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Paper des Monats
- ja (62)
Ancient papyri are a written heritage of culture that flourished more than 3000 years ago in Egypt. One of the most significant collections in the world is housed in the Egyptian Museum and Papyrus Collection in Berlin, from where the samples for our investigation come. The papyrologists, curators and conservators of such collections search intensely for the analytical detail that would allow ancient papyri to be distinguished from modern fabrications, in order to detect possible forgeries, assess papyrus deterioration state, and improve the design of storage conditions and conservation methods. This has become the aim of our investigation. The samples were studied by a number of methods, including spectroscopic (FTIR, fluorescent-FS, Raman) diffractional (XRD) and chromatographic (size exclusion chromatography-SEC), selected in order to determine degradation parameters: overall oxidation of lignocellulosic material, degree of polymerization and crystallinity of cellulose. The results were correlated with those obtained from carefully selected model samples including modern papyri and paper of different composition aged at elevated temperature in humid air. The methods were classified in the order SEC > FS > FTIR > XRD, based on their effectiveness in discriminating the state of papyri degradation. However, the most trustworthy evaluation of the age of papyri samples should rely on several methods.
The study deals with the application of the high-power hybrid-laser arc welding process on up to 15 mm thick pipe segments with the intention to avoid end crater imperfections during closing of the circumferential welds, where the pipes were turned during welding in 1G- and 2Gpositions.
Different techniques such as laser power ramp-down, abrupt switch-off of the laser power and change of the magnification of the laser spot diameter and defocusing of the laser beam relative to the workpiece were tested to remove the laser energy from the process. It could be shown that a high defocusing of the optic system above 40 mm with a resulting beam diameter > 2.9 mm in a short overlap length of approx.
20 mm leads to the formation of a cup-shaped weld seam, which is preferred for avoidance of cracks and pores in the end crater. A laser optics with motor-driven lens system was used for the welding experiments to defocuse the laser beam without changing the position of the arc.
The study deals with the influence of the heat input and the resulting cooling times on the microstructure and Charpy impact toughness of single-pass laser hybrid welded 20-mm thick high-strength steel S690QL. The main focus is on the change of the mechanical properties over the entire seam thickness. The cooling times were measured in-situ using a pyrometer and an optical fibre in three different depths of the seam where Charpy impact test specimens were also later taken. Thereby, three different heat inputs from 1.3 kJ/mm to 2 kJ/mm were investigated. Despite the observed decreased values of both t8/5-cooling time and the Charpy impact toughness in the root part of the seam, the required impact toughness of 38 J/cm2 could be reached in dependance on applied heat input, especially at the heat input of 1.6 kJ/mm.
The study deals with the determination of the influence of an externally applied oscillating magnetic field on the melt pool dynamics in high power laser beam and hybrid laser arc welding processes. An AC magnet was positioned under the workpiece which is generating an upward directed electromagnetic force to counteract the formation of the droplets. To visualise the melt flow characteristics, several experiments were carried out using a special technique with mild steel from S355J2 with a plate thickness of up to 20 mm and a quartz glass in butt configuration. The profile of the keyhole and the melt flow were recorded with a highspeed camera from the glass side. Additionally, the influence of the magnetic field orientation to the welding direction on the filler material dilution on laser hybrid welding was studied with variating oscillation frequency. The element distribution over the whole seam thickness was measured with X-ray fluorescence (XRF). The oscillation frequency demonstrated a great influence on the melt pool dynamics and the mixing of the elements of the filler wire. The highspeed recordings showed, under the influence of the magnetic field, that the melt is affected under strong vortex at the weld root, which also avoids the formation of droplets.
One of the challenges of the high-power hybrid laser welding of thick steels is the sensitivity of the process of the process to manufacturing tolerances. This usually leads to a time-consuming preparation of the welding edges, such as milling. The study deals with the influence of the edge quality of milled and plasma-cut steel made of S355J2 with a wall thickness of 20 mm on the laser hybrid welded seam quality. Furthermore, the gap bridgeability and the tolerances towards edge misalignment was investigated. An AC magnet was used as backing support to prevent sagging and positioned under the workpiece, to generate an upwards directed electromagnetic pressure. The profiles of the edges and the gap on the top and root side were measured using a digital camera. Single-pass laser hybrid welds of plasma-cut edges could be welded using a laser beam power of just 13.7 kW. A gap bridgeability up to 2 mm and misalignment of edges up to 2 mm could be achieved successful. Additionally, the independence of the cutting side and the welding side was shown, so that samples were welded to the opposite side to their cutting. For evaluation of internal defects or irregularities, X-ray images were carried out. Charpy impact strength tests were performed to determine the toughness of the welds.
It is already known that the laser beam welding (LBW) or hybrid laser-arc welding (HLAW) processes are sensitive to manufacturing tolerances such as gaps and misalignment of the edges, especially at welding of thick-walled steels due to its narrow beam diameter. Therefore, the joining parts preferably have to be milled. The study deals with the influence of the edge quality, the gap and the misalignment of edges on the weld seam quality of hybrid laser-arc welded 20-mm-thick structural steel plates which were prepared by laser and plasma cutting. Single-pass welds were conducted in butt joint configuration. An AC magnet was used as a contactless backing. It was positioned under the workpiece during the welding process to prevent sagging. The profile of the edges and the gap between the workpieces were measured before welding by a profile scanner or a digital camera, respectively. With a laser beam power of just 13.7 kW, the single-pass welds could
be performed. A gap bridgeability up to 1 mm at laser-cut and 2 mm at plasma-cut samples could be reached respectively.
Furthermore, a misalignment of the edges up to 2 mm could be welded in a single pass. The new findings may eliminate the need for cost and time-consuming preparation of the edges.
The hybrid laser arc welding (HLAW) process provides many advantages such as improved gap bridgeability, deep penetration and misalignment of edges, that is why the process is used increasingly in industrial applications e.g. shipbuilding, power plant industry and line-pipe manufacturing. The obvious encountered problem for single pass welding in flat position is the gravity drop-out at low welding velocities. With the usage of an electromagnetic weld pool support system, which is based on generating Lorentz forces within the weld pool, wide seams followed by reduced welding velocities could be achieved in this study leading to the realization of a gap bridgeability up to 1 mm, misalignment of edges up to 2 mm and a single pass weld up to 28 mm thickness with a 20-kW fibre laser. These developments expand the boundaries of the HLAW process for different industrial applications. As a result, less accurate preparation of the edges would be sufficient, which saves time for manufacturing.
Hybrid laser-arc welding offers many advantages, such as deep penetration, good gap bridge-ability, and low distortion due to reduced heat input. The filler wire which is supplied to the process is used to influence the microstructure and mechanical properties of the weld seam.
A typical problem in deep penetration high-power laser beam welding with filler wire and hybrid laser-arc welding is an insufficient mixing of filler material in the weld pool, leading to a non-uniform element distribution in the seam. In this study, oscillating magnetic fields were used to form a non-conservative component of the Lorentz force in the weld pool to improve the element Distribution over the entire thickness of the material. Full penetration hybrid laser-arc welds were performed on 20-mm-thick S355J2 steel plates with a nickel-based wire for different arrangements of the oscillating magnetic field. The Energy-dispersive X-ray spectroscopy (EDS) data for the distribution of two tracing elements (Ni and Cr) were used to analyze the homogeneity of dilution of the filler wire.
With a 30° turn of the magnetic field to the welding direction, a radical improvement in the filler material distribution was demonstrated. This would lead to an improvement of the mechanical properties with the use of a suitable filler wire.
The laser hybrid welding process offers many advantages regarding deep penetration, increased welding velocity and with the help of the supplied filler wire an improved bridgeability to gap and misalignment tolerances. High power laser systems with a power of approx. 30 kW are already available on the market. Nevertheless, multi-layer technology with an arc process is still used for welding of plates from a thickness from 20 mm. A potential cause is the process instability with increasing laser power. It is inevitable that gravity drop-out due to the high hydrostatic pressure at increasing wall thickness especially at welding in flat position and with a low welding speed. The surface tension decreases with increasing root width resulting from low welding velocities. To prevent such inadmissible defects of the seam a use of weld pool support is required. Usual weld pool support systems such as ceramic or powder supports require a mechanical detachment which is time-consuming. The electromagnetic weld pool support system described in this work shows an alternative weld pool support which works contactless. It is based on generating Lorentz forces in the weld pool due to oscillating magnetic field and induced eddy currents. This innovative technology offers single pass welds up to 28 mm in flat position and reduced welding velocity with a laser power of just 19 kW. It also leads to improved mechanical-technological properties of the seams because of the slow cooling rate. With usage of an electromagnetic weld pool support the limitation of the hybrid laser arc welding process in the thick sheet metal will be extend.
The sliding behaviors of two simplified tribofilms with amorphous structure consisting either of SiO₂ molecules or C atoms were simulated by molecular dynamics modeling. The objective was to identify mechanisms explaining the experimentally observed lubricating properties of the two amorphous films. The impacts of layer thickness, normal pressure, temperature and different substrate materials were studied systematically, while the sliding velocity was kept constant at 30 m/s. While the layer thickness was not critical, all the other parameters showed special effects under certain conditions. Normal pressure impeded void formation and could even eliminate voids if applied at high temperature. Stick-slip sliding was changed to smooth sliding at high temperature due to void healing. Considering the carbon film, high friction forces and shearing of the entire film was observed with diamond substrates, whereas interface sliding at low friction forces and an amorphous layer of iron mixed with carbon was observed if the supporting substrates consisted of α-Fe. Both films show a decrease of friction forces and smooth sliding behavior at elevated temperature, corresponding well to the tribological behavior of and advanced nanocomposite sliding against a steel disc under severe stressing conditions when high flash temperatures can be expected.
Time-dependent in situ measurement of atmospheric corrosion rates of duplex stainless steel wires
(2018)
Corrosion rates of strained grade UNS S32202 (2202) and UNS S32205 (2205) duplex stainless steel wires have been measured, in situ, using time-lapse X-ray computed tomography. Exposures to chloride-containing (MgCl2) atmospheric environments at 50 °C (12–15 M Cl− and pH ~5) with different mechanical elastic and elastic/plastic loads were carried out over a period of 21 months. The corrosion rates for grade 2202 increased over time, showing selective dissolution with shallow corrosion sites, coalescing along the surface of the wire. Corrosion rates of grade 2205 decreased over time, showing both selective and pitting corrosion with more localised attack, growing preferentially in depth. The nucleation of stress corrosion cracking was observed in both wires.
Creep and creep damage behavior of stainless steel 316L manufactured by laser powder bed fusion
(2022)
This study presents a thorough characterization of the creep properties of austenitic stainless steel 316L produced by laser powder bed fusion (LPBF 316L) contributing to the sparse available data to date. Experimental results (mechanical tests, microscopy, X-ray computed tomography) concerning the creep deformation and damage mechanisms are presented and discussed. The tested LPBF material exhibits a low defect population, which allows for the isolation and improved understanding of the effect of other typical aspects of an LPBF microstructure on the creep behavior. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant of 316L was also tested. To characterize the creep properties, hot tensile tests and constant force creep tests at 600 °C and 650 °C are performed. The creep stress exponents of the LPBF material are smaller than that of the conventional variant. The primary and secondary creep stages and the times to rupture of the LPBF material are shorter than the hot rolled 316L. Overall the creep damage is more extensive in the LPBF material. The creep damage of the LPBF material is overall mainly intergranular. It is presumably caused and accelerated by both the appearance of precipitates at the grain boundaries and the unfavorable orientation of the grain boundaries. Neither the melt pool boundaries nor entrapped gas pores show a significant influence on the creep damage mechanism.
Characterization of Ti-6Al-4V fabricated by multilayer laser powder-based directed energy deposition
(2022)
Laser powder-based directed energy deposition (DED-L) is increasingly being used in additive manufacturing (AM). As AM technology, DED-L must consider specific challenges. It must achieve uniform volume growth over hundreds of layers and avoid heat buildup of the deposited material. Herein, Ti–6Al–4V is fabricated using an approach that addresses these challenges and is relevant in terms of transferability to DED–L applications in AM. The assessment of the obtained properties and the discussion of their relationship to the process conditions and resulting microstructure are presented. The quality of the manufacturing process is proven in terms of the reproducibility of properties between individual blanks and with respect to the building height. The characterization demonstrates that excellent mechanical properties are achieved at room temperature and at 400 °C.
As the most electronegative element, fluorine has a strong influence on material properties such as absorption behaviour or chemical and thermal stability. Fluorine can be easily integrated into coordination polymers (CPs) via a fluorinated acetate, here trifluoroacetate in Ba(CF3COO)2, or directly via a metal fluorine bond (BaF(CH3COO)). In the present study both possibilities of fluorine integration were tested and their effect on structure and properties of barium coordination polymers was investigated in comparison with the non-fluorinated barium acetate (Ba(CH3COO)2). In addition to the study of their thermal behaviour and their decomposition temperature, the CPs structures were tested for their application as possible anode materials in lithium ion batteries and for their sorption of water and ammonia. The properties of the CPs can be traced back to the individual structural motifs and could thus trigger new design ideas for CPs in LIBs and/or catalysis.
Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
This study investigates the mechanochemical reactions between AgBr 3-picolylamine and 4-picolylamine. The use of different stoichiometry ratios of the reagents allows [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n to be obtained, and we report the new structures of [(AgBr)2(3-pica)]n and [(AgBr)2(4-pica)]n which are characterized by the presence of the following: (a) infinite inorganic chains, (b) silver atom coordinated only by bromide atoms and (c) argentophilic interactions. Furthermore, we studied the interconversion of [(AgBr)(n-pica)]n/[(AgBr)2(n-pica)]n by mechanochemical and thermal properties. The in situ experiments suggest that [(AgBr)(3-pica)]n is kinetically favoured while [(AgBr)2(3-pica)]n is converted into [(AgBr)(3-pica)]n only with a high excess of the ligand. Finally, the liquid nature of the ligands is not sufficient to assist the grinding process, and the complete reaction is observed with the addition of a small quantity of acetonitrile.
The progress in X-ray detector electronics (sensitivity and speed) allows meanwhile fast single photon detection by a matrix detector. Combined photon counting and energy discrimination is implemented in the electronic circuit of each detector pixel. The company XCounter developed detectors based on CdTe single crystals, which can be tiled to larger areas and have a pixel size of 100ìm. The largest area available in beginning of 2014 is 50x75 mm². These detectors have very promising properties, which make them very suitable for NDT applications:
1. A CdTe attenuation layer of 750 µm thickness allows efficient X-ray detection up to ca. 300 keV. In counting mode only photon noise is important; no other detector noise sources need to be considered. There is no Offset signal without radiation.
2. Each of the detector pixels has two energy thresholds. These can be used for dual energy imaging for materials separation. Also the suppression of scattered radiation by energy thresholding will improve the image contrast sensitivity. First experiments will be presented which demonstrate the advantages of this new detector technology over the conventional charge integrating detectors.
A challenge is the development of a modified detector calibration procedure, which becomes critical at longer exposure times.
Since decades the evaluation of flaw indications on radiographs from welds or castings are based on well accepted reference film catalogues from organizations like IIW (weldments), ASTM (castings) or DGZfP (D5 recommendation on heavy steel castings). Today, the transformation of classical film radiography to the digital world is in full progress. Some ASTM standards do not permit the evaluation of digital radiographs in reference to film catalogues. Therefore, these reference film catalogues have to be converted into the digital age too. BAM is supporting this transition by high definition film scanning. The result is a corresponding reference image catalogue. The different standard organizations selected different ways to distribute the digital data. ASTM used high definition film scanning at 10 μm pixel size and distribution of a huge amount of high-res data via DVD. The user sub-samples these high-res data during catalogue import to the resolution of his system. The comparison is done by synchronized image viewing on the computer work station. IIW recently decided to distribute their ISO 5817 reference images installed on tablets, which are used for image viewing too. The tablet image has to be compared with the digital image on the system monitor. DGZfP transformed their D5 reference radiographs into a PDF for monitor viewing. This is the simplest and cheapest solution, but still allows the full usage of the catalogue in the digital era. The status of ongoing work in progress will be discussed.
In den letzten zwei Jahren wurden 11 neue Standards/Standardrevisionen zur RT veröffentlicht (ohne Strahlenschutz) und 5 werden dafür gestrichen. Es wird über die neuen Anforderungen ausgewählter Normen bzw. Normrevisionen informiert und insbesondere auch über die veränderten Parameter, die bei Prüfpraxis und bei der Klassifizierung zu berücksichtigen sind. Das wichtigste Projekt ist die Revision der DIN EN ISO 17636-1, -2, RT von Schweißverbindungen, in ISO TC 44 SC 5 WG 1. Die Standards zur Schweißnahtprüfung in der Kerntechnik, DIN 25435, wurden ins Englische übertragen und bei ISO TC 85 SC 6 bearbeitet. Hauptaktivität bei ASTM ist gegenwärtig die Überarbeitung der CT-Standards und die Berücksichtigung der Anforderungen an das dimensionelle Messen. Der Guide ASTM E 1441 zur Bestimmung von MTF, Kontrast-Detail-Funktion (CDF) und Kontrast-Diskrimination-Diagramm (CDD) wird revidiert. E 2445 zur CR Long Term Stability wird ebenfalls revidiert. Die Revision soll auch in die ISO 16371-1 eingehen. Dazu ist ein Round Robin-Test geplant. Auch die Standards zur Durchstrahlungsprüfung auf Korrosion und Ablagerungen in Rohren mit Röntgen- und Gammastrahlen (EN 16407-1, -2, 2014) wurden revidiert. Diese Revision wurde als DIN EN ISO 20769-1, -2 2018 veröffentlicht und EN 16407 wird zurückgezogen. Die Revision der Standards EN 12543 und EN 12679 zur Messung der Brennfleckgröße und der Strahlergröße ist mit Verzögerung in Überarbeitung, um die digitalen Detektoren und Messmöglichkeiten mit Bildverarbeitungsprogrammen zu berücksichtigen. Ein Entwurf zur Messung der Brennfleckgröße von nano-Fokusröhren wird derzeit vom Europäischen Metrologie-Programm EMPIR gefördert. Zur radiographischen Gussteilprüfung wurde der Standard EN 12681 revidiert und 2018 veröffentlicht. Er wurde um Zulässigkeitsgrenzen erweitert und die digitale Radiographie wurde in Teil 2 berücksichtigt.