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Organisationseinheit der BAM
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using
these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ∼3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ∼5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ∼4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. We also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration.
The lead authors failed to name two collaborators as co-authors. The authors listed should include:
Miss Claudia L. Compean-Gonzalez (ORCID:
0000-0002-2367-8450) and Dr. Giacomo Ceccone (ORCID:
0000-0003-4637-0771).
These co-authors participated in VAMAS project A27, provided data that were analyzed and presented in this publication (and supporting information), and reviewed the manuscript before submission.
CCQM key comparison K-129 for the quantitative analysis of Cu(In,Ga)Se2 (CIGS) films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of mole fractions of Cu, In, Ga and Se in a thin CIGS film. The measurand of this key comparison is the average mole fractions of Cu, In, Ga and Se of a test CIGS alloy film in the unit of mole fraction (mol/mol). Mole fraction with the metrological unit of mol/mol can be practically converted to atomic fraction with the unit of at%.
In this key comparison, a CIGS film with certified mole fractions was supplied as a reference specimen to determine the relative sensitivity factors (RSFs) of Cu, In, Ga and Se. The mole fractions of the reference specimen were certified by isotope dilution - inductively coupled plasma/mass spectrometry (ID-ICP/MS) and are traceable to the SI. A total number counting (TNC) method was recommended as a method to determine the signal intensities of the constituent elements acquired in the depth profiles by Secondary Ion Mass Spectrometry (SIMS), X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). Seven NMIs and one DI participated in this key comparison. The mole fractions of the CIGS films were measured by depth profiling based-SIMS, AES and XPS. The mole fractions were also measured by non-destructive X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX).
In this key comparison, the average degrees of equivalence uncertainties for Cu, In, Ga and Se are 0.0093 mol/mol, 0.0123 mol/mol, 0.0047 mol/mol and 0.0228 mol/mol, respectively. These values are much smaller than that of Fe in a Fe-Ni alloy film in CCQM K-67 (0.0330 mol/mol). This means that the quantification of multi-element alloy films is possible by depth profiling analysis using the TNC method.
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.
Infolge der Betriebsbeanspruchung unterliegen Eisenbahnschienen an
ihrer Fahrkante sog. Rollkontakt-Ermüdung. Diese entsteht bevorzugt in Bögen
durch eine Kaltverformung des Schienenstahls und zeigt sich anfänglich in einer erhöhten
Verfestigung des kontaktbeanspruchten Oberflächenbereichs. Im weiteren
Verlauf entstehen zahlreiche, flach in das Schieneninnere verlaufende Risse sog.
Head Checks. Diese Risse neigen ab einem gewissen Stadium dazu, in das Innere
der Schiene abzukippen, was im Endstadium zu einem Schienenbruch führen kann.
Seit einigen Jahren wird in Deutschland bei der DB AG das Wirbelstromverfahren
erfolgreich zur zerstörungsfreien Prüfung der Schädigungstiefe von Head Checks
eingesetzt. Hiermit wurde u. A. angestrebt, zuverlässige Planungsgrößen für den
Einsatz von Instandhaltungsmaßnahmen zu erhalten, durch deren gezielten Einsatz
ein weiteres Risswachstum wirkungsvoll unterbunden werden kann. Bereits bei einem
der ersten systematischen Einsätze der Wirbelstromprüfung an einer Bogenstrecke
mit hohem Betriebsaufkommen wurde auffällig, dass die Ermüdungsrisse
nicht gleichmäßig entlang des Bogens verteilt auftraten, sondern sich auf kurze Distanzen
Anhäufungen von Rissbefall mit intakten, unbefallenen Abschnitten abwechselten.
Solch wellenförmiges Auftreten von Head Checks wurde auch in den nachfolgenden
Prüfergebnissen der Wirbelstromprüfung vielerorts beobachtet. Aus der
Literatur war bekannt, dass sich die Ermüdungsrisse bevorzugt in verfestigten Materialzonen
bilden. Mit Hilfe von Härtemessungen konnte an verlegten und befahrenen
Schienen gezeigt werden, dass die unbefallenen Zonen etwa die Grundhärte des
Schienenwerkstoffes aufwiesen, während die mit Ermüdungsrissen befallenen Zonen
um ca. 10 25% erhöhte Härtewerte aufwiesen. Die Wirbelstromprüfung reagiert
sehr empfindlich auf Veränderungen der Materialeigenschaften. Somit lassen
sich Verfestigungen der o. g. Art leicht auch ohne jedes Vorhandensein von Ermüdungsrissen
bereits nachweisen. Im Zuge einer längerfristigen Beobachtung einer
neu gebauten Strecke konnte herausgefunden werden, dass sich nach einer gewissen
Betriebszeit wellenförmig verteilte Zonen mit Prüfsignalen, die auf Verfestigungen
schließen lassen auftraten. Im weiteren zeitlichen Ablauf bildeten sich Ermüdungsrisse
tatsächlich in den vorher bestimmten Stellen mit Verfestigung, während die
Zonen ohne diese Prüfsignale weitgehend rissfrei blieben. Diese Ergebnisse zeigen,
dass die Wirbelstromprüfung das Potential besitzt, mögliche Orte der Entstehung
von Ermüdungsrissen in einem extrem frühzeitigen Stadium nachzuweisen.
A pilot study for the quantitative surface analysis of multi-element alloy films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this pilot study is to ensure the equivalency in the measurement capability of national metrology institutes for the quantification of multi-element alloy films. A Cu(In,Ga)Se2 (CIGS) film with non-uniform depth distribution was chosen as a representative multi-element alloy film. The atomic fractions of the reference and the test CIGS films were certified by isotope dilution - inductively coupled plasma/mass spectrometry. A total number counting (TNC) method was used as a method to determine the signal intensities of the constituent elements, which are compared with their certified atomic fractions. The atomic fractions of the CIGS films were measured by various methods, such as Secondary Ion Mass Spectrometry (SIMS), Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), X-Ray Fluorescence (XRF) analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). Fifteen laboratories from eight National Metrology Institutes (NMIs), one Designated Institute (DI) and six non-NMIs participated in this pilot study. Although the average atomic fractions of 18 data sets showed rather poor relative standard deviations of about 5.5 % to 6.8 %, they were greatly improved to about 1.5 % to 2.2 % by excluding 5 strongly deviating data sets from the average atomic fractions. In this pilot study, the average expanded uncertainties of SIMS, XPS, AES, XRF and EPMA were 3.84%, 3.68%, 3.81%, 2.88% and 2.90%, respectively. These values are much better than those in the key comparison K-67 for composition of a Fe-Ni alloy film. As a result, the quantification of CIGS films using the TNC method was found to be a good candidate as a subject for a CCQM key comparison.
The stabilization of crystal phases and nanostructured morphologies is an essential topic in application-driven design of mesoporous materials. Many applications, e.g. catalysis, require high temperature and humidity. Typical metal oxides transform under such conditions from a metastable, low crystal-line material into a thermodynamically more favorable form, i.e. from ferrihy-drite into hematite in the case of iron oxide. The harsh conditions induce also
a growth of the crystallites constituting pore walls, which results in sintering and finally collapse of the porous network. Herein, a new method to stabi-lize mesoporous templated metal oxides against sintering and pore collapse is reported. The method employs atomic layer deposition (ALD) to coat the internal mesopore surface with thin layers of either alumina or silica. The authors demonstrate that silica exerts a very strong influence: It shifts hematite formation from 400 to 600 °C and sintering of hematite from 600 to 900 °C.
Differences between the stabilization via alumina and silica are rationalized by a different interaction strength between the ALD material and the ferrihydrite film.
The presented approach allows to stabilize mesoporous thin films that require a high crystallization temperature, with submonolayer quantity of an ALD material, and to apply mesoporous materials for high temperature applications.
A silicon MIS-structure prepared with thin layers of the super-ionic conductor LaF3 and Pd is used to detect hydrogen. The sensor is able to detect hydrogen in a concentration range from below one ppm to the lower flammable limit in air which is 4 vol.-%. The chip operates at room temperature which results in an extremely low energy consumption compared to other hydrogen sensors. Only once per day a short heating pulse is necessary to reactivate the sensor chip. In cooperation with the BAM, a long-term experiment was carried out. The duration of the measurement was about three months, with a hydrogen exposure every two weeks. The sensor signal remained stable over the measured period.
A hydrogen sensor based on a silicon Metal/Solid Electrolyte/Insulator/Semiconductor (MEIS) structure with thin layers of the super-ionic conductor LaF3 and Pd gate metal was investigated in a hybrid structure on a resistance heater mounted on a ceramic substrate. The sensor was operated at room temperature, however, a short heating impulse once a day ensures a fast and reproducible dynamic behavior. The sensor was characterized in the concentration range typical for alarm levels up to 40% of the lower flammability limit and shows a logarithmic dependency of the sensor signal from the hydrogen concentration and a mean sensitivity of about 140 mV/decade. The response time (t90) is about 8 s. In a long term test for a period of three month, the sensor was exposed to hydrogen every two weeks. The sensor signal was shown to be stable in dynamic behavior, sensitivity and signal difference.
Crack detection in metallic samples at high surface temperature, hostile and hazardous environments, etc. is challenging situation in any manufacturing industries. Most of the present NDE methods are suitable only for lower surface temperatures, especially room temperature. In this situation, we need a fast and non-contact NDT method which can be applied even in high sample surface temperature. Laser thermography is one of the techniques having a high potential in non-contact inspection. As a preliminary investigation, in this article, we have studied the potentiality of laser line thermography in crack detection at room temperature. In laser line thermography, a continuous wave (CW) laser is used to generate a laser line, which in turn is used to scan the metal surface. The heat distribution over the sample surface is recorded by an infrared thermal (IR) camera. Two different approaches are reported in this work. Firstly, a stationary laser line source and its interaction with cracks; secondly, moving laser line source scanning over a surface with crack. When the distance between crack centre to laser line centre increases, crack detectability will decrease; and when laser power increases, crack detectability will increase. A dedicated image processing algorithm was developed to improve the detectability of the cracks. To understand the heat transfer phenomenon, a simplified 3D model for laser thermography was developed for the heat distribution during laser heating and was validated with experimental results. Defects were incorporated as a thermally thin resistive layer (TTRL) in numerical modeling, and the effect of TTRL in heat conduction is compared with experimental results.
Alloy 36 (1.3912), also known as “Invar,” is an alloy with 36% nickel. The alloy has a remarkably low thermal expansion coefficient in certain temperature ranges. This peculiarity is called the invar effect, which was discovered in 1896 by the Swiss physicist Charles Édouard Guillaume. Therefore, it is used in applications in which dimensional stability is critical, such as molding tools for composite materials in aerospace, automotive applications, or liquified natural gas (LNG) cargo tanks. Moreover, increasingly complex structures and the optimization of resource efficiency also require additive manufacturing steps for the production or repair of components. Additively manufactured components have a heterogeneous microstructure and anisotropic mechanical properties. In addition, the manufactured components require subsequent machining surface finishing, like finish milling, to achieve their final contour. Nickel iron alloys are difficult to machine. Additionally, inhomogeneous microstructure may lead to unstable cutting forces and conditions. In part I of this investigation, the initial alloy 36 is modified with the elements Ti, Zr, and Hf up to a maximum of 0.33 wt.-%. The influence of the modification elements on the microstructure as well as on the hardness of the AM components is examined. Furthermore, one modification is applied to metal arc welding process and investigated. Part II focuses on the effect of the alloy modifications on machinability as well as on the surface integrity of plasma-transferred-arc-welded (PTA) and finish milled invar components.
A heptazine-based polymer network (HMP-3) with a donor–acceptor (D–A) structure was prepared and tested as catalyst for photocatalytic hydrogen evolution from water. Compared to other heptazine-based materials, which are typically prepared at high temperatures and have recently received much interest as metal-free photocatalysts, the low-temperature protocol applied here allows the defined introduction of organic functional groups within the polymer backbone. The structure of HMP-3 contains alternating heptazine and benzothiadiazole moieties as electron acceptors connected by aminobenzene bridges as electron donors. The resulting material leads to enhanced hydrogen evolution compared to graphitic carbon nitride materials prepared at high temperatures (>500 8C) most probably because of the stabilization of photogenerated charge carriers in the D–A structure.
The photoinduced pseudorotaxane formation between a photoresponsive axle and a tetralactam macrocycle was investigated in solution and on glass surfaces with immobilized multilayers of macrocycles. In the course of this reaction, a novel photoswitchable binding station with azobenzene as the photoswitchable unit and diketopiperazine as the binding station was synthesized and studied by NMR and UV/Vis spectroscopy. Glass surfaces have been functionalized with pyridine-terminated SAMs and subsequently withmultilayers of macrocycles through layer-by-layer self assembly.
A preferred orientation of the macrocycles could be confirmed by NEXAFS spectroscopy. The photocontrolled Deposition of the axle into the surface-bound macrocycle-multilayers was monitored by UV/Vis spectroscopy and led to an increase of the molecular order, as indicated by more substantial linear dichroism effects in angle-resolved NEXAFS spectra.
The supply and processing of materials for highly stressed components are usually cost-intensive. Efforts to achieve cost and resource efficiency lead to more complex structures and contours. Additive manufacturing steps for component repair and production offer significant economic advantages. Machining needs to be coordinated with additive manufacturing steps in a complementary way to produce functional surfaces suitable for the demands. Regarding inhomogeneity and anisotropy of the microstructure and properties as well as production-related stresses, a great deal of knowledge is still required for efficient use by small- and medium-size enterprises, especially for the interactions of subsequent machining of these difficult-to-machine materials. Therefore, investigations on these influences and interactions were carried out using a highly innovative cost-intensive NiCrMo alloy (IN725). These alloys are applied for claddings as well as for additive component manufacturing and repair welding using gas metal arc welding processes. For the welded specimens, the adequate solidification morphology, microstructure and property profile were investigated. The machinability in terms of finishing milling of the welded surfaces and comparative analyses for ultrasonic-assisted milling processes was examined focussing on surface integrity. It was shown that appropriate cutting parameters and superimposed oscillating of the milling tool in the direction of the tool rotation significantly reduce the mechanical loads for tool and workpiece surface. This contributes to ensure a high surface integrity, especially when cutting has to be carried out without cooling lubricants.
A pilot study (PS) has been performed under the Consultative Committee for Amount of Substance (CCQM) / Surface Analysis Working Group (SAWG) with the objective to compare the atomic fractions of Cu, In, Ga and Se in CIGS alloy films. Four polycrystalline CIGS films with different atomic fractions were fabricated by variation of the relative atomic fraction of Ga on 100 mm x 100 mm soda-lime glass (SLG) substrates. Similar to real solar cells the atomic fractions of the four elements (Cu, In, Ga, Se) are not homogeneous with depth. For the analysis of the CIGS layers of about 2 μm thickness depth profiling with surface analysis techniques such as XPS, AES and SIMS was recommended. A CIGS alloy reference sample with atomic fractions certified by isotope dilution ICP-MS at KRISS has been also put at disposal by the coordinator of the comparison. The certified values were close to the atomic fractions of the samples to be analyzed. Hence, the atomic fractions of Cu, In, Ga and Se in the CIGS films could be determined by the relative sensitivity factors (RSF) derived from the reference CIGS film. The total ion intensities of the constituent elements were obtained by the total number counting (TNC) method.