - 103565 PB - Elsevier B.V. AN - OPUS4-51573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Spurenbestandteile in frühmittelalterlichem Ägyptisch Blau als Informationsträger N2 - Naturwissenschaftliche Belege für die Verwendung von Ägyptisch Blau, dem klassischen Blaupigment der römischen Antike, an frühmittelalterlichen Wandmalereien in Mittel- und Südeuropa sind bisher nur vereinzelt greifbar. Das hier diskutierte monochrom blaue Fragment einer Freskomalerei auf Tünche gehört zum zweiten Kirchenbau von St. Peter ob Gratsch (Südtirol, Norditalien); zumindest der Putzmörtel ist gemäß Radiocarbondatierung im 5. oder 6. Jahrhundert n. Chr. zu verorten. Das flächendeckende Abrastern der Probenoberfläche mittels Ramanmikrospektroskopie vermochte neben dem farbgebenden Cuprorivait (und Pflanzenschwarz aus der Untermalung) 26 begleitende Mineralien bis in den Spurenbereich nachzuweisen. Diese erstaunliche Vielfalt ist nur durch mikrospektroskopische Bildgebung in hoher Ortsauflösung zugänglich, ein solch vertiefter Einblick in die Mineralogie der zugrundeliegenden Rohstoffe als auch Umwandlungsreaktionen während Herstellung, Applikation und Alterung des künstlichen Blaupigmentes also an die Weiterentwicklung der analytischen Verfahren gebunden. Insbesondere die natürlichen Verunreinigungen des Quarzsandes liefern Indizien auf die Produktionsstätte: die beiden Klinopyroxene Augit und Aegirin deuten beispielsweise auf magmatischen Aktivitäten ausgesetzte Ablagerungen (oder auf vulkanische Aktivität bereits im Liefergebiet). Zusammen mit Diopsid und Feldspaten, einschließlich des seltenen Celsian, sind sie der Literatur zufolge charakteristischer Bestandteil von vom Fluss Volturno in den Golf von Gaeta transportierten carbonathaltigen Sedimenten. Im Verein mit der archäologischen Evidenz für die Erzeugung von Ägyptisch Blau in Cumae und Liternum und den übereinstimmenden Ausführungen der beiden römischen Fachschriftsteller Vitruv und Plinius der Ältere spricht dies für ein Fabrikat aus dem Golf von Pozzuoli. Als Kupferquelle wurde angesichts des Nachweises von Chalkosin (und Chalkopyrit) vermutlich ein sulfidisches Kupfererz nach Rosten zu Kupferoxid eingesetzt, als schmelzpunktsenkendes Flussmittel wohl ein gemischt-alkalisches, das heißt eine Mischung von Natrium- und Kaliumsalzen in Form von Pflanzenasche. Zum Teil mit Cuprorivait verwachsene, nicht gänzlich umgesetzte Quarzkristalle bei nur geringsten Spuren von Silikatglas lassen auf eine überwiegende Festkörperreaktion (Festphasensintern) schließen; das Aufschmelzen der Rohstoffe zu Glas dürfte bei der Pigmentsynthese eher eine untergeordnete Rolle gespielt haben. KW - Ägyptisch Blau KW - Ramanmikrospektroskopie KW - Spektroskopische Bildgebung KW - Cuprorivait KW - Amorpher Kohlenstoff PY - 2021 VL - 34 SP - 109 EP - 122 PB - Wernersche Verlagsgeselltschaft CY - Worms AN - OPUS4-53758 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Trace compounds in Early Medieval Egyptian blue carry information on provenance, manufacture, application, and ageing N2 - Only a few scientific evidences for the use of Egyptian blue in Early Medieval wall paintings in Central and Southern Europe have been reported so far. The monochrome blue fragment discussed here belongs to the second church building of St. Peter above Gratsch (South Tyrol, Northern Italy, fifth/ sixth century A.D.). Beyond cuprorivaite and carbon black (underpainting), 26 accessory minerals down to trace levels were detected by means of Raman microspectroscopy, providing unprecedented insights into the raw materials blend and conversion reactions during preparation, application, and ageing of the pigment. In conjunction with archaeological evidences for the manufacture of Egyptian blue in Cumae and Liternum and the concordant statements of the antique Roman writers Vitruvius and Pliny the Elder, natural impurities of the quartz sand speak for a pigment produced at the northern Phlegrean Fields (Campania, Southern Italy). Chalcocite (and chalcopyrite) suggest the use of a sulphidic copper ore, and water-insoluble salts a mixed-alkaline flux in the form of plant ash. Not fully reacted quartz crystals partly intergrown with cuprorivaite and only minimal traces of silicate glass portend solid-state reactions predominating the chemical reactions during synthesis, while the melting of the raw materials into glass most likely played a negligible role. KW - Egyptian blue KW - Raman microspectroscopy KW - Spectoscopic imaging KW - Cuprorivaite KW - Amorphous carbon PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537591 DO - https://doi.org/10.1038/s41598-021-90759-6 VL - 11 SP - 1 EP - 12 PB - Nature Portfolio AN - OPUS4-53759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Kraft, Ronja A1 - Dariz, P. T1 - Shedding light onto the spectra of lime - Part 2: Raman spectra of Ca and Mg carbonates and the role of d-block element luminescence N2 - We previously described the observation of a characteristic narrowband red luminescence emission of burnt lime (CaO), whose reason was unknown so far. This study presents Raman spectra of Mg5 CO3)4(OH)2∙4H2O, Mg5(CO3)4(OH)2, MgCO3, CaMgCO3 and CaCO3 (in limestone powder) as well as luminescence spectra of their calcination products. Comparison of the latter revealed MgO:Cr3+ as the source of the red lime luminescence in all studied samples, containing magnesium oxide as major component, minor component or trace. Spectral characteristics and theoretical background of the luminescence emission of d-block elements integrated in crystal lattices are discussed with the aim of sharpening the awareness for this effect in the Raman community and promoting its application in materials analysis. The latter is demonstrated by the Raman microspectroscopic imaging of the distributions of both Raman-active and Raman-inactive phases in clinker remnants in a 19th-century meso Portland cement mortar sample, which contain relatively high amounts of free lime detected in the form of both luminescing CaO and Raman-scattering Ca(OH)2, owing to exposure of the surface of the thin section to humid air. A combination of light and Raman spectroscopy revealed a calcium–magnesium–iron sulphide phase, indicating sulphurous raw materials and/or solid fuels employed in the calcination process, which in contrast to previously described morphologies of sulphides in cement clinker form extensive greenish black layers on free lime crystals. KW - Calcium carbonates KW - Raman spectroscopy KW - Luminescence KW - Magnesium carbonates KW - Meso Portland cement PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537611 DO - https://doi.org/10.1002/jrs.6174 SN - 0377-0486 VL - 52 IS - 8 SP - 1462 EP - 1472 PB - Wiley Analytical Science AN - OPUS4-53761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Hidde, Julia A1 - Grünier, Sophie A1 - Jungnickel, Robert A1 - Dariz, P. A1 - Riedel, Jens A1 - Neuhaus, B. T1 - Ageing effects in mountig media of microscope slide samples from natural history collections: A case study with Canada balsam and Permount™ N2 - Microscope slide collections represent extremely valuable depositories of research material in a natural history, forensic, veterinary, and medical context. Unfortunately, most mounting media of these slides deteriorate over time, with the reason for this not yet understood at all. In this study, Raman spectroscopy, ultraviolet–visible (UV–Vis) spectroscopy, and different types of light microscopy were used to investigate the ageing behaviour of naturally aged slides from museum collections and the experimentally aged media of Canada balsam and Permount™, representing a natural and a synthetic resin, respectively, with both being based on mixtures of various terpenes. Whereas Canada balsam clearly revealed chemical ageing processes, visible as increasing colouration, Permount™ showed physical deterioration recognisable by the increasing number of cracks, which even often impacted a mounted specimen. Noticeable changes to the chemical and physical properties of these mounting media take decades in the case of Canada balsam but just a few years in the case of Permount™. Our results question whether or not Canada balsam should really be regarded as a mounting medium that lasts for centuries, if its increasing degree of polymerisation can lead to a mount which is no longer restorable. KW - Deterioration KW - Microscope slides KW - Mounting media KW - Raman spectroscopy KW - UV–Vis spectroscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537632 DO - https://doi.org/10.3390/polym13132112 VL - 13 IS - 13 SP - 1 EP - 27 PB - MDPI CY - Basel AN - OPUS4-53763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Wortmann, U. G. A1 - Vogl, Jochen A1 - Schmid, Thomas T1 - Beautiful Pietàs in South Tyrol (Northern Italy): local or imported works of art? N2 - The study, dedicated to Beautiful Pietàs conserved in South Tyrol (Northern Italy), aims to establish, for the first time, a connection between Austroalpine raw materials and the high-fired gypsum mortars constituting the Gothic figure groups in question. The origin and chronology of this stylistically and qualitatively differing ensemble have been subject of art historical debate for nearly a century. The discourse is dominated by three main hypotheses: itinerary of an Austrian artist versus itinerary of the work of art created in an artist’s workshop in Austria versus itinerary of the stylistic vocabulary via graphical or three-dimensional models. The comparison of the δ34S values and the 87Sr/86Sr ratios of the gypsum mortars and Austroalpine sulphate deposits (in a compilation of own reference samples and literature data) points to the exploitation of sediments in the Salzkammergut and possibly also in the evaporite district of the Eastern Calcareous Alps, thus evidencing the import of the sculptures and not the activities of local South Tyrolean or itinerant artists. Two geochronological units are distinguishable: The Pietà in the Church St. Martin in Göflan can be assigned to Upper Permian raw material, whereas the metrologically consistent sculptures in the Church of Our Lady of the Benedictine Abbey Marienberg and in the Chapel St. Ann in Mölten correlate with deposits of the Early Triassic (or the Lower-Middle Triassic transition). The medieval gypsum mortars also differ in their mineralogical characteristics, i.e. in their geologically related minor components, as in the first case, characterised by a significant proportion of primary anhydrite, natural carbonate impurities mainly consist of calcite (partly converted to lime-lump-like aggregates), whereas in the second group dolomite (or rather its hydration products after pyrometamorphic decomposition) predominates, accompanied by celestine, quartz and potassium feldspar. The Pietà in the Cathedral Maria Himmelfahrt in Bozen turned out to be made of Breitenbrunn calcareous sandstone (Leitha Mountains, Burgenland, Austria), which is why the sample is not considered in the geochemical analysis. KW - High-fired gypsum mortar KW - Sulphur isotope KW - Strontium isotope KW - Polarised light microscopy KW - Raman microspectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545610 DO - https://doi.org/10.1186/s40494-022-00678-6 SN - 2050-7445 VL - 10 IS - 1 SP - 1 EP - 17 PB - Springer Nature AN - OPUS4-54561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bernhardt, Y. A1 - Csaszar, L. A1 - Dengiz, N. A1 - Fuchs, M. A1 - Gautzsch, T. A1 - Gohlke, Dirk A1 - Hahn-Jose, T. A1 - Heckel, Thomas A1 - Hillger, W. A1 - Hufschläger, Daniel A1 - Ilse, D. A1 - Kiel, M. A1 - Labud, P. A1 - Schubert, F. A1 - Sommerhuber, R. A1 - Szewieczek, A. A1 - Waschkies, T. T1 - Richtlinie zur Charakterisierung von luftgekoppelten Ultraschallwandlern N2 - Zur Charakterisierung von luftgekoppelten Ultraschallwandlern werden mehrere verschiedene Methoden und Verfahren angewendet. Durch die unterschiedlichen Herangehensweisen werden oft unterschiedliche Prüfkopfpara-meter und Schallfeldgrößen ermittelt, was einen direkten Vergleich von Datenblättern erschwert. Für die Charakterisierung von Kontakt- und Tauchtechnikprüfköpfen hat sich ISO 22232-2:2021 bereits etabliert, allerdings ist diese Norm nicht auf die luftgekoppelten Wandlertechnologien direkt übertragbar. Daher erkannten Hersteller, Forschungseinrichtungen und Anwender den Bedarf an einer Richtlinie zur einheitlichen Charakterisierung von luftgekoppelten Wandlern. Gemeinsam arbeiten sie aktuell im Rahmen des Unterausschusses „Luftgekoppelte Ultraschallprüfung“ der DGZfP an der Erstellung einer solcher Richtlinie mit dem Anspruch, die bestehende Normung um die luftgekoppelte Prüfung zu erweitern und somit die Vereinheitlichung der Charakterisierung dieser Wandler zu erleichtern. In diesem Beitrag wird ein Überblick über den geplanten Inhalt der Richtlinie und über die Methoden zur akustischen Charakterisierung von luftgekoppelten Ultraschallwandlern gegeben. Insbesondere werden verschiedene Methoden der Ermittlung von wichtigen Wandlerparametern wie z.B. Empfindlichkeit, Mittenfrequenz, Bandbreite, Fokusgröße und Fokusabstand dargestellt und verglichen. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Lutgekoppelte Ultraschallprüfung KW - Prüfkopf KW - Charakterisierung KW - Richtlinie PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552918 SP - 1 EP - 7 AN - OPUS4-55291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Xin A1 - Thomas, P. T1 - Phase Error Evaluation via Differentiation and Cross-Multiplication Demodulation in Phase-Sensitive Optical Time-Domain Reflectometry N2 - Phase-sensitive optical time-domain reflectometry (jOTDR) is a technology for distributed vibration sensing, where vibration amplitudes are determined by recovering the phase of the backscattered light. Measurement noise induces phase errors, which degrades sensing performance. The phase errors, using a differentiation and cross-multiplication (DCM) algorithm, are investigated theoretically and experimentally in a jOTDR system based on a phase retrieval configuration consisting of an imbalanced Mach–Zehnder interferometer (IMZI) and a 3 x 3 coupler. Analysis shows that phase error is highly dependent on the AC component of the obtained signal, essentially being inversely proportional to the product of the power of the light backscattered from two locations. An analytical expression was derived to estimate the phase error and was confirmed by experiment. When applied to the same measurement data, the error is found to be slightly smaller than that obtained using in-phase/quadrature (I/Q) demodulation. The error, however, increases for longer measurement times. KW - Distributed fiber sensing KW - Phase-sensitive optical time-domain reflectometry KW - Phase error PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580501 UR - https://www.mdpi.com/2304-6732/10/5/514 DO - https://doi.org/10.3390/photonics10050514 SN - 2304-6732 VL - 10 IS - 5 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-58050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, P. A1 - Chakraborty, Gouri A1 - Roeser, J. A1 - Vogl, S. A1 - Rabeah, J. A1 - Thomas, A. T1 - Integrating Bifunctionality and Chemical Stability in Covalent Organic Frameworks via One-Pot Multicomponent Reactions for Solar-Driven H2O2 Production N2 - Multicomponent reactions (MCRs) can be used to introduce different functionalities into highly stable covalent organic frameworks (COFs). In this work, the irreversible three-component Doebner reaction is utilized to synthesize four chemically stable quinoline-4-carboxylic acid DMCR-COFs (DMCR-1−3 and DMCR-1NH) equipped with an acid−base bifunctionality. These DMCR-COFs show superior photocatalytic H2O2 evolution (one of the most important industrial oxidants) compared to the imine COF analogue (Imine-1). This is achieved with sacrificial oxidants but also in pure water and under an oxygen or air atmosphere. Furthermore, the DMCR-COFs show high photostability, durability, and recyclability. MCR-COFs thus provide a viable materials’ platform for solar to chemical energy conversion. KW - Reactions KW - Bifunctionality KW - Postsynthetic modification KW - Multicomponent PY - 2022 DO - https://doi.org/10.1021/jacs.2c11454 SN - 0002-7863 VL - 145 IS - 5 SP - 2975 EP - 2984 PB - ACS Publications AN - OPUS4-56922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Raman focal point on Roman Egyptian blue elucidates disordered cuprorivaite, green glass phase and trace compounds N2 - The discussed comparative analyses of Roman Imperial pigment balls and fragmentary murals unearthed in the ancient cities of Aventicum and Augusta Raurica (Switzerland) by means of Raman microspectroscopy pertain to a predecessor study on trace compounds in Early Medieval Egyptian blue (St. Peter, Gratsch, South Tyrol, Northern Italy). The plethora of newly detected associated minerals of the raw materials surviving the synthesis procedure validate the use of quartz sand matching the composition of sediments transported by the Volturno river into the Gulf of Gaeta (Campania, Southern Italy) with a roasted sulphidic copper ore and a mixed-alkaline plant ash as fluxing agent. Thus, the results corroborate a monopolised pigment production site located in the northern Phlegrean Fields persisting over the first centuries A.D., this in line with statements of the antique Roman writers Vitruvius and Pliny the Elder and recent archaeological evidences. Beyond that, Raman spectra reveal through gradual peak shifts and changes of band width locally divergent process conditions and compositional inhomogeneities provoking crystal lattice disorder in the chromophoric cuprorivaite as well as the formation of a copper-bearing green glass phase, the latter probably in dependency of the concentration of alkali flux, notwithstanding that otherwise solid-state reactions predominate the synthesis. KW - Raman microspectroscopy KW - Egyptian blue KW - Cuprorivaite PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559028 DO - https://doi.org/10.1038/s41598-022-19923-w SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 12 PB - Nature Publishing Group CY - London AN - OPUS4-55902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bernhardt, Y. A1 - Császár, L. A1 - Dengiz, N. A1 - Fuchs, M. A1 - Gaal, Mate A1 - Gautzsch, T. A1 - Gohlke, Dirk A1 - Hahn-Jose, T. A1 - Heckel, Thomas A1 - Hillger, W. A1 - Hufschläger, Daniel A1 - Ilse, D. A1 - Kiel, M. A1 - Kornely, M. A1 - Labud, P. A. A1 - Marhenke, T. A1 - Schubert, F. A1 - Sommerhuber, R. A1 - Steinhausen, R. A1 - Szewieczek, A. A1 - Wachter, L. A1 - Waschkies, T. T1 - Characterization and verification of air-coupled ultrasonic probes N2 - This guideline was drafted following and complementing the norm ISO 22232-2:2020(E) to include air-coupled ultrasonic transducers. This document specifies the characteristics of probes used for non-destructive air-coupled ultrasonic testing with center frequencies above 20 kHz, with focusing or without focusing means. KW - Air-coupled ultrasound KW - Ultrasonic testing KW - Guideline KW - Probe KW - Characterization PY - 2022 SN - 978-3-947971-26-8 VL - Guideline US 08 SP - 1 EP - 23 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin ET - Edition September 2022 AN - OPUS4-56228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Chemical imaging of historical mortars by Raman microscopy N2 - Raman microspectroscopic imaging was just recently introduced into the analysis of cement stone. Here, we demonstrate this approach on 19th-century Roman and Portland cement mortars and extend it to gypsum-based samples originating from a medieval stucco sculpture (high-burnt gypsum) and a stucco ornament prefabricated at the beginning of the 20th century (plaster of Paris). Furthermore, the distributions of dolomite and Calcite were mapped in an accessory mineral grain with approx. 500 nm lateral Resolution demonstrating the ability for studying alteration processes such as dedolomitisation. As we would like to make this approach accessible to other researchers, we discuss its present status, advantages, limitations and pitfalls. KW - Raman microscopy KW - Chemical imaging KW - Cement clinker KW - Gypsum KW - Dedolomite PY - 2016 DO - https://doi.org/10.1016/j.conbuildmat.2016.03.153 SN - 0950-0618 VL - 114 SP - 506 EP - 516 PB - Elsevier Science CY - Oxford, UK AN - OPUS4-36661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Granulierte Hochofenschlacke als Mörtelzuschlag im 19. Jahrhundert in der Schweiz N2 - Als schweizweit einziger Hersteller produzierte die Gesellschaft der Ludwig von Roll'schen Eisenwerke seit den 1870er Jahren granulierte Hochofenschlacke. Im Blashochofen von Choindez im Schweizer Jura wird bis Mitte der 1920er Jahre Bohnerz aus dem Delsberger Becken, das kontemporär publizierten Analysen zufolge als Spuren- bzw. Schwermetalle Titan, Chrom, Blei und Vanadium enthält, zu grauem Roheisen verhüttet. In zementgebundenen Mörtelmischungen des 19. und frühen 20. Jahrhunderts aus verschiedenen Regionen der Schweiz finden sich neben reliktischen Hüttensandsplittern vereinzelt bis zu fünfhundert Mikrometer große scharze Kugeln mit grünlichem Schimmer, wohl nicht gemahlener Schlackensand. Deren mittels Ramanmikroskopie (Phasenbestand) und energiedispersiver Röntgenspektroskopie am Rasterelektronenmikroskop (Elementanalytik) ermittelte Mineralogie ergibt in Form von Plattnerit PbO2, Rutil TiO2 und vermitlich Chromit Fe(II)Cr2O4 bzw. Nichromit (Ni,Co,Fe(II))(Cr,Fe(III),Al)2)4 Übereinstimmungen mit den nur die Elementzusammensetzung berücksichtigenden historischen Resultaten. Ebenfalls im Zusammenhang mit dem das Bohnerz begleitenden Boluston samt Huppererde zu sehen sind die Minerale Coelestin SrSO4 und Zirkon ZrSiO4, des Weiteren der Siliciumcarbidpolymorph Moissanit SiC als Reaktionsprodukt von Quarzsand und Brennstoff. Die Kohärenz zwischen um die Jahrhundertwende durchgeführten Analysen von Rohmaterial als auch Ofenbruch aus dem in Choindez betriebenen Hochofen und den in diesem Beitrag diskutierten Resultaten moderner analytischer Methoden spricht für den Gebrauch von granulierter Schlacke aus dem Hause Ludwig von Roll als Mörtelzuschlag. Die Hüttensandkörner, eigentlich latent hydraulisch, sind aufgrund der fehlenden Aufbereitung zu grob für eine effektive Hydratation und deshalb trotz reaktiver Glasphase und Klinkermineralien (Belit Ca2SiO4 und Monocalciumaluminat CaAl2O4) intakt in der Bindemittelmatrix erhalten. N2 - From the 1870s the Ludwig von Roll ironworks produced granulated blast furnace slag in Choindez (Jura, Switzerland) as a by-product of the smelting of bean ore excavated until 1926 in the Delsberg Basin. According to historical analyses, this iron ore deposit contais heavy and trace metals such as titanium, chromium, lead and vanadium. In mortar samples from different regions of Switzerland originating from the 19th and early 20th centuries, residues of granulated blast furnace slag are observable as angular glassy particles in the binder matrix. In addition, black spherical grains with greenish lustre (up to 500 micrometres in diameter), probably not ground granulated blast furnace slag, can be distinguished sporadically in thin sections. Raman microscopy as well as scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX) measurements have revealed, inter alia, the presence of the crystalline components plattnerite PbO2, rutile TiO2 and presumably chromite Fe(II)Cr2O4 or nichromite (Ni,Co,Fe(II))(Cr,Fe(III),Al)2O4. These findings are consistent with historical analyses, which were restricted to the determination of the elemental (not phase) composition of the raw material processed by the Ludwig von Roll ironworks. Furthermore the minerals celestine SrSO4 and zircon ZrSiO4 can be linked to bean ore and bole from Delsberg, and likewise the silicon carbide moissanite SiC, which is a reaction product of quartz sand and coke. The coherence if the results of historical chemical analyses and of modern microscopic imaging and spectroscopy methods described here pinpoints the Ludwig von Roll ironworks as the most probable supplier of the granulated blast furnace slag that was added to the mortars under investigation. The unreacted remnants exhibit defined boundaries; no hydration rims are observable despite the glassy nature of the latent hydraulic aggregate, which contains cement clinker minerals (belite and calcium aluminate) as crystalline components. Not finely ground, the spheroids are too coarse for an effective hydration reaction and act as inert filler. KW - Granulierte Hochofenschlacke KW - Raman Mikroskopie KW - REM-EDX KW - Granulated blast furnace slag KW - Raman microscopy KW - SEM-EDX PY - 2015 VL - 29 IS - 2 SP - 293 EP - 304 PB - Wernersche Verlagsgesellschaft mbH CY - Worms AN - OPUS4-36651 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Álvarez-García, J. A1 - Izquierdo-Roca, V. A1 - Pistor, P. A1 - Schmid, Thomas A1 - Pérez-Rodríguez, A. ED - Abou-Ras, D. ED - Kirchartz, T. ED - Rau, U. T1 - Raman spectroscopy on thin films for solar cells N2 - In the present chapter, the capabilities of Raman spectroscopy for the advanced characterisation of thin films for solar cells are reviewed. Raman spectroscopy is an optical, nondestructive technique based on the inelastic scattering of photons with elemental vibrational excitations in the material. The line shape and position of the Raman bands are determined by the crystalline structure and chemical composition of the measured samples, being sensitive to the presence of crystalline defects, impurities and strain. Presence of peaks characteristic of different phases also allows for the identification of secondary phases that are strongly related to the growth and process conditions of the films. All these aspects account for a strong interest in the analysis of the Raman spectra, providing a powerful nondestructive analytical tool for the structural and chemical assessment of the films. In addition, the combination of a Raman spectrometer with an optical microscope also allows for achieving a high spatial resolutions (of below 1 µm) when mapping surfaces and analyzing depth-resolved phase distributions in thin films. The present chapter is divided into four main sections: The two first ones are devoted to a revision of the Fundamentals of Raman spectroscopy (Section 17.2) and Vibrational modes in crystalline materials (Section 17.3). Section 17.4 deals with the main experimental considerations involved in the design and implementation of a Raman scattering setup. This is followed by a detailed description of the application of Raman scattering for the structural and chemico-physical analysis of thin film photovoltaic materials (Section 17.5), with the identification of crystalline structure and secondary phases, evaluation of film crystallinity, analysis of chemical composition of semiconductor alloys, characterisation of nanocrystalline and amorphous layers, stress effects and crystal orientations. This includes the description of corresponding state of the art and recent case examples that illustrate the capabilities of the Raman technique for the advanced characterisation of layers and process monitoring in thin-film photovoltaic technologies. KW - Thin-film solar cells KW - Polycrystalline materials KW - Raman spectroscopy KW - Raman microscopy PY - 2016 UR - http://eu.wiley.com/WileyCDA/WileyTitle/productCd-3527339922.html SN - 978-3-527-33992-1 SP - 469 EP - 499 PB - Wiley & Sons, Ltd. CY - Oxford, UK AN - OPUS4-37451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Jakob, C. A1 - Ectors, D. A1 - Neubauer, J. A1 - Schmid, Thomas T1 - Measuring the Burning Temperatures of Anhydrite Micrograins in a High-Fired Medieval Gypsum Mortar N2 - Typical feature of high-fired medieval gypsum mortars is a compact microstructure of squat gypsum crystals containing firing products as remains of the calcination process. So far, the burning history of the binder is estimated based on morphological characteristics of the latter. A novel Raman microspectroscopy approach provides access to the calcination temperatures of individual anhydrite grains based on quantifiable spectroscopic changes appearing due to gradual variations of crystallinity, as independently confirmed by X-ray diffraction analysis of anhydrites synthesised at temperatures between 500°C and 900°C. The approach was successfully applied to the high-fired gypsum mortar of a South Tyrolean stucco sculpture of a pieta dated around 1420. Microparticles of burned anhydrite II with firing temperatures scattered around 650°C and clusters of thermally damaged natural anhydrite II crystals from the raw material were identified and imaged. KW - Analytical methods KW - Gypsum technology KW - High-fired gypsum mortar KW - Raman microspectroscopy KW - Thermal anhydrite PY - 2017 DO - https://doi.org/10.1002/slct.201701260 VL - 2 IS - 28 SP - 9153 EP - 9156 PB - Wiley VCH Verlag AN - OPUS4-42458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Temperaturindikatoren in mittelalterlichen Hochbrandgipsen: Eine Ramanmikrospektroskopische Studie N2 - Infolge der beschränkten Kontrollmöglichkeiten über die in einem Meiler oder Feldofen herrschenden Parameter konstituiert mittelalterliche Hochbrandgipse ein Gemisch aus verschiedenen Anhydritstufen. Basierend auf modernen Versuchsbränden dienen in der gealterten Gipsmatrix nicht oder nur teilweise hydratisiert erhaltene Brenngutkörner üblicherweise anhand der morphologischen Eigenschaften der Anhydritkristalle der groben Einschätzung der zumindest lokal im Ofen bzw. im stückigen Brenngut erreichten Temperaturwerte. Die bildgebende Ramanmikroskopie ermöglicht die kornspezifische Bestimmung der Hitzeeinwirkung über den Grad der sich im Ramanspektrum abbildenden thermischen Beeinträchtigung der Thermoanhydritphasen, als auch deren Unterscheidung von primärem Anhydrit aus der Gipslagerstätte, da diesen eine höhere Kristallinität kennzeichnet. Hier beispielhaft diskutierte Ramananalysen an zwei reliktischen Brenngutkörnern lassen auf Brenntemperaturen von 650°C bzw. 800°C schließen. Pyrometamorphe Phasenneubildungen der natürlichen Verunreinigungen des Rohgipses liefern aufgrund ihres Bildungs- und Stabilitätsbereiches zusätzliche Hinweise. Im Beitrag erörtert werden die an die Dehydratation von magnesiumreichem Chlorit korrelierte Genese von Forsterit sowie die Zersetzung von Dolomit zu Calcit und Periklas, welcher beim Anmachen des Mörtels zu Brucit gelöscht wird und im Laufe der Zeit in der Gipsmatrix zu Magnesit carbonatisiert; beide pyrometamorphen Reaktionen erfordern Temperaturen von über 800°C. KW - Ramanmikrospektroskopie KW - Mineralthermometer KW - Gips PY - 2018 SN - 0931-7198 VL - 32 IS - 1 SP - 69 EP - 78 PB - Wernersche Verlagsgesellschaft mbH CY - Worms AN - OPUS4-47041 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Traulsen, Ch. H.-H. A1 - Darlatt, Erik A1 - Baytekin, B. A1 - Heinrich, Thomas A1 - Deutinger, P. M. A1 - Huth, K. A1 - Unger, Wolfgang A1 - Schalley, Ch. T1 - Programmable multilayers of nanometer-sized macrocycles on solid support and stimuli-controlled on-surface pseudorotaxane formation N2 - Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities. KW - NEXAFS KW - XPS KW - Supramolecular Chemistry KW - Multilayers KW - Pyridine KW - UV/Vis KW - Macrocycles KW - Pseudorotaxanes PY - 2013 DO - https://doi.org/10.1039/c3sc50558h VL - 4 IS - 8 SP - 3131 EP - 3139 AN - OPUS4-42668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genga, R. M. A1 - Glaser, D. A1 - Rokebrand, P. A1 - Cornish, L. A. A1 - Woydt, M. A1 - Gradt, Thomas A1 - Janse van Vuuren, A. A1 - Polese, C. ED - von Leipzig, K. ED - Sacks, N. ED - McClelland, M. T1 - Laser shock peening: A NbC based cermet enhancement alternative for improved GCI interrupted face-milling N2 - Attempts were made to improve the properties and machining performance of NbC based cermet cutting inserts for face milling of grey cast iron (GCI) (BS 1452/GG35) by spark plasma sintering (SPS), use of sub-stoichiometric NbC (NbC₀ˏ₈₈), Cr₃C₂ and Mo₂C additives and laser shock peening (LSP). The microstructure, hardness, fracture toughness and Young’s modulus of WC–Co, NbC₀ˏ₈₈-Co and NbC₀ˏ₈₈-Ni cermet-based inserts were investigated for machining performance. Additions of Mo₂C and manufacture by SPS significantly refined the NbC₀ˏ₈₈-Ni/Co cermet’s carbide grain size from ~5.0 μm to <0.9 μm, which increased the hardness (by ~4GPa) and wear resistance. Laser shock peening (LSP) improved the fracture toughness of all the inserts, from 10% (in the SPS WC based in cermets) to ~100% (in the LPS NbC based cermets). Uncoated cutting inserts were manufactured from the sintered cermets in an SNMA (double sided square insert without a chipformer on the cutting edge) shape (12.7 × 12.7 × 4.3 mm³, 1.6 mm nose radius). The inserts were used for interrupted face-milling of GCI at cutting speeds (ν˛) ranging from 100 m/minute (400 rpm)–500 m/minute (2000 rpm) and depths of cut (ɑₚ) of 0.2–1.0 mm. The insert wear was measured after every pass and analyzed by annular dark field scanning transmission electron microscopy (ADF-STEM). Cutting temperatures were measured with a high-speed thermal camera and forces were measured using a Kistler dynamometer. During machining at ν˛ = 200 m/minute and ɑₚ = 1.0 mm, WC–Co inserts had the lowest flank wear rate (FWR), although LSP significantly improved the tool life of the NbC₀ˏ₈₈-Ni inserts, significantly reducing the FWR from 148.63 μm/minute to 99.79 μm/minute (by ~33%) and the average resultant force from 1257 ± 15 N to 535 ± 15 N. During machining at ν˛ = 500 m/minute and ɑₚ = 0.2 mm, LSP significantly lowered the FWRs of the NbC₀ˏ₈₈ inserts, giving better tool life than all the WC based inserts. Generally, LSP improved the NbC₀ˏ₈₈ inserts’ tool life, reducing the flank wear rate by up to 33% during roughing and 63% during finishing. T2 - 8th International Conference on Competitive Manufacturing (COMA ’22) CY - Stellenbosch, South Africa DA - 09.03.2022 KW - Niobium carbide KW - Laser shock peening KW - Face milling KW - Tool wear PY - 2023 SN - 978-3-031-15602-1 SN - 978-3-031-15601-4 SN - 978-3-031-15604-5 DO - https://doi.org/10.1007/978-3-031-15602-1_62 SN - 2194-0525 SN - 2194-0533 N1 - Serientitel: Lecture notes in production engineering – Series title: Lecture notes in production engineering SP - 871 EP - 889 PB - Springer CY - Cham AN - OPUS4-62689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Christensen, J. B. A1 - Jørgensen, A. A. A1 - Vandborg, M. H. A1 - Thomas, P. J. A1 - Lu, Xin A1 - Failleau, G. A1 - Eisermann, R. A1 - Grüner-Nielsen, L. A1 - Balslev-Harder, D. A1 - Lassen, M. A1 - Krenek, S. T1 - Fiber-artefact methodology and calibration framework for Brillouin-based fiber sensing N2 - We propose, and demonstrate, the use of a fiber-optical measurement artefact as a metrological tool for traceable distance calibration of distributed optical fiber sensors. The constructed fiber artefact consists of a lead-in fiber coupled to a fiber loop using a 3-dB coupler and is used to calibrate both a home-build Brillouin-OTDR setup and a custom version of a commercial Brillouin-OTDR interrogator build for distributed temperature sensing. For both interrogators, we demonstrate distance calibrations with 1-meter uncertainty (k=1) in the offset length and 0.1 % (1 m/km) uncertainty (k = 1) in the distance scale factor. In addition, it is shown that the fiber artefact can be used to assess undesired distance-dependent measurement biases. KW - Distributed temperature sensing KW - Metrology KW - Distributed optical fiber sensing KW - Brillouin optical time-domain reflectrometry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618853 DO - https://doi.org/10.1364/OE.544659 SN - 1094-4087 VL - 32 IS - 26 SP - 45483 EP - 45493 PB - Optica Publishing Group AN - OPUS4-61885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Shedding light onto the spectra of lime: Raman and luminescence bands of CaO, Ca(OH)2 and CaCO3 N2 - In microscopy studies of 19th-century cement stone, we found free lime in the form of darkened spherical structures, as they were described in the literature already. When trying to determine their phase composition by Raman spectroscopy, we encountered contradictive assignments in literature spectra of the lime phases CaO, Ca(OH)2 and CaCO3 and observed strong spectral features that have been ignored or erroneously assigned so far. In this study we present Raman spectra of pure lime phases and of a naturally grown calcite crystal, burnt limestone (quick lime, mainly CaO), aged slaked lime putty (mainly Ca(OH)2), and carbonated lime putty (mainly CaCO3). Based on the results, we shed light mainly onto these two questions: (1) Does CaO have a Raman spectrum? (2) Which features in the spectra are luminescence bands that could be (and already have been) misinterpreted as Raman bands? We proof our assignment of luminescence bands in lime phases by using three different laser wavelengths for excitation, and give hypotheses on the origin of the luminescence as well as practical advices on how to identify these misleading features in Raman spectra. This article is mainly addressed to users of Raman spectroscopy in different fields of material analysis who might not be aware of the presence of interfering bands in their spectra. KW - (Free) lime KW - Lime cycle KW - Lime phases KW - Calcium compounds KW - Luminescence PY - 2015 DO - https://doi.org/10.1002/jrs.4622 SN - 0377-0486 SN - 1097-4555 VL - 46 IS - 1 SP - 141 EP - 146 PB - Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-32559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Ferruginous phases in 19th century lime and cement mortars: A Raman microspectroscopic study N2 - Raman microscopic imaging was just recently introduced into the analysis of residual Roman and Portland cement grains in 19th century cement stone, displaying evidence of the experimental adaptation of contemporary technological knowledge and practice to local circumstance. Beyond calcium ferrites, this study deals with ferruginous clinker phases that are atypical compared to present-day commercial conditions of manufacture, such as iron oxides, clinopyroxenes or pyroxenoids. Analog, microtexture, mineralogy and chemical composition of pulverized ferrosilicate slag used in the course of the 19th century as mineral additive in lime mortar reflect local resource utilization, recording the melting history within the furnace and the effectiveness of the reduction process of a single smelting event. In the case of the discussed example, chemical imaging by Raman microscopy allowed deducing a lime-rich, low-silica melt exposed to fairly reducing conditions because of the detection of the pyrometallurgic phases fayalite (Fe2SiO4), kirschsteinite (CaFeSiO4) and calcioolivine (Ca2SiO4) in zoned olivine laths and (with the melilite gehlenite, Ca2Al2SiO7) in the Interstitial matrix, cross-cut by dendritic wuestite (FeO). The presented analytical approach faces the high spatial complexity of such mortar samples by microspectroscopic imaging with micrometer lateral resolution and their chemical complexity by extracting the rich chemical information content from Raman spectra. Intensity maps of marker bands provide spatial phase distributions. Furthermore, maps of peak positions can give access to the dissemination of spectroscopically similar phases of solid solution series (e.g., olivine and calcium Aluminate ferrite) as well as varying amounts of incorporated foreign cations (e.g., in hematite). KW - Residual cement grains KW - Ferrite KW - Iron oxide KW - Slag KW - Olivine KW - Raman microspectroscopy PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.04.009 SN - 1044-5803 SN - 1873-4189 VL - 129 SP - 9 EP - 17 PB - Elsevier AN - OPUS4-40039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Neubauer, J. A1 - Goetz-Neunhoeffer, F. A1 - Schmid, Thomas T1 - Calcium aluminates in clinker remnants as marker phases for various types of 19th-century cement studied by Raman microspectroscopy N2 - In the second half of the 19th century, Roman and Portland cements played an essential role as active hydraulic binder material in building construction and façade ornamentation. Size and heterogeneous phase assemblage of unhydrated cement clinker remnants in historical cement stone differ significantly from those of remnants occurring in modern Portland cement clinker burnt in rotary kilns due to limitations of the production technology available in the 19th century (e.g., comminution and homogeneity of the feedstock, burning temperature and regime in the intermittently operated shaft kilns, grinding machinery). In the common analytical approach, thin sections and fracture surfaces of historical Roman and Portland cement mortars are characterised regarding their mineralogical composition and microstructure using optical and electron microscopic imaging techniques. Raman microspectroscopy can be additionally employed for petrographic examination, overcoming some limitations of the methods used so far. The determination of the phase content of residual cement clinker grains in the hydrated matrix allows for the differentiation of Roman and Portland cement binders. As marker phases, we propose the calcium aluminates CA, C12A7, C2AS and C3A – besides the commonly used calcium silicates C2S and C3S – because of their different formation temperatures and stability fields. This study focuses on the identification of different calcium aluminate and aluminoferrite phases in clinker remnants in samples of cast ornaments of three buildings in Switzerland raised between 1875 and 1893; the obtained Raman spectra are compared with fingerprint spectra of the corresponding pure, synthesised clinker phases collected with the same instrument for an unambiguous data interpretation. In addition to these phases, mainly minerals showing no hydraulic activity, such as, wollastonite CS, rankinite C3S2, free lime, portlandite, iron oxides, garnets, augite, albite and feldspathoids have been identified in the sampled historical cement stones by Raman microspectroscopy. As there is a strong relationship between coexisting clinker phases and the chemical composition of the raw meal as well as the burning and cooling history during clinkering, the results can help in understanding the physical and mechanical characteristics of historical cement mortars. This knowledge is fundamental for the choice and the formulation of appropriate repair materials with tailored properties employed in the field of restoration and preservation of the architectural heritage of the 19th and early 20th centuries. KW - Roman cement KW - Meso Portland cement KW - Portland cement KW - Clinker relicts KW - Raman microspectroscopy PY - 2016 DO - https://doi.org/10.1127/ejm/2016/0028-2577 SN - 0935-1221 SN - 1617-4011 VL - 28 IS - 5 SP - 907 EP - 914 AN - OPUS4-39046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang A1 - Lippitz, Andreas A1 - Gross, Thomas A1 - Rohrer, P. A1 - Saur, W. A1 - Erdmann, J. A1 - Gorsler, H.-V. ED - Mittal, K. L. T1 - The improvement in adhesion of polyurethane-polypropylene composites by short-time exposure of polypropylene to low and atmospheric pressure plasmas KW - Polyurethane-polypropylene adhesion KW - Low pressure plasma pretreatment KW - Atmospheric pressure plasma treatment KW - Short-time exposure KW - Relevance of functional groups to adhesion KW - Molecular orientation at polymer surfaces PY - 1996 SN - 90-6764-201-0 SP - 49 EP - 72 PB - VSP CY - Utrecht AN - OPUS4-7007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang A1 - Lippitz, Andreas A1 - Gross, Thomas A1 - Rohrer, P. A1 - Saur, W. A1 - Erdmann, J. A1 - Gorsler, H.-V. T1 - The improvement in adhesion of polyurethane-polypropylene composites by short-time exposure of polypropylene to low and atmospheric pressure plasmas KW - Polyurethane-polypropylene adhesion KW - Low pressure plasma pretreatment KW - Atmospheric pressure plasma treatment KW - Short-time exposure KW - Relevance of functional groups to adhesion KW - Molecular orientation at polymer surfaces PY - 1995 SN - 0169-4243 SN - 1568-5616 VL - 9 IS - 5 SP - 575 EP - 598 PB - VNU Science Press CY - Utrecht AN - OPUS4-7010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Almagro, J.-F. A1 - Busch, P. A1 - Gohil, D. D. A1 - Saunders, S. R. J. A1 - Sloof, W. G. A1 - Thiot, J.-F. A1 - Schneider, H. A1 - Whitwood, M. A1 - Wirth, Thomas T1 - Electron-Probe MICROanalysis of LighT Elements - Measurement Methods and Certified Reference Materials (MICROLITE) PY - 2000 IS - 266 SP - 1 EP - 35 PB - National Physical Laboratory CY - Teddington, Middlesex AN - OPUS4-6843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kuhmann, J. A1 - Harde, P. A1 - Pech, O. A1 - Pittroff, W. A1 - Preuß, A. A1 - Adolphi, B. A1 - Wirth, Thomas A1 - Österle, Werner ED - Reichl, H. T1 - Fluxless flip-chip bonding for the photonic assembly - comparison between evaporated SnPb (60/40) and AuSn (80/20) solder T2 - 5th International Conference on Micro-Electro-, -Opto-, -Mechanical Systems and Components CY - Potsdam, Germany DA - 1996-09-17 PY - 1996 SN - 3-8007-2200-3 VL - 5 SP - 91 EP - 97 PB - VDE-Verl. CY - Berlin AN - OPUS4-2544 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 - GEN A1 - Hieronymus, Hartmut A1 - Kasch, Thomas A1 - Fomin, P. A1 - Trotsyuk, A. ED - Doerffer, P. T1 - Modeling of film and surface detonations T2 - 5th International Symposium on Experimental and Computational Aerothermodynamics of Internal Flows ; 5th ISAIF CY - Gdansk, Poland DA - 2001-09-04 PY - 2001 SN - 83-88237-35-7 VL - 2 SP - 935 EP - 943 PB - IFFM Publ. CY - Gda´ nsk AN - OPUS4-1157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stadthaus, Meinhard A1 - Thomas, Hans-Martin A1 - Migoun, N. A1 - Porkhorenko, P. A1 - Gnusin, A. ED - Thompson, D. T1 - On the Reliability of the Quantitative Evaluation of Penetrant Systems Quality N2 - The market of the penetrant systems is increasing every year. A sensitivity of the penetrant systems is one of the main criteria for a customer. Therefore the importance of reliable result of the determination of penetrant systems sensitivity is increasing as well. It was established in our experiments that repeating the procedure of type testing in accordance with ISO EN 3452-2, in many cases one can obtain rather variable results for the sensitivity level. The goal of our investigations was to establish the principal factors, influencing upon the result of penetrant system type testing. Our results show that the values of the duration of such penetrant inspection technological stages as penetrant and developer applications may be considerably lower than the values recommended by ISO EN 3452-2 for the type testing. At the same time the character of the procedure's realisation of excess penetrant removal and developer application strongly influences upon the type testing results. Some recommendations for obtaining more reliable results of the determination of penetrant system sensitivity are worked out and proposed. ©2002 American Institute of Physics. T2 - 28th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Brunswick, ME, USA DA - 2001-07-29 PY - 2001 SN - 0-7354-0061-X DO - https://doi.org/10.1063/1.1473037 SN - 0743-0760 SN - 0094-243X N1 - Serientitel: AIP conference proceedings – Series title: AIP conference proceedings IS - 615 SP - 1991 EP - 1996 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-1531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller-Rochholz, J. A1 - Bronstein, Z. A1 - Schröder, Hartmut A1 - Rybak, Thomas A1 - Zeynalov, Eldar A1 - v. Maubeuge, K. P. ED - Delmas, P. T1 - Long-term behaviour of geosynthetic drains - excavations on landfills after up to 12 years service T2 - 7th International Conference on Geosynthetics (ICG) CY - Nice, France DA - 2002-09-22 PY - 2002 SN - 90-5809-525-8 VL - 2 SP - 565 EP - 568 PB - Balkema CY - Lisse AN - OPUS4-1902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Editorial for the special issue "Modern Raman spectroscopy of minerals" N2 - Raman spectroscopy provides vibrational fingerprints of chemical compounds enabling their unambiguous identification. The assignment of Raman spectra to minerals is straightforward, if appropriate reference data is accessible. Modern couplings of Raman spectroscopy with microscopy (Raman microspectroscopy) merge the high structural specificity with down to sub-micrometre spatial resolution. This analytical tool has high potential not only in the identification of minerals from natural sources but also for studying the complex microstructure and mineral distribution of both ancient and modern man-made materials. In addition to the chemical identity of minerals, Raman spectra are affected by crystal orientations (varying relative Raman band intensities); (sub)stoichiometric compositional changes (e.g., in solid solution series), traces of foreign ions, strain (the latter three shifting Raman bands); and crystallinity (changing Raman band widths), enabling a comprehensive physico-chemical characterisation of minerals. Thus, Raman spectroscopy – including its in situ measurement capabilities – provides possibilities to study mineral paragenesis in both, natural and man-made samples at the micrometre scale. While in 1928 the first experimental evidence for inelastic light scattering was provided by C. V. Raman and K. S. Krishnan by using sunlight for excitation, filters for selecting the inelastically scattered light, and their eyes for detection (later, photographic plates for acquisition of spectra were employed), modern Raman spectrometers make use of laser excitation, dispersive spectrographs and charge coupled device (CCD) detection. This Special Issue includes technological developments and applications in the field of modern Raman spectroscopy of minerals in a broad sense, from natural mineral deposits and archaeological objects to inorganic phases in man-made materials. The studied minerals include fossil resins, typical rock-forming minerals (calcite, quartz, forsterite), iron-sulphur species (e.g., mackinawite), a range of sulphates (gypsum, bassanite, anhydrite III, anhydrite II, celestine, barite, ternesite), as well as silicate minerals like garnets (e.g., almandine). KW - Raman spectroscopy KW - Raman microspectroscopy KW - Mineral identification KW - Physico-chemical characterisation of minerals KW - Mineral paragenesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515041 DO - https://doi.org/10.3390/min10100860 VL - 10 SP - 860 PB - MDPI CY - Basel AN - OPUS4-51504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Jungnickel, Robert A1 - Dariz, P. T1 - Insights into the CaSO4–H2O System: A Raman-Spectroscopic Study N2 - Even though being the subject of natural scientific research for many decades, the system CaSO4–H2O, consisting of the five crystalline phases gypsum, bassanite, and the anhydrites III, II, and I, has left many open questions for research. Raman spectroscopy was used because of its structural sensitivity and in situ measurement capability to obtain further insight by studying phase transitions in both ex situ and in situ experiments. The findings include significant contributions to the completeness and understanding of Raman spectroscopic data of the system. The dehydration path gypsum–bassanite–anhydrite III was shown to have strong parallels to a physical drying process, which depends on many parameters beyond the burning temperature. Raman band width determination was demonstrated to enable the quantitative discrimination of α-bassanite and β-bassanite as well as the postulated three sub-forms of anhydrite II (AII), which are all based on differences in crystallinity. In the latter case, the observed continuous structural variations over increasing burning temperatures were elucidated as a combination of decreasing surface areas and healing of crystal lattice defects. We propose an only two-fold sub-division of AII into reactive “disordered AII” and much less reactive “crystalline AII” with a transition temperature of 650°C ± 50 K. KW - Gypsum KW - Bassanite KW - Hemihydrate KW - Anhydrite KW - Raman spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506701 DO - https://doi.org/10.3390/min10020115 SN - 2075-163X VL - 10 IS - 2 SP - 115, 35 PB - MDPI CY - Basel AN - OPUS4-50670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Demidov, Alexandr A1 - Eschlböck-Fuchs, S. A1 - Kazakov, Alexander Ya. A1 - Gornushkin, Igor B. A1 - Kolmhofer, P. J. A1 - Pedarnig, J. D. A1 - Huber, N. A1 - Heitz, J. A1 - Schmid, Thomas A1 - Rössler, R. A1 - Panne, Ulrich T1 - Monte Carlo standardless approach for laser induced breakdown spectroscopy based on massive parallel graphic processing unit computing N2 - The improved Monte-Carlo (MC) method for standard-less analysis in laser induced breakdown spectroscopy (LIBS) is presented. Concentrations in MC LIBS are found by fitting model-generated synthetic spectra to experimental spectra. The current version of MC LIBS is based on the graphic processing unit (GPU) computation and reduces the analysis time down to several seconds per spectrum/sample. The previous version of MC LIBS which was based on the central processing unit (CPU) computation requested unacceptably long analysis times of 10's minutes per spectrum/sample. The reduction of the computational time is achieved through the massively parallel computing on the GPU which embeds thousands of co-processors. It is shown that the number of iterations on the GPU exceeds that on the CPU by a factor > 1000 for the 5-dimentional parameter space and yet requires > 10-fold shorter computational time. The improved GPU-MC LIBS outperforms the CPU-MS LIBS in terms of accuracy, precision, and analysis time. The performance is tested on LIBS-spectra obtained from pelletized powders of metal oxides consisting of CaO, Fe2O3, MgO, and TiO2 that simulated by-products of steel industry, steel slags. It is demonstrated that GPU-based MC LIBS is capable of rapid multi-element analysis with relative error between 1 and 10's percent that is sufficient for industrial applications (e.g. steel slag analysis). The results of the improved GPU-based MC LIBS are positively compared to that of the CPU-based MC LIBS as well as to the results of the standard calibration-free (CF) LIBS based on the Boltzmann plot method. KW - Monte Carlo simulation KW - Parallel computing KW - Calibration-free laser-induced breakdown spectroscopy KW - Post-breakdown laser induced plasma KW - Quaternary oxides PY - 2016 DO - https://doi.org/10.1016/j.sab.2016.09.016 VL - 125 SP - 97 EP - 102 PB - Elsevier B.V. AN - OPUS4-38489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Strehlow, P. A1 - Banach, Ulrich A1 - Hübert, Thomas T1 - Keramische Tieftemperatursensoren KW - Tieftemperatursensor KW - Keramik KW - Sensor PY - 1996 VL - 1995 SP - 274 EP - 275 CY - Braunschweig AN - OPUS4-691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Czerwensky, Michael A1 - Birkholz, M. A1 - Kanschat, P. A1 - Weiss, Thomas A1 - Lips, K. T1 - Low-temperature electron-paramagnetic-resonance study of extrinsic and intrinsic defects in CuGaSe2 KW - Electron-paramagnetic resonance KW - EPR PY - 1999 SN - 1098-0121 SN - 0163-1829 SN - 0556-2805 SN - 1095-3795 SN - 1550-235X VL - 59 IS - 19 SP - 12268 EP - 12271 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eschlböck-Fuchs, S. A1 - Huber, N. A1 - Ahamer, C. M. A1 - Hechenberger, J. G. A1 - Kolmhofer, P. J. A1 - Heitz, J. A1 - Rössler, R. A1 - Demidov, Alexander A1 - Schmid, Thomas A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Pedarnig, J. D. T1 - Application of laser-induced breakdown spectroscopy for the analysis of slags in industrial steel production N2 - Laser-induced breakdown spectroscopy (LIBS) is a fast and versatile technique for (semi) quantitative element analysis of solids, liquids, gases, and particulate matter. The LIBS method is used for optical sensing in various branches of industrial production. In the contribution we review some of our recent results on LIBS analysis of slags from secondary metallurgy in industrial steel making. Major oxides in steel slags are measured at-line and after homogenization using a calibration-free (CF) method. Two approaches for CF analysis based on the Boltzmann plot method and on the calculation of synthetic spectra are compared for the analysis of quaternary oxides. We also present the research in cooperation with our industrial partners in the process-analytical chemistry network PAC. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Vienna, Austria DA - 30.11.2015 KW - Laser-induced breakdown spectroscopy (LIBS) KW - Process analytical technology KW - Steel slag PY - 2015 PB - Plandruck+ Gesellschaft m.b.H. CY - Wien AN - OPUS4-39005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, A. A1 - Lischeid, G. A1 - Koch, Matthias A1 - Lentzsch, P. A1 - Sommerfeld, Thomas A1 - Müller, M.H. T1 - Co-Cultivation of Fusarium, Alternaria, and Pseudomonas on Wheat-Ears Affects Microbial Growth and Mycotoxin Production N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads. Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9). Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies. KW - Antagonists KW - Microbe interactions KW - Mycotoxins KW - Priority effect KW - SOM-SM PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521554 DO - https://doi.org/10.3390/microorganisms9020443 VL - 9 IS - 2 SP - 443 PB - MDPI AN - OPUS4-52155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krenek, S. A1 - Eisermann, R. A1 - Failleau, G. A1 - Lu, Xin A1 - Thomas, P. A1 - Kjeldsen, H. A1 - Anhalt, K. T1 - Fibre-optic thermometry to support the clean energy transition N2 - The measurement and control of temperature plays a key role in achieving the European Green Deal targets for a low carbon energy system. Fibre-optic thermometry is an emerging technology that can improve temperature measurement in extreme environments for energy providers and industry due to its distributed sensing and immunity to electromagnetic fields. Various applications for optimisation and monitoring in the energy sector are described, covering the whole range from energy generation to transmission and consumption. However, fibre-optic thermometers have cross sensitivities to other quantities (e.g., strain and humidity) and ageing effects that need to be investigated, quantified and minimised to obtain traceable and reliable measurements. This is particularly important so that applications in critical infrastructure can benefit from future measurements that are not possible with conventional sensors. The European INFOTherm project aims to overcome the limitations that currently prevent the widespread use of fibre-optic thermometry by creating a dedicated European metrology infrastructure for research, development and calibration. First results on measurement uncertainty, improvement of measurement techniques and practical field tests are presented. KW - Industrial processes optimisation KW - Fibre-optic thermometry KW - Distributed temperature sensing KW - Traceability KW - Thermal energy storage KW - Electrical grid resilience PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640075 DO - https://doi.org/10.1515/teme-2025-0044 SN - 2196-7113 VL - 92 IS - 9-10 SP - 392 EP - 405 PB - De Gruyter Brill AN - OPUS4-64007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni A1 - Onel, Yener A1 - Wolk, Thomas A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Müller, Bernd R. T1 - Evaluating porosity in cordierite diesel particulate filter materials: advanced X-ray techniques and new statistical analysis methods T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 2014-10-06 KW - Porous ceramics KW - Diesel particulate filters KW - Pore orientation KW - X-ray computed tomography KW - X-ray refraction KW - DIVA algorithm KW - Phase contrast KW - Edge artefact KW - Soft matter radiography KW - Wavelet transform KW - Huygens elementary waves PY - 2014 SN - 978-80-214-5018-9 SP - 1 EP - 8(?) AN - OPUS4-31973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Ehrig, Karsten A1 - Haarring, Holger A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Meinel, Dietmar A1 - Müller, Bernd R. A1 - Onel, Yener A1 - Staude, Andreas A1 - Wolk, Thomas T1 - Industrial and synchrotron X-ray CT applications for materials characterisation N2 - The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. We shall show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. We will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces. T2 - iCT Conference 2014 - Conference on industrial computed tomography CY - Wels, Austria DA - 25.02.2014 KW - X-ray absorption and refraction CT KW - Quantitative image analysis KW - Statistical analysis KW - Complex microstructure PY - 2014 SN - 978-3-8440-2557-6 SP - 15 EP - 31 PB - Shaker CY - Aachen AN - OPUS4-30484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Xin A1 - Christensen, J. A1 - Thomas, P. A1 - Failleau, G. A1 - Eisermann, R. A1 - Hicke, Konstantin A1 - Krenek, S. T1 - Fiber artefact for performance evaluation of time domain distributed fiber sensor interrogators N2 - Distributed fiber sensing (DFS) is a powerful tool for structural health monitoring (SHM), allowing continuous and seamless measurements of temperature and strain along the fiber. The spatial accuracy of a DFS interrogator, as a key parameter of the system, is vital for precisely locating structural perturbations or defects. Its evaluation and calibration methods however attract little attention. A fiber optic artefact based on a fiber loop is developed to evaluate distance accuracy and signal quality for both self-developed and commercial sensing systems based on Rayleigh, Raman, and Brillouin scattering effects, respectively. The measured distance is corrected to remove the influence of the pulse width. Additionally, the obtained SNRs are compared for different loop trips and pulse widths, assisting to assess signal quality for SHM applications. KW - Structural health monitoring KW - Distributed fiber sensing KW - Distributed temperature sensing KW - Fiber artefact KW - Spatial correction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648966 DO - https://doi.org/10.1088/1361-6501/ae214e VL - 36 IS - 11 SP - 1 EP - 10 PB - IOP Publishing Ltd CY - Bristol, UK AN - OPUS4-64896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiler, Geraldine A1 - Hübner, Wolfgang A1 - Gradt, Thomas A1 - Klein, P. A1 - Friedrich, K. T1 - Friction and wear of PTFE composites at cryogenic temperatures N2 - This paper presents investigations on the tribological behaviour of PTFE composites against steel at cryogenic temperatures. The results showed that the friction coefficient decreases with temperature down to 77 K, but did not follow a linear evolution further down to extreme low temperatures. It can be stated that the cryogenic environment has a significant influence on the tribological performance of the polymer composites. The effect of low temperatures was more clearly detected at low sliding speed, where friction heat is reduced. A change in wear mechanism from adhesive to abrasive was observed in this case. SEM and AFM analyses showed that the PTFE matrix composites investigated under these experimental conditions have transferred material onto the disc down to very low temperatures. Chemical analyses indicate the presence of iron fluorides. KW - PTFE composites KW - Cryogenic tribology KW - Transfer film PY - 2002 DO - https://doi.org/10.1016/S0301-679X(02)00035-X SN - 0301-679X VL - 35 IS - 7 SP - 449 EP - 458 PB - Butterworth-Heinemann CY - Oxford AN - OPUS4-1866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiler, Geraldine A1 - Hübner, Wolfgang A1 - Gradt, Thomas A1 - Klein, P. T1 - Friction and Wear of Carbon Fibre Filled Polymer Composites at Room and Low Temperatures PY - 2004 SN - 0933-5137 SN - 1521-4052 VL - 35 IS - 10/11 SP - 683 EP - 689 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-6866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Mayr, P. A1 - Nitsche, A. A1 - Mente, Tobias A1 - Böllinghaus, Thomas T1 - Hydrogen diffusion in creep-resistant 9% Cr P91 multi-layer weld metal N2 - Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot be excluded, and hydrogen removal should be done before PWHT. KW - Creep resisting materials KW - Diffusion KW - Hydrogen KW - Weld metal KW - Post weld heat treatment KW - Microstructure PY - 2020 DO - https://doi.org/10.1007/s40194-019-00828-8 SN - 0043-2288 VL - 64 IS - 2 SP - 267 EP - 281 PB - Springer AN - OPUS4-50471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Phase composition and burning history of high-fired medieval gypsum mortars studied by Raman microspectroscopy N2 - The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Not hydrated clusters of firing products preserved in the binder matrix are a typical feature of such mortars. A novel Raman microspectroscopic approach, providing access to the burning history of individual anhydrite grains, was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for tracing and visualising pyrometamorphic reactions in natural impurities of the kiln run. In the discussed examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 to periclase MgO and lime CaO yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Hydration of periclase in the mixed gypsum paste containing sulphate ions also resulted in magnesium sulphate hydrates, here identified in the form of hexahydrite MgSO4·6H2O. Lower burning temperatures left the accessory minerals in their pristine form, but can be traced by measuring the spectra of individual anhydrite crystals in grains of firing products and evaluating Raman band widths. Throughout the present study, calcination temperatures ranging from approx. 600°C to 900°C were determined. KW - High-fired gypsum mortar KW - Anhydrite KW - Dolomite KW - Forsterite KW - Raman microspectroscopy PY - 2019 DO - https://doi.org/10.1016/j.matchar.2019.03.013 VL - 151 SP - 292 EP - 301 PB - Elsevier Inc. AN - OPUS4-48102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Hentschel, Manfred P. A1 - Onel, Yener A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Wolk, Thomas A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Müller, Bernd R. T1 - Bewertung von Porositätsparametern in Cordierit-Diesel-Partikelfilter-Materialien mit fortgeschrittenen Röntgenverfahren und statistischer Analyse N2 - Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Cordierit KW - Poröse Keramik KW - Porenorientierung KW - Röntgenrefraktion KW - Computer-Tomographie KW - 3D-Mikrostruktur PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-312946 SN - 978-3-940283-61-0 VL - 148 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31294 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Borghetti, P. A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Garcia, S. A1 - Gómez, E. A1 - Blanco, M. A1 - Alberto, G. A1 - Martra, G. T1 - Organic surface modification and analysis of titania nanoparticles for self‐assembly in multiple layers N2 - The characteristics of TiO2 coatings can greatly influence their final performance in large‐scale applications. In the present study, self‐assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with, for example, silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3‐aminopropyl)triethoxysilane (APTES) or (3‐aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino‐groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape, and specific surface area have been functionalized. Fourier‐transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), SEM/ energy‐dispersive X‐ray spectroscopy (EDS), XPS, Auger electron spectroscopy (AES), and Time‐of‐Flight (ToF)‐SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA. KW - TiO2 KW - Nanoparticles KW - Surface functionalization KW - Layer-by-layer deposition KW - Surface chemical analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508601 DO - https://doi.org/10.1002/sia.6842 SN - 1096-9918 VL - 52 IS - 12 SP - 829 EP - 834 PB - John Wiley & Sons Ltd AN - OPUS4-50860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Dariz, P. ED - Ziemann, M. T1 - Raman band widths of anhydrite II reveal the burning history of high-fired medieval gypsum mortars N2 - The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Because of the absence of medieval textbooks, the observation of high-temperature, low-pressure mineral transformations and the correlation of phases coexisting in not hydrated binder relicts in the gypsum matrix to the mineralogy of the raw material and the burning conditions constitute the only source to the historical technological know-how. The CaSO4–H2O system consists of five crystalline phases, which can be discriminated by structural analysis methods, such as Raman spectroscopy, due to obvious differences in their spectroscopic data: gypsum (CaSO4 ⋅ 2 H2O), bassanite (hemihydrate, CaSO4 ⋅ ½ H2O), anhydrite III (CaSO4), anhydrite II (CaSO4), and anhydrite I (CaSO4). Only recently, it was possible to demonstrate that small spectroscopic variations exist also within the relatively large stability range of anhydrite II from approx. 180°C to 1180°C: all Raman bands narrow with increasing burning temperature applied in the synthesis from gypsum powder. The determination of band widths of down to 3 cm-1 and differences between them of a few tenths of a wavenumber is not a trivial task. Thus, this contribution discusses peak fitting and strategies for correction of instrument-dependent band broadening. Raman maps of polished thin sections of gypsum mortars provide access to the burning histories of individual remnant thermal anhydrite grains and enable the discrimination of natural anhydrite originating from the gypsum deposit. This novel analytical method was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for following pyrometamorphic reactions in natural impurities of the raw material. In the presented examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Lower burning temperatures, which leave the accessory minerals in their pristine form, can be traced by measuring the spectra of anhydrite crystalites in grains of firing products and evaluating Raman band widths. Throughout the applications of this analytical method so far, calcination temperatures ranging from approx. 600°C to 900°C were determined. T2 - 10th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Potsdam, Germany DA - 03.09.2019 KW - Raman microspectroscopy KW - High-fired medieval gypsum mortars KW - Raman band width KW - Gypsum dehydration KW - Thermal anhydrite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496204 SP - 36 EP - 37 PB - University of Potsdam CY - Potsdam AN - OPUS4-49620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Jungnickel, R. A1 - Dariz, P. T1 - Raman band widths of anhydrite II reveal the burning history of high‐fired medieval gypsum mortars N2 - When used as a mineral binder, gypsum is thermally dehydrated and mixed with water, resulting in a paste hardening in the backreaction to calcium sulphate dihydrate (CaSO4 · 2 H2O). Although nowadays mainly hemihydratebased (CaSO4 · ½ H2O) binders are employed, higher firing temperatures in medieval kilns yielded anhydrite II (CaSO4). Except for the discrimination of the metastable phases anhydrite III and I due to different crystal structures, variations within the production temperature range of anhydrite II (approximately 300 to 1180°C) were not analytically accessible until recently. This study describes the development of an analytical technique, which is based on steady changes of band widths in room‐temperature Raman spectra of anhydrite II as a function of burning temperature. Raman microspectroscopic mapping experiments enable to pinpoint individual unreacted grains of thermal anhydrite in mortars and to discriminate them from natural anhydrites originating from the raw gypsum. The determination of band full widths at half maximum of down to 3 cm−1 and differences between them of a few tenths of wavenumbers is not a trivial task. Thus, a focus of this work is on peak fitting and strategies for correction of instrument‐dependent band broadening, which is often neglected also beyond the field of mortar analysis. Including other potential influences on band widths, burning temperatures of 400 to 900°C can be retraced in high‐fired medieval gypsum mortars with an uncertainty of approximately ± 50 K, as demonstrated with sample material of a stucco sculpture dated around 1400. KW - Analytical methods KW - Gypsum dehydration KW - High-fired gypsum mortar KW - Raman band width determination KW - Thermal anhydrite PY - 2019 DO - https://doi.org/10.1002/jrs.5632 SN - 1097-4555 VL - 50 IS - 8 SP - 1154 EP - 1168 PB - Wiley AN - OPUS4-48757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -