Ingenieurwissenschaften und zugeordnete Tätigkeiten
Filtern
Erscheinungsjahr
- 2022 (367) (entfernen)
Dokumenttyp
- Vortrag (367) (entfernen)
Sprache
- Englisch (254)
- Deutsch (110)
- Mehrsprachig (2)
- Spanisch (1)
Referierte Publikation
- nein (367)
Schlagworte
- Additive Fertigung (29)
- Additive manufacturing (24)
- Additive Manufacturing (17)
- Korrosion (17)
- Ultraschallunterstütztes Fräsen (12)
- Laser beam welding (11)
- Alloy 36 (9)
- Laser-induced periodic surface structures (LIPSS) (9)
- Mechanochemistry (9)
- Nanoparticles (9)
Organisationseinheit der BAM
- 9 Komponentensicherheit (132)
- 6 Materialchemie (91)
- 5 Werkstofftechnik (66)
- 9.4 Integrität von Schweißverbindungen (64)
- 7 Bauwerkssicherheit (50)
- 9.2 Versuchsanlagen und Prüftechnik (40)
- 8 Zerstörungsfreie Prüfung (38)
- 6.1 Oberflächen- und Dünnschichtanalyse (31)
- 9.3 Schweißtechnische Fertigungsverfahren (27)
- 7.6 Korrosion und Korrosionsschutz (26)
Eingeladener Vortrag
- nein (367) (entfernen)
Thermal spraying provides a rapid method for additive deposition of various ceramics as electrical insulation in applications where polymers are not suitable. New applications in complex shaped additive manufactured metal parts are emerging for example in large scale electrical devices. Microstructural and dielectric evaluation of coatings is crucial to the employment of such free-form processes. The properties and microstructure of the plasma sprayed alumina coatings are compared with dense reference samples of the same powder produced by spark plasma sintering (SPS). To obtain dense bulk samples from the coarse alumina powder for spray coating, SPS is used.
Samples are fabricated by atmospheric plasma spraying (APS) of commercially available alumina powder (d50 = 33 µm) on copper substrates and by SPS of the same powder. Microstructure and porosity were analyzed by optical microscopy and scanning electron microscopy (SEM). Phase compositions were determined by X-ray diffraction (XRD). Dielectric properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructure and dielectric properties of the coating and bulk material are compared to assess whether the coating is suitable for use in electrical insulation application.
Nanoforms with at least one dimension below 100 nm have an important part to play in more and more areas of our daily life. Therefore, risk assessment of these materials is becoming increasingly important. In this context, the European Chemical Agency (ECHA) considered eleven physico-chemical properties as relevant, of which the following six are essential for the registration: chemical composition, crystallinity, particle size, particle shape, surface chemistry and specific surface area. Four of these priority properties can be obtained with electron microscopy and surface analytics like XPS and ToF-SIMS. The reliability of this data must be ensured, especially for their use for grouping and read across approaches. On the other hand, the “reproducibility” crisis has revealed major shortcomings in the reliability of published data.
In a case study, we show how the quality of the data can be ensured by using existing standards and protocols of each step in the workflow of sample characterization. As exemplary samples, two Al-coated TiO2 samples as nanopowders were selected from the JRC repository, capped either with a hydrophilic or a hydrophobic organic ultrathin shell. SEM results provided the size and shape of the nanoparticles, a first overview about the composition was obtained with EDS. XPS and ToF-SIMS supplied the surface chemistry, especially information about the shell and the coating of the particles. Standards and protocols of all steps of the analytical workflow including preparation and data reduction are discussed regarding reliable and reproducible data. Additionally, uncertainties for the different steps are specified.
Only such a detailed description of all these factors allows a comprehensive physico-chemical characterization of the nanoparticles with understanding of their potential risk assessment.
The novel lab-based HAXPES spectrometer (ULVAC-PHI Quantes) gives us the possibility to measure XPS at 1486.6 eV (monochromatic Al Kα source) and HAXPES at 5414.9 eV (monochromatic Cr Kα source) on a sample at the same position. The surface analysis with this spectrometer leads to an information depth of about 10 nm for XPS and in comparison, to an analysis of deeper regions of about 30 nm for HAXPES measurements. This method provides a nondestructive way to distinguish between the near-surface region of the nanoparticles and the whole nanoparticle. Additionally, HAXPES gives access to deeper core levels at higher energy.
An application of this technique is presented using nanoparticles. The results shown were obtained with nanoparticles, that were treated differently by means of sterilization for nanosafety (i.e., before studying their toxicity it is important to establish whether nanomaterials are sterile and, if not, to be treated either via microwave or autoclave sterilisation). As a complementary method, the data is compared with SEM and EDX measurements. All methods demonstrate the influence of sterilization. More specifically, these results show that the sterilization step must be considered in the physical-chemical description of the particles for establishing reliable (quantitative structure-activity) relationships.
Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Additiv gefertigte (AM) dreifach periodische metallische minimale Oberflächenstrukturen (TPMSS, aus dem Englischen Triply Periodic Minimum Surface Structures) erfüllen mehrere Anforderungen sowohl im biomedizinischen als auch im technischen Bereich: Abstimmbare mechanische Eigenschaften, geringe Empfindlichkeit gegenüber Herstellungsfehlern, mechanische Stabilität und hohe Energieabsorption. Allerdings stellen sie auch einige Herausforderungen in Bezug auf die Qualitätskontrolle dar, die ihre erfolgreiche Anwendung verhindern können. Tatsächlich ist die Optimierung des AM-Prozesses ohne die Berücksichtigung struktureller Merkmale wie Fertigungsgenauigkeit, interne Defekte sowie Oberflächentopographie und -rauheit unmöglich. In dieser Studie wurde die quantitative zerstörungsfreie Analyse von Ti-6Al-4V-Legierung TPMSS mit Hilfe der Röntgen-Computertomographie (XCT) durchgeführt. Es werden mehrere neue Bildanalyse-Workflows vorgestellt, um die Auswirkungen der Aufbaurichtung auf die Wanddickenverteilung, die Wanddegradation und die Verringerung der Oberflächenrauheit aufgrund des chemischen Ätzens von TPMSS zu bewerten. Es wird gezeigt, dass die Herstellungsgenauigkeit für die Strukturelemente, die parallel und orthogonal zu den hergestellten Schichten gedruckt werden, unterschiedlich ist. Verschiedene Strategien für das chemische Ätzen zeigten unterschiedliche Pulverabtragsfähigkeiten und damit ein Gradient der Wanddicke. Dies wirkte sich auf die mechanische Leistung unter Druck durch die Verringerung der Streckspannung aus. Eine positive Auswirkung des chemischen Ätzens ist die Verringerung der Oberflächenrauhigkeit, die möglicherweise die Ermüdungseigenschaften der Bauteile verbessern kann. Schließlich wurde XCT eingesetzt, um die Menge des zurückgehaltenen Pulvers mit der Porengröße des TPMSS zu korrelieren, wodurch der Herstellungsprozess weiter verbessert werden kann.
Unter Passivität versteht man den Korrosionsschutz durch dünne, festhaftende Schichten aus Korrosionsprodukten. Für den schadensfreien Einsatz nichtrostender Stähle ergeben sich daraus zwei grundsätzliche Anforderungen.
Erstens muss sich die Passivschicht vollständig ausbilden können. Dabei sind die Oberflächenausführung, die mechanische Bearbeitung, die Elementverteilung, Ausscheidungen, die Wärmeeinbringung z.B. bei der schweißtechnischen Verarbeitung, Anlauffarben, sowie die chemische Nachbehandlung bzw. Konditionierung der Oberflächen von großer Bedeutung. Zweitens muss die Repassivierung von Defektstellen unter den Einsatzbedingungen möglich sein. Für das Repassivierungsvermögen sind die Legierungszusammensetzung, mögliche kritische Betriebszustände, prozessbedingte Besonderheiten, wie etwa Stagnationsbedingungen und Reinigungsprozesse von Bedeutung.
The fabrication of laser-generated surface structures on titanium and titanium alloys has recently gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, the effective number of laser pulses per beam spot area, etc. A simple way to characterize laser-generated surface structures is by means of optical microscopy (OM) or white light interference microscopy (WLIM). The latter can address the surface topography, while having a lateral resolution limit of ~(lambda)/2 (lambda = illumination wavelength). To resolve morphologies with spatial periods significantly smaller than (lambda)/2, scanning electron microscopy (SEM) is often used, taking benefit of the reduced de Broglie wavelength associated to the electrons of several keV energy. However, all the above-mentioned techniques lack the necessary depth-resolution to reveal and quantify sub-surface material modifications of these laser-generated structures. Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) represents a promising surface analytical technique for studying laser-induced chemical surface alterations since the method combines a high surface sensitivity with the capability to perform a depth-profiling of the laser-affected surface zone. In this study we combine WLIM and high-resolution SEM with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti-6Al-4V alloys upon irradiation by near infrared ultrashort laser pulses (1030 nm, 925 fs) at different laser fluence levels, effective number of pulses, and at different pulse repetition rates (1 – 400 kHz). We show how this combined surface analytical approach allows to evaluate alterations in the surface chemistry and topography of the laser-generated surface structures depending on the laser processing parameters
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The challenges in the residual stress analysis of AM components are discussed on the basis on the show studies performed in BAM. Also, the synchrotron X-ray refraction technique, available in BAM, is presented, showing example of in-situ heating test of Al10SiMg AM material.
Design methodology of vessel produced by L PBF stainless steel using representative specimens
(2022)
This work presents the preliminary results of an ongoing project with a double objective: on the one hand, the characterisation of the mechanical properties against fatigue damage of an additively manufactured 316 stainless steel produced by laser powder bed-based (L-PBF) technology; on the other hand, the implementation of numerical simulation techniques able to predict the mechanical behaviour of the material in order to optimise and reduce the design costs of vessels used in the chemical sector. The current state of the work developed in this research framework allows showing the first batch of experimental results of crack propagation rate (FCGR) and high cycle fatigue (HCF) tests. The geometry of the vessels studied presents three clearly differentiated regions, either in terms of thickness (11-15 mm) or concerning the inclination of the walls to the direction of manufacturing (0º - 45º). The experimental campaign carried out so far allows identifying the differences in behaviour when comparing different extraction locations around the vessel. This is due to the variations in thermal cycles that the deposited material undergoes during the manufacturing process. Therefore, this causes variations in the microstructure which lead to changes in the response of the material. In this work, these differences are analysed qualitatively and quantitatively from the results of FCGR and HCF, thus allowing to locate the regions with the highest risk in terms of structural integrity against fatigue. This preliminary phase together with the numerical simulation of the additive manufacturing process are key to achieving a reliable description and modelling of the material. The latter will make it possible to address the priority aim of this project, involving the manufacture of independent samples whose properties are representative of the original material extracted from the reference vessels. It is, therefore, a comprehensive methodology for the design of additively manufactured components based on the localised fatigue mechanical properties of representative specimens.
La tecnología de fabricación aditiva (AM) continúan progresando y permitiendo alcanzar diseños cada vez más complejos y optimizados. La industria química es uno de los sectores donde componentes AM han adquirido un gran interés. La falta hasta la fecha de una directiva europea que regule la inspección, certificación y aceptación de equipos sometidos a presión hace necesario progresar en esta línea. El objetivo que se persigue en este trabajo es el de desarrollar una metodología de diseño sobre componentes fabricados aditivamente basada en la estimación de vida a fatiga de las zonas más susceptibles de sufrir dicho tipo de fallo. El estudio comprende diversas facetas de análisis, simulaciones numéricas, análisis de la microestructura del material y una extensa campaña experimental. La evaluación de la integridad estructural se realiza aplicando mecánica de fractura. La historia térmica a lo largo del proceso de fabricación determina la microestructura del componente en cada región y, por ende, influye en las propiedades mecánicas en cada una. Se presentan los resultados preliminares de un proyecto de investigación en curso dirigido a la caracterización de propiedades mecánicas en recipientes de presión producidos por fusión láser en lecho de polvo (L-PBF, por sus siglas en inglés) de acero inoxidable 316L. Se detallan los resultados preliminares en términos de velocidad de crecimiento de grietas por fatiga (FCGR), y se comparan los resultados de probetas extraídas de diferentes regiones de los depósitos.
Quantification of the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials
(2022)
Surface-functionalized organic and inorganic nanoparticles (NP) are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. NP performance in such applications depends not only on particle size, size distribution, and morphology, but also on surface chemistry, i.e. the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. Methods for FG quantification should be simple, robust, reliable, fast, and inexpensive, and allow for the characteriza-tion of a broad variety of nanomaterials differing in size, chemical composition, and optical properties.
Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG such as amine, carboxy, thiol and aldehyde functionalities, we investigated and compared various analytical methods commonly used for functional group quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance, mass spectrometry, and thermal analysis methods.
Genormte künstliche Bewitterungstests sind häufig nicht spezifisch für die Anwendungssituation oder das Material. Das macht die Entwicklung spezifischer Tests erforderlich. Für deren Entwicklung müssen Maximalparameter der Anwendungssituation bekannt sein, womit dann der künstliche Test formuliert wird und dessen Bedingungen werden dann solange optimiert, bis die Korrelation der Effekte von natürlichem und künstlichem Test ausreichend ist.
Für Untersuchungen der Freisetzung kann der verbleibende Rest in der Probe und/oder die freigesetzte Menge in Luft, Boden, Wasser bestimmt werden.
Im ersten Beispiel der Witterungswirkung wurde die Freisetzung von Kohlenstoff-Nanoröhrchen (CNT) aus Polymer-Kompositen untersucht (unter Verwendung von empfindlich-nachweisbarer radioaktiver 14C-Markierung für einzelne CNT-Partikel), in einem zweiten die Freisetzung von anorganischen und organischen Bestandteilen aus elastomeren Bestandteilen von Sportböden (Bahnen und Kunstrasen) in Wasser.
To assess the ability of cracks to grow, a robust determination of the threshold against fatigue crack propagation ∆Kth is of paramount importance. The standards ASTM E647 and ISO 12108 introduce operational definitions of ∆Kth based on the crack propagation rate da/dN. For evaluating ∆Kth, both suggest fitting a linear function to a defined subset of the logarithmic ∆K – da/dN test data, where ∆Kth follows by evaluating the linear function at da/dN = 10-7 mm/cycle and da/dN = 10-8 mm/cycle, respectively.
In general, this kind of fit suffers from a bad representation of the actual curvature of the crack propagation curve. Therefore, we propose a robust method for evaluating ∆Kth using a non-linear function that reduces the artificial conservativeness induced by the evaluation method as well as the susceptibility to scatter in test data and the influence of test data density. The method is calibrated against a large set of S690QL crack growth data obtained from a total of 48 specimens, and validated against a set of S355NL and S960QL data (3 specimens each), obtained as a part the IBESS (integral fracture mechanics determination of the fatigue strength of welds) project.
Nach einer kurzen Einführung in die Schallemissionsprüfung und -Analyse wird ein Versuchsstand vorgestellt, der im Rahmen des Themenfeldprojektes Seal Waste Safe installiert wurde. Schwerpunkt des Vortrages sind die Schallemissionsmessungen an einem 150 l Demonstrator aus Salzbeton und einem weiteren aus alkali-aktiviertem Material. Neben der konventionellen Schallemissionsanaylse mit Aktivitäts- und Intensitätsparametern der Zeitsignale, werden auch frequenzbasierte Parameter zur Analyse andiskutiert.
In pursuing the automated synthesis of metal nanoparticles (NPs), the capabilities of the “Chemputer” are deployed, for the first time, into the field of inorganic chemistry. Metal NPs have a substantial impact across different fields of science, such as photochemistry, energy conversion, and medicine. Among the commonly used nanoparticles, silver NPs are of special interest due to their antibacterial properties and applications in sensing and catalysis. However, many of the methods used to synthesize Ag NPs often do not result in well-defined products, the main obstacles being high polydispersity or a lack of particle size tunability.
The Chemputer is a modular, automated platform developed by the Cronin group for execution of multi-step, solution based organic synthesis. The machine has been further implemented at BAM, where we used this setup to perform automated organic syntheses, autonomously controlled by feedback derived from online NMR. In the Chemputer liquids can be transferred across a backbone, constructed from HPLC selection valves and syringe pumps. The Chemputer operates in a batch mode, common laboratory devices, such as heaters and glassware like round bottom flasks, are connected to the backbone, forming reaction modules. Solutions can be manipulated in these modules, and as all operations are controlled through a software script, reproducibility among individual syntheses is high. Likewise, any adjustments of the synthesis conditions, if required, are straightforward to implement and are documented in the reaction log file and a code versioning system.
We characterised Chemputer-synthesized nanoparticles using small-angle X-ray scattering, dynamic light scattering and further methods, showing that automated synthesis can yield colloids with reproducible and tuneable properties. The approach is an important first step towards the automation of nanoparticle syntheses in a modular, multipurpose platform. The modularity of the Chemputer opens many possibilities for the synthesis of a variety of different NP morphologies and sizes and potentially more complex structures. These advances and further work can help in the general investigations of silver nanoparticles by supplying a reliable and reproducible method of their synthesis and removing tacit knowledge by significantly reducing the experimental bias.
The complexity of any microstructural characterization significantly increases when there is a need to evaluate the icrostructural evolution as a function of temperature. To date, this characterization is primarily performed by undertaking elaborative ex-situ experiments where the material’s heating procedure is interrupted at different temperatures or times. Moreover, these studies are often limited to a region smaller than the representative elementary volume, which can lead to partial or even biased interpretations of the collected data. This limitation can be greatly overcome by using in-situ synchrotron X-ray refraction (SXRR).
Die additive Fertigung (ugs. „3D-Druck“) ist bei der Herstellung von hochkomplexen metallischen Bauteilen, bionisch inspiriertem Leichtbau oder Prototypen nicht mehr wegzudenken.
Für die konventionelle Fertigung hat sich das bestehende System der Qualitätsinfrastruktur (QI) bewährt. Die additive Fertigung vergrößert den gestalterischen Spielraum von möglichen Bauteilgeometrien und Prozessfehlern jedoch erheblich. Hier gerät die QI an ihre Grenzen, sodass die Fertigung und Zulassung sicherheitsrelevanter Bauteile sehr zeit- und kostenintensive Versuche erfordern. Eine moderne digitale QI erlaubt eine effizientere Qualitätssicherung für additiv gefertigte Bauteile. Dies erfordert eine durchgängig digitale Abbildung des physischen Materialflusses.
The talk gives an introduction into gas metal arc welding and its relation to plasma science as well as current challenges in welding research concerning research data management and the application of the FAIR principles.
The WelDX project is introduced and the main goals are discussed and contrasted with the current features of the weldx API.
Different internal and public facing use cases focusing on research data management and their implementation using weldx are presented.
The interactive part of the presentation displays some advanced multi layer use cases and data analysis using the weldx API as well as the integration of materials properties into weldx.
In typical material oriented research projects numerous types and sources of data need to get connected to form the final outcome. The data-structures have to be described in a manner semantically concise enough so that all participants share the meaning and at the same time flexible enough to allow connecting findings and facts that have not been connected before.
The present contribution describes the approach that is being taken in a public funded research project with two cooperating research institutes. The aim of the data-management solution is to describe and interlink three main entity types: material entities like a test specimen that is under observation, immaterial entities like a fatigue life model and processes that generate and transform the immaterial and material entities.
The shared understanding of what is described by the data is achieved by referring to existing linked data resources. In addition a common thesaurus that is subject to ongoing discussion is used for concepts and terms that need precision beyond publicly available concept descriptions. The data associated with the entities and processes and entities is rather small and well structured. The entities and processes covered by the vocabularies are typical to laboratories performing fatigue testing and microstructure analysis. Through the interlinking of the entities and processes it becomes possible to intuitively understand the knowledge that is accumulating in the database. For example it is easy to trace the history of a creep test specimen starting from the chemical composition that has been analyzed for the heat, continuing with the heat treatment of the material, going into the creep test itself with the associated creep data and finally finding the transmission electron microscopy images that have been taken from the crept sample.
The presented approach is prototypical way to tackle the sustainable management of structured open research data. Open questions remain for example with the management of attributions, the acceptance of an increased effort in data creation and the access control to specific regions of the data. On the other hand the approach sketches what added value can be created, if the community adopts and contributes to the linked data principles.
The presentation shows systematic investigations to describe the corrosion and corrosion product formation processes of pure zinc under the climatic conditions currently prevailing in the Federal Republic of Germany. The investigations in their entirety aim at questioning current and establishing new ways of looking at the formation of corrosion products of pure zinc under atmospheric corrosion conditions. Thus, they make a significant contribution in understanding corrosion protection by zinc and zinc coatings. In particular, the focus is placed on the initial stage of the corrosion product formation. A systematic investigation of this time range, which is characterized by very reactive corrosion products, is only made possible by using gel-type electrolytes. The short periods of time at the beginning of weathering is now measurable and their influence on the formation of corrosion products and the kinetics of layer formation describable. By combining the new electrochemical approach with gravimetric, microscopic and analytical methods, new insights could be gained both on a methodic and scientific level.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process.
Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites.
In this study, the influence of aging and mean stress on fatigue of the aluminium-alloy EN AW-2618A is investigated. Therefore axial fatigue tests are carried out on smooth specimens. The experiments show that the fatigue life decreases with increasing mean stress. Furthermore, the tests with the overaged specimens demonstrate that the number of cycles to failure is decreasing with increasing aging time.
Chemical heuristics are essential to understanding molecules and materials in chemistry. The periodic table, atomic radii, and electronegativities are only a few examples. Initially, they have been developed by a combination of physical insight and a limited amount of data. It is now possible to test these heuristics and generate new ones using automation based on Materials Informatic tools like pymatgen and greater amounts of data from databases such as a Materials Project. In this session, I'll speak about heuristics and design rules based on coordination environments and the concept of chemical bonding. For example, we have tested the Pauling rules which describe the stability of materials based on coordination environments and their connections on 5000 oxides from the Materials Project. In addition, we have created automated processes for analyzing the chemical bonding situation in crystalline materials with Lobster (www.cohp.de) in order to discover new heuristics and design rules.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Gezeigt werden die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Beispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
Nichtrostende Duplexstähle (DSS) werden häufig verwendet, insbesondere bei Anwendungen, die eine hohe Festigkeit in Verbindung mit einer hohen Korrosionsbeständigkeit in aggressiven Medien erfordern. Beispiele hierfür sind Kraftwerkskomponenten und maritime Anwendungen. Beim Schweißen dieser Stähle kann es zu lokalen Schwankungen in der chemischen Zusammensetzung kommen. Dies führt zu einer Ferritisierung des Werkstoffs und beeinträchtigt die mechanischen Eigenschaften der Bauteile. In dieser Arbeit wurden Versuche zum Wolfram-Inertgas-Schweißen (WIG) mit DSS durchgeführt. Die Analyse der chemischen Zusammensetzung wurde in situ mit Hilfe der laserinduzierten Plasmaspektroskopie (LIBS) durchgeführt. Ziel der Arbeit ist es, die chemische Zusammensetzung in der Schweißnaht verschiedener DSS quantitativ zu messen und mögliche Einflüsse der Schweißparameter auf die Mikrostruktur des Werkstoffs zu ermitteln. Gemessen wurden die chemischen Konzentrationen der Hauptlegierungselemente Cr, Ni, Mn auf der Oberfläche der Probe während des Schweißprozesses und des Abkühlungsprozesses. Mn und Ni sind Austenitstabilisatoren, deren Gehalt beim Schweißen durch die Verwendung bestimmter hochlegierter Schweißzusatzwerkstoffe zunimmt. Die Spektren wurden alle 1,3 s in einem Abstand von etwa 2 mm aufgezeichnet. Während des Abkühlungsprozesses wurde der Ort der Messung nicht verändert. Die LIBS-Methode eignet sich nachweislich zur quantitativen Darstellung der chemischen Zusammensetzungen während des Schweißvorgangs.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced.
Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden.
Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden.
The processing of laser-induced periodic surface structures (LIPSS) represents a simple and robust way for the nanostructuring of solids that allows creating a wide range of surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. While the currently available laser and scanner technology already allows surface processing rates at the m2/min level, industrial applications of LIPSS are sometimes hampered by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. This presentation aims to identify some unsolved scientific problems related to LIPSS, discusses the pending technological limitations, and sketches the current state of theoretical modelling. Hereby, it is intended to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry.
Using nanofiber-like cell appendages, secreted proteins and sugars, bacteria can establish initial surface contact followed by irreversible adhesion and the formation of multicellular biofilms. Here, the stabilizing extracellular biofilm matrix together with physiological changes on the single cell level leads to an increased resilience towards harsh environmental conditions, antimicrobials, the host immune response and established cleaning procedures. Persistent microbial adhesion on e.g., medical implants, in water supply networks or food-processing industry is often associated with chronic inflammation, nosocomial and foodborne infections, enhanced biofouling and product contamination. To prevent persistent microbial colonization, antibacterial surface strategies often target the initial steps of biofilm formation and impede adhesion of single cells before a mature biofilm is being formed. While chemical coatings have been widely used, their restricted biocompatibility for eukaryotic cells and attenuated antibacterial-effects due to compound release limit their areas of application and alternative strategies focus on modified surfaces topographies to impede bacterial adhesion. In this work, we used ns-UV laser treatment (wavelength 248 nm and a pulse duration of 20 ns) to generate laser-induced periodic surface structures (LIPSS) with different submicrometric periods ranging from ~210 to ~610 nm on commercial poly(ethylene terephthalate) (PET) foils. Following structurally and chemically analyses, PET samples were subjected to bacterial colonization studies with Escherichia coli TG1, a bacterial test strain with a strong biofilm formation capacity due to the formation of nanofiber-like cell-appendages (pili). Bacterial adhesion tests revealed that E. coli repellence decisively depends on the spatial periods of the LIPSS with the strongest reduction (~91%) in cell adhesion observed for LIPSS periods of 214 nm. Scanning electron microscopy and additional biofilm studies using a pili-deficient E. coli TG1 strain revealed the importance of extracellular appendages in the bacterial repellence observed here, thus, pointing out new antibiotics-free strategies for antibacterial surfaces by impeding nanofiber-mediated bacterial adhesion.
Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined.
This presentation focuses on the basic ideas and current status of the development of an arithmetical method to predict the failure rotational speed of turbine disks. The certification specification requires that a gas turbine aero-engine must hold 5 minutes at overspeed conditions without critical failure. Therefore, instead of experimental proof from spin-tests using test-disks similar to engine components, it is considered to use simple specimen with similar test conditions compared to real overspeed scenarios. These test conditions, or stress fields are determined using arithmetical method, e.g. finite element method, with consideration of fracture mechanics under quasi-static conditions with a given rotational speed.
Failure modes like hoop burst and rim peeling are considered during determination of stress fields. Various crack-tip parameters are used to explore the similarity of stress field between simple specimen and real overspeed scenarios. Additionally, probabilistic aspects and the implementation of a global stability criterion for overspeed analysis are also considered.
Aero-engine turbine disks are safety-relevant components which are operated under high thermal and mechanical stress conditions. The actual part qualification and certification procedures make use of spin-tests conducted on production-similar disks. While these tests provide, on the one hand, a reliable definition of the critical conditions for real components, on the other hand they represent a relevant cost item for engine manufacturers. The aim of this work is to present part of a fracture mechanics-based procedure under development which aims at replacing the tests on production-similar disks with lab tests on fracture mechanics specimens. In particular, the rim-peeling failure mode is considered as case study. A semi-circular surface crack is modelled at the most stressed region at the diaphragm of a turbine disk, with the crack plane perpendicular to the radial direction. The crack is therefore subjected to a biaxial stress state and grows under increasing rotational speed until it triggers the rim-peeling failure. The finite element simulation of the cracked disk considers the real thermal and mechanical loading conditions. In order to design a lab representative specimen, beside the crack driving force, expressed in terms of J-integral, also the constraint to plastic deformation e.g., stress triaxiality, at the crack-tip must be similar for the same crack in the specimen and in the disk. This has been achieved and as expected, both the highest J-integral and constraint factor are calculated at the same location along the crack front for both disk and specimen. The results of the structural integrity assessment in the form of a Failure Assessment Diagram (FAD) show good agreement between designed specimen and disk both in terms of expected failure mode and value of the critical speed. Probabilistic aspects are also considered in the calculations.
In den letzten Jahren haben additive Fertigungstechnologien an Bedeutung gewonnen. Für komplexe Funktionsbauteile oder die Produktion von Werkstücken in kleinen Stückzahlen kann das Laser-Pulverbettschmelzen eingesetzt werden. Hohe Sicherheitsanforderungen, z. B. in der Luft- und Raumfahrt, erfordern eine umfassende Qualitätskontrolle. Daher werden nach der Fertigung zerstörungsfreie Offline-Prüfverfahren wie die Computertomographie eingesetzt. In jüngster Zeit wurden zur Verbesserung der Rentabilität und Praktikabilität zerstörungsfreie Online-Prüfverfahren wie die optische Tomographie entwickelt. In diesem Beitrag wird die Anwendbarkeit der Wirbelstromprüfung mit GMR Sensoren für die online Prüfung von PBF-LB/M Teilen demonstriert. Die Ergebnisse einer online Wirbelstromprüfung mit GMR Sensoren und einer Ein-Draht-Anregung werden gezeigt. Während des Produktionsprozesses wird für jede Lage eine Wirbelstromprüfung durchgeführt. Trotz hochauflösender Arrays mit 128 Elementen wird durch eine angepasste Hardware die Prüfdauer geringgehalten. So kann die Messung während des Beschichtungsvorgangs durchgeführt werden, ohne den Fertigungsprozess signifikant zu verlangsamen. Eine online Wirbelstromprüfung eines stufenförmigen Testkörpers aus Haynes282 über 184 Lagen zeigt, dass die Kanten nicht nur in der aktuellen Lage detektiert werden können, sondern auch in einer Tiefe von 400 µm, wenn eine Anregungsfrequenz von 1,2 MHz gewählt wird.
Ni alloys are cost intensive materials and generally classified as difficult-to-cut materials. However, machining of these materials is needed especially in case of alloy 36 (1.3912), which is commonly used in mould construction for the production of fibre-reinforced composites. With regard to repair, modification and manufacturing of such components, additive manufacturing offers significant economic advantages. Nevertheless, subsequent machining steps are needed to achieve the final component contour and defined surface conditions. Dependent on the material and machining process conditions, detrimental tensile residual stresses may be the result on the machined surface, having negative impact on the component performance and safety. Recent studies exhibited that hybrid machining processes, such as ultrasonic-assisted milling (USAM), are suitable for achieving favourable residual stress states at the surface of difficult-to-cut Ni-Cr alloys. In this investigation, wire arc additive manufactured (WAAM) specimens of alloy 36 were finish milled under different milling conditions. In addition to the machined surfaces condition and topology, the surface-near residual stresses were analysed using X-ray diffraction (XRD). Especially for low cutting speeds, significantly improved surface properties, roughness parameters and lower mechanical and microstructural degradations were found for the specimen machined with USAM compared to conventional milling. The improved surface integrity could furthermore be observed by a significant reduction of the tensile residual stresses in the surface boundary area.
Untersuchungsmethoden beim Fräsen additiv gefertigter schwer spanbarer Kobalt-Chrom-Legierungen
(2022)
Für den Anlagenbau werden hochbelastete Komponenten aus Co-Cr-Legierungen hergestellt. Dabei ist die Zerspanung so herausfordernd, dass additive Fertigungsschritte oft wirtschaftlicher sind. Diese bedingen aber vorwiegende heterogene, anisotrope Gefüge und Eigenschaften und bei nachfolgender Fräsbearbeitung unstetige Zerspankräfte und instabile Spanvorgänge. Hierbei können hybride Zerspanprozesse helfen, hohe Belastungen für Werkzeug und Werkstückoberfläche zu minimieren. Diesbezügliche Charakterisierungen erfordern speziell adaptierte Zerspanungsanalysen.
Anhand eines Anwendungsbeispiels, bei dem eine Modifikation der Ausgangslegierung mit 1 % Hf erfolgte, wird die Wechselwirkung zwischen Gefügemorphologie und Fräsprozess dargestellt, der konventionelle mit einem hybriden ultraschallunterstützten Fräsprozess verglichen und die Charakterisierung des Werkzeugverschleißes anhand zweier verschiedener Fräser betrachtet. Analysen auftretender Prozesskräfte mittels Piezo-Mehrkomponenten-Dynamometer, der Werkzeugoszillation mittels Laser-Vibrometer und zusätzliche In-situ-Temperaturmessungen der Werkzeugschneiden mittels Highspeed-Pyrometer bilden den Kern der neuen Zerspanungsprüftechnik.
Die vorgestellten Untersuchungsmethoden bilden die Vorgänge bei der Zerspanung additiv gefertigter Werkstoffe detailliert und reproduzierbar ab. Sowohl Legierungsmodifikation als auch hybride Prozessbedingungen lassen gezielte Einflüsse zur deutlichen Verbesserung der Zerspanungssituation zu.
Ni alloys are cost intensive materials and generally classified as difficult-to-cut materials. However, machining of these materials is needed especially in case of alloy 36 (1.3912), which is commonly used in mould construction for the production of fibre-reinforced composites. With regard to repair, modification and manufacturing of such components, additive manufacturing offers significant economic advantages. Nevertheless, subsequent machining steps are needed to achieve the final component contour and defined surface conditions. Dependent on the material and machining process conditions, detrimental tensile residual stresses may be the result on the machined surface, having negative impact on the component performance and safety. Recent studies exhibited that hybrid machining processes, such as ultrasonic-assisted milling (USAM), are suitable for achieving favourable residual stress states at the surface of difficult-to-cut Ni-Cr alloys. In this investigation, wire arc additive manufactured (WAAM) specimens of alloy 36 were finish milled under different milling conditions. In addition to the machined surfaces condition and topology, the surface-near residual stresses were analysed using X-ray diffraction (XRD). Especially for low cutting speeds, significantly improved surface properties, roughness parameters and lower mechanical and microstructural degradations were found for the specimen machined with USAM compared to conventional milling. The improved surface integrity could furthermore be observed by a significant reduction of the tensile residual stresses in the surface boundary area.
Artificial bone replacement by individual customized three-dimensional resorbable bioactive glass has not yet been widely established in the clinical use. This is mainly due to the antagonism of sintering ability and suitable bioactivity. Competitive crystallization often prevents the generation of dense sintered bodies, especially for additive manufactured 3D structures. Previous studies of the fluoride-containing glass F3 have shown its potential to combine both sintering ability and suitable bioactivity. Furthermore, the occurring sintering blockade by surface crystallization of Na2CaSi2O6 was tunable by glass particle size.
In this study the glasses F3, F3-Cu with 1 mol% CuO added at the expense of CaO and the well-known 13-93 were chosen to determine the influence of surface crystallization on 3D printed sinter bodies. For this purpose, grain size fractions in range of smaller 32 µm to 315 µm in fraction size of 6-20 µm were sieved from jaw crushed glass frit as well as glass cubes were cut from casted blocks for all glasses. Sintering behavior of both pressed and printed powder compacts was observed via heating microscopy. Crystallization was determined by DTA and crystallization progress was monitored on fractured sinter bodies and polished cubes via electron and laser scanning microscopy as well as with diffractometry.
Depending on grain size the formation of crystalline support framework along former grain boundaries shows the capability to stabilize fully densified sinter bodies before softening. Beside of this, the generation of complex hierarchic porosity was possible as well.
Most of the in-service failures of welded structures are due to fatigue damage occurring in the joints. Damage tolerant approaches based on the principles of Fracture Mechanics have been shown to play a key role in this framework, as the fatigue limit is defined by the non-propagating condition of multiple defects at the weld toe. The fatigue limit assessment can be performed using the cyclic R-curve analysis which consists in comparing the driving force of a crack propagating into a component, which depends on the geometry, material and external loads, with its resistance curve, i.e. the cyclic R-curve. The crack propagation occurs whenever the crack driving force is higher than the resistance to fatigue crack propagation, while the crack is arrested in the opposite case. Consequently, this suggests that the fatigue limit of a component is defined as that stress level at which the crack driving force curve is tangent to the crack resistance curve. In the present work, the cyclic R-curve analysis has been adopted for determining the fatigue limit of stress-relieved transverse non-load-carrying joints made of S355 structural steel and subjected to fatigue axial loadings. Experimental tests have been performed to evaluate the fatigue limit of the joints. The driving force, identified by the applied Stress Intensity Factor (SIF), has been evaluated by means of linear elastic finite element analysis taking advantage of the Peak Stress Method for its rapid estimation. Based on the experimental observations that the crack initiation and early crack growth phases in welded joints occur within the Heat Affected Zone (HAZ) the cyclic R-curve has been experimentally derived for both the base metal and HAZ material.
Präsentation zum geplanten BAM-Forschungsvorhaben ("Safe transport of stabilized polymerizing substances: Investigation on the degradation of selected stabilizers"), bezogen auf den sicheren Transport (Straße, See) von polymerisierenden Substanzen. Der Schwerpunkt liegt dabei auf den systematischen Untersuchungen - mittels Thermal Activity Monitor (TAM IV) - zum zeitlichen Abbau des Stabilisators bei der Polymerisation sowie auf der Bestimmung der entsprechenden volumenabhängigen selbstbeschleunigenden Polymerisation (SAPT).
Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1.
The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, 'textbook' image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase.
Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals (Fig. 1). Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7 (Fig 2). These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
A large amount of publicly available data is reproduced every day in the field of materials science, while these kind of material data can have different formats and types like paper-type publications, standards, datasheets or isolated datasets in repositories. However, gathering a specific library from such extensive and diverse material data is always challenging for the materials scientists and engineers, since the time-related limitations are not allowed to fully access the large publicly available databases; search across these disparate databases, manage the large volumes of heterogeneous datasets, and integrate data from multiple sources. To address these challenges and make data findable, accessible, interoperable, and reusable (FAIR), an efficient data management system is necessary to build comprehensive, documented, and connected data spaces in the future. A formal standardized knowledge representation through an ontology can address such problems and make data more available and interoperable between related domains. Ontology can also rich machine processable semantic descriptions that increases the performance of scientific searches. In this regard, the Platform MaterialDigital (PMD) is currently working on developing a high-level ontology for the materials and material related processes. For example, in one of the PMD projects of “KupferDigital”, we will try to develop a data ecosystem for digital materials research based on ontology-based digital representations of copper and copper alloys. As a case study, this paper describes the methodology for ontology development of Brinell hardness, based on PMD core ontology. The methodology we describe includes the following steps; gathering the required domain terminology from different resources like standards (DIN EN ISO 6506-1) and test reports, representing the performance of a standard-conformant hardness test and the treatment of the recorded values up to a “reportable” hardness value for a material, designing the process chain according to the semantic technologies, and developing a domain-level ontology of Brinell hardness based on PMD ontology semantic formalization. Apart the mentioned methodology, some interesting tools and methods were introduced and ontology design challenges and possible solutions for modelling materials and processes were discussed. Furthermore, a dataset from the Brinell hardness measurement of cast copper samples is prepared for testing the query process.
In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted.
NIR-excitable lanthanide nanocrystals (LnNC) show multi-color emission pattern composed of a multitude of narrow bands of varying intensity in the ultraviolet, visible, near-infrared, and short-wave infrared detectable with miniaturized optical instruments and simple color (RGB) cameras in complex environments. This makes these chemically inert luminescent materials ideal candidates for anticounterfeiting and authentication applications as well as for modules in optical sensors in which the LnNCs can be used as nanolamps in combination with analyte-sensitive fluorophores or the temperature sensitivity of defined emission bands can be utilized.
Therefore, we are building up and exploring a platform of LnNC with application-specifically tuned size, composition, and surface chemistry.
With the introduction of a hydrogen-based energy and national economy, safety-relevant components for hydrogen technologies are becoming increasingly important. Characteristic of hydrogen technologies are, for example, harsh environmental conditions such as cryogenic or high-pressure storage, corrosion issues in fuel cells and electrolyzers, turbines, and many more. Additive manufacturing of components is becoming increasingly important and irreplaceable for the production of complex technical systems. Using the case studies of burners for gas turbines and electrodes and membranes for polymer (PEMFC) and solid oxide (SOFC) fuel cells, this article shows the potential of additive manufacturing of components. At the same time, however, the challenge of considering divergent mechanical properties depending on the direction of assembly in a "hydrogen-compatible" manner is also highlighted. Finally, the challenges posed by additive manufacturing and hydrogen for materials testing are highlighted under scenarios that are as realistic as possible.
MALDI-ToF mass spectrometry for the characterization of biobased polymers suitable for depollution
(2022)
In this work, bio-based polymers were synthesized and designed as polymers phases for adsorption of a variety of pollutants from aqueous solutions. The obtained adsorption results showed that the integration of bio-sourced synthons generate attractive hydrophilicity, and wettability of the resulting adsorbent phase. Such polymers phases enable stronger interactions with the organic and inorganic pollutants in water.
A wide variety of different bio-based polymers structures (e. g. poly(ethersulfones, poly(etherphosphines or poly(etherpyridines) with different functional groups were successfully designed in order to adapt chemical structure to different pollutants type and matrice nature.
In order to characterize and to determine the correlation between polymer structures and nature of interaction with pollutants, different analytical technics (NMR, GPC, ATG, DSC, Mass spectrometry) were successfully used. Amongst them, MALDI TOF mass spectrometry plays a superior role since this technique enables the simultaneous determination of the polymer structure, polymer end groups and molecular weight.
This work focusses on the characterization of synthesized polymers. The chemical structure of the repeating unit, the nature of the end groups, as well as the molecular weight, which are all important for the specific interactions of the polymer with the pollutants were clearly determined and suggestions to improve these interactions by changing the synthetic pathway could be given.
Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1.
The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, 'textbook' image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase.
Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals. Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
Calcium sulfate minerals are abundant in natural and engineered environments in the form of three phases: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these phases from aqueous solution have been the subject of intensive research, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, The formation of the different crystalline phases involves several steps including a common amorphous precursor.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure. The actual crystallization occurs by the restructuring and coalescence of the "bricks" into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Such a process yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous single crystal structure.
These observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway might preserve in the final crystal structure an “imprint” of their growth pathways. Indeed, by considering large anhydrite crystals from the famous Naica Mine we observed a suite of correlated self-similar void defects spanning multiple length-scales. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from an original particle-mediated growth. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
Die technischen Möglichkeiten der robotischen Glasschmelzanlage der BAM werden vorgestellt.
Over the years, industrial and human activities and agricultural practices have caused a serious threat to human health and the environment. Indeed, it has been demonstrated that these activities are responsible for the presence of pollutants in the soil, air and water.
Water is one of the most strategic issues today, as it is associated with the living world. Therefore, water pollution is becoming a universal scourge that leads to environmental degradation, decrease of water quality and threatens public health.
Water pollution is mainly due to the discharge of certain harmful chemical compounds that are not very or not at all biodegradable (phenolic compounds, heavy metals, hydrocarbons, dyes, pesticides, etc.) by various industries: chemical, pharmaceutical, textile, food processing, etc. The impact of these industrial effluents on fauna and flora is very harmful. A sensitization of the socio-economic actors and the public, accompanied by a severe regulation in relation to the discharges, would contribute to fight against this drift, but also, by the development of effective methods allowing to remove these pollutants, not only in an analytical purpose but also of depollution.
Thus and within the framework of the preservation of an environment with regard to any anthropogenic activity, our research topic relates to the use of original biosourced polymeric phases for the extraction of the organic compounds and the heavy metals in aqueous mediums.
Therefore, we have proceeded to the synthesis and characterization of a large variety of monomers, polymers and cross-linked materials. These products, partially derived from biomass, contain various functional groups with the ability to interact with chemical components without discriminating effect.
The developed polymer phases have been successfully used for the adsorption of some organic pollutants and heavy metals in synthetic aqueous solutions.
Phenolic compounds constitute a widespread and important class of water pollutants that should be efficiently removed from wastewater because of their toxicity even at low concentrations. They are indeed discharged in the liquid effluents from various factories: chemical, petrochemical, paper, wood, metallurgy and cocking plants 1. Phenols are also found in the waste waters of agroindustrial processes like the olive oil mills, tomato processing and wine distilleries 2,3. These contaminants cause several health problems for humans and aquatic organisms 4. Therefore, numerous studies on the removal of polyphenols from wastewaters have been conducted and many techniques have been used. Among them, adsorption is considered to be the best effective and low cost method. In this context, we have focused our efforts on optimizing adsorption process by development of novel, low-cost adsorbents derived from biobased byproducts with high adsorptive capacity.
The main aim of this study is to synthesize triazole-based poly(ether-pyridine)s as new synthetic adsorbent phases for the extraction of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polycondensation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinic monomers as well as resulting polymers was confirmed by 1H and 19F NMR spectroscopic methods. The thermal behaviour of the obtained PEPTs was characterized using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Their uptake performance to eliminate organic compounds was determined using High Performance Liquid Chromatography (HPLC).
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Nanoparticle Populations
(2022)
Two new projects P15 Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension and P16 Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension have been started at VAMAS/TWA 34 under the lead of BAM. First results are presented and discussed.
In diesem Vortrag werden die Hintergründe, Ziele und ausgewählte Ergebnisse aus dem IGF-Vorhaben zu Korrosionsuntersuchungen an alternativen nichtrostenden Stählen vorgestellt. Weiterhin werden die Vorteile dieser Stähle hinsichtlich mechanisch -technologischer Eigenschaften sowie deren Kosten gegenüber den klassischen austenitischen nichtrostenden Stählen aufgezeigt.
Dieser Vortrag stellt die technologischen und industriellen Meilensteine bei der Etablierung von Lean Duplex Stählen im Bereich des Bauwesens vor. Ein weiterer Blick geht auf die weiteren Entwicklungen an der BAM hinsichtlich der Ausweitung der Kapazitäten und Standorte atmosphärischer Bewitterungsstände der BAM.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. For silicate glasses we found a good correlation between the calculated surface energy of crystal faces and oriented surface nucleation. Surface energies were estimated assuming that crystal surfaces resemble minimum energy crack paths along the given crystal plane. This concept was successfully applied by Rouxel in calculating fracture surface energies of glasses. Several oriented nucleation phenomena can be herby explained assuming that high energy crystal surfaces tend to be wetted by the melt. This would minimize the total interfacial energy of the nucleus. Furthermore, we will discuss the evolution of the microstructure and its effect on the preferred crystal orientation.
Additively manufactured (AM) triply periodic metallic minimum surface structures (TPMSS, from the English Triply Periodic Minimum Surface Structures) fulfill several requirements in both biomedical and engineering fields: tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some quality control challenges that may prevent their successful application. In fact, optimization of the AM process is impossible without considering structural features such as manufacturing accuracy, internal defects, and surface topography and roughness. In this study, quantitative nondestructive analysis of Ti-6Al-4V alloy TPMSS was performed using X-ray computed tomography (XCT). Several new image analysis workflows are presented to evaluate the effects of buildup direction on wall thickness distribution, wall degradation, and surface roughness reduction due to chemical etching of TPMSS. It is shown that the fabrication accuracy is different for the structural elements printed parallel and orthogonal to the fabricated layers. Different strategies for chemical etching showed different powder removal capabilities and thus a gradient in wall thickness. This affected the mechanical performance under compression by reducing the yield stress. A positive effect of chemical etching is the reduction of surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of powder retained with the pore size of the TPMSS, which can further improve the manufacturing process.
A paradigm shift in the description of creep in metals can only occur through multi-scale imaging
(2022)
The description of creep in metals has reached a high level of complexity; fine details are revealed by all sorts of characterization techniques and different theoretical models. However, to date virtually no fully microstructure-driven quantitative description of the phenomenon is available. This has brought to interesting inconsistencies; the classic description of (secondary) creep rests on the so-called power law, which however: a- has a pre-factor spanning over 10 orders of magnitude; b- has different reported exponents for the same material; c- has no explanation for the values of such exponents.
Recently, a novel description (the so-called Solid State Transformation Creep (SSTC) Model) has been proposed to tackle the problem under a different light. The model has two remarkable features: 1- it describes creep as the accumulation of elementary strains due to dislocation motion; 2- it predicates that creep is proceeding by the evolution of a fractal arrangement of dislocations. Such description, however, needs a great deal of corroborating evidence, and indeed, is still incomplete.
To date, we have been able to observe and somehow quantify the fractal arrangement of microstructures through Transmission Electron Microscopy (TEM), observe the accumulation of dislocations at grain boundaries by EBSD-KAM (Electron Back-Scattered Diffraction-Kernel Angular Misorientation) analysis, quantify the kinetic character (solid state transformation) of experimental creep curves, and estimate the sub-grain size of the fractal microstructure through X-ray refraction techniques. All pieces of the mosaic seem to yield a consistent picture: we seem being on the right path to reconstruct the whole elephant by probing single parts of it. What is still missing is the bond between the various scales of investigation.
The homogeneous introduction of organic additives is a prerequisite for good processability of ceramic powders during dry pressing. The addition of organic additives by wet route via ceramic slurries offers advantages over dry processing. The organic content can be reduced and a more homogeneous distribution of the additives on the particle surface is achieved. In addition to the measurements of zeta potential and viscosity, sedimentation analysis by optical centrifugation was also tested and successfully used to characterize the ceramic slurries and accurately evaluate of the suitability of different types, amounts, and compositions of organic additives.
Spray drying of well-stabilized slurries usually results in mostly hollow granules with a hard shell leading to sintered bodies with defects and reduced strength and density. By purposefully degrading the slurry stability after dispersion of the ceramic powder, the drying behavior of the granules in the spray drying process and thus the granule properties can be influenced. Destabilization of the slurry and thus partial flocculation was quantified by optical centrifugation. Spray drying of the destabilized alumina slurries resulted in "non-hollow" granules without the detrimental hard shell and thus improved granule properties.
Further improvement of the granules was achieved by installing ultrasonic atomization in the spray dryer. A narrower granule size distribution was achieved, which had a positive effect on, among other things, the flowability of the granules.
Specimens produced from this granules had fewer defects of smaller size, leading to better results for the density and strength of the sintered bodies. The observations made for alumina could be transferred to zirconia and as well to ZTA with 20 wt% zirconia.
In line with the industrial trend of additive manufacturing, cold spray as a non-laser-based process is becoming increasingly important for many fields of application. For the evaluation of additive manufacturing of winding components made of copper for large electrical high-voltage machines, material and component properties such as electrical conductivity, mechanical load capacity and the component size that can be produced are of particular importance. In this context, the cold spray process offers advantages over laser-based additive manufacturing processes such as laser powder bed fusion (LPBF) or laser cladding by using the kinetic energy of the copper powder particles to generate particle cohesion. To investigate the electrical conductivity as well as the mechanical load capacity of cold spray parts, specimens were machined out of cold sprayed bulk copper deposits. The characteristic values were obtained with regard to the direction of deposition, which is defined by the direction of the robot’s movement. Thus, for the investigation of the component properties, specimens were provided that had been produced both longitudinally and transversely as well as orthogonally to the direction of deposition. The results of the investigations show that both the electrical conductivity and the mechanical load capacity of the specimen have a strong preferential direction of the specimen orientation with respect to the direction of deposition. Furthermore, it could be shown that by increasing the deposition height, there is an increasing oxygen content in the sample material, combined with increasingly significant defect networks. These effects have a negative impact on the electrical conductivity as well as on the mechanical load capacity. As a conclusion, further need for investigation is identified in the optimization of the process parameters as well as in the deposition strategy for the additive manufacturing of large-volume components with cold spray.
Bei der Auslegung von Achsschenkeln für Nutzfahrzeuge wird für den Überlastfall ein fail-safe-Kriterium (kontrolliertes Versagen) als Basisphilosophie angesetzt. Gefordert wird, dass sich der Achsschenkel auch unter Akzeptanz begrenzten Risswachstums hinreichend elastisch-plastisch verformen kann, ohne dass es zum Bruch kommt. Der Fahrer soll anschließend anhand der bleibenden Verformungen bemerken können, dass mit seinem Fahrzeug etwas nicht in Ordnung ist. Eine Voraussetzung für dieses Bauteilverhalten ist eine hinreichende Bruchzähigkeit des Werkstoffs. Diese, wie auch die Rissspitzenbeanspruchung, müssen ermittelt wer-den, um den bruchmechanischen Sicherheitsnachweis führen zu können. Zur Ermittlung der mechanisch-technologischen und bruchmechanischen Werkstoffeigenschaften wurde ein Prüfkonzept entwickelt, bei dem die Proben an der potenziell kritischen Stelle direkt aus den geschmiedeten Achsschenkeln entnommen werden. Die experimentelle Werkstoffcharakterisierung bildet dann die Beanspruchungsbedingungen beim Überlastereignis ab. Im Rahmen der Produktion stehen jedoch nur Kerbschlagarbeitswerte zur Verfügung und aufwändige bruchmechanische Versuche sollen vermieden werden. Deshalb wurde eine Korrelation zur Abschätzung der vorhandenen Bruchzähigkeit aus der Kerbschlagarbeit herangezogen. Es ergibt sich eine Ergebnismatrix, die die Einflussgrößen Versagenswahrscheinlichkeit, Temperatur und Bruchzähigkeit verknüpft. Abschließend wird ein erster Vergleich der abgeschätzten mit den experimentell ermittelten Bruchzähigkeitswerten gezogen. Dieser weist aus, dass die abgeschätzten Werte geringfügig konservativ sind.
Der Kerbschlagbiegeversuch ist seit der ersten Hälfte des letzten Jahrhunderts standardisiert und seit langem als Prüfverfahren international genormt. Weltweit sind zu garantierende Werte der Kerbschlagenergie (KV) und Übergangstemperaturen (TÜ) in Produktnormen und Regelwerken festgelegt. Unter bestimmten Bedingungen besteht dabei die Option, statt Normalproben Untermaßproben zu prüfen. Im Rahmen einer Untersuchung der BAM wurde der aktuelle Status von Prüf- und Produktnormen sowie Regelwerken zur Bewertung der Bauteilintegrität hinsichtlich ihres Umgangs mit Untermaßprobenergebnissen erfasst. Zur Schaffung einer geeigneten aktuellen Datenbasis wurden an ISO-V-Proben der Dicken 2,5, 5,0, 7,5 und 10,0 mm aus vier aktuellen Baustählen KV2-T-Kurven ermittelt. Es wurden unterschiedliche Vorgehensweisen zur Kurvenanpassung und Festlegung von Übergangstemperaturen praktiziert. Ferner kamen verfügbare Ansätze zur Skalierung von Untermaßprobenergebnissen auf die Werte von Normalproben zur Anwendung. Das Ausmaß des Probendickeneffektes ist werkstoff- und temperaturabhängig. Im Bereich der Werkstoffprüfung ist akzeptiert, dass die Ergebnisse von Normal- und Untermaß-proben nicht ohne Weiteres ineinander überführt werden können. Der Stand der Produktnormung und der Regelwerke ist jedoch im besten Falle als unzureichend, vielfach jedoch schlicht als falsch zu bezeichnen. In einem weiten anwendungsrelevanten Temperaturbereich werden hier sogar deutlich nicht-konservative Skalierungsergebnisse geliefert. Die betroffenen Produkt-normenreihen und Regelwerke müssen überarbeitet werden.
The modern economy is dependent on catalysis, which is main efforts to create environmentally and energy-friendly technologies. The storage of excess electrical energy into chemical energy by splitting water into hydrogen and oxygen is a feasible solution to this energy demand. Due to their abundance on Earth and inherent stability in alkaline solution, transition-metal oxides have become one of several viable alternatives to noble-metal catalysts. Since NiFe oxide is one of the most active oxygen evolution reaction (OER) electrocatalysts for alkaline water electrolysis, it has been the subject of extensive research.
In this work, NiFe2O4 nanoparticles (NPs) of various sizes, specific stoichiometric and non-stoichiometric Fe:Ni surface ratios are synthesized. we will use a combination of ultra-high vacuum surface analysis techniques, such as time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS), to obtain the detailed characterization of the OER electrocatalysts top-surface layer, which is required to identify the rate-limiting step intermediates, and surface morphological changes at the electrolyte/catalyst.
X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials.
Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis
(2022)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. The recently started project FIB sample processing for TEM is highlighted. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved. Planed regional VAMAS Workshops in Germany in 2023 are announced.
Turbinenscheiben sind thermisch und mechanisch hochbeanspruchte, sicherheitsrelevante Komponenten in Gasturbinen. Ihre Integrität wird in Bauteiltests unter Überdrehzahlbedingungen nachgewiesen. Kontext des Aufsatzes ist die Erarbeitung einer zusätzlichen Bewertungsebene auf der Grundlage von Versuchen unter monotoner Beanspruchung, die die Beanspruchung im Bauteil realistisch wiedergeben soll. Dazu werden zwei Typen von bruchmechanischen Proben anwendungsnah ausgelegt und aus einer Turbinenscheibe ausgeschnitten: Der erste Typ ist eine biaxiale Probe, die die Beanspruchung und den Dehnungsbehinderungszustand am Diaphragm der Turbinenscheibe abbildet, die zweite eine bruchmechanische Probe, die die einachsige Beanspruchung und den Dehnungsbehinderungszustand am Bore der Turbinenscheibe wiedergibt.
Im Rahmen eines Schadentoleranzansatzkonzepts ist anschließend jeweils ein halbelliptischer Riss an den genannten Stellen der Turbinenscheibe zu betrachten. Mittels numerischer Berechnungen wird ein kritischer Punkt auf der Rissfront des Risses am Diaphragm bestimmt, dort wo die höchste Rissspitzenbelastung (J-Integral) auftritt. Auf der Basis der Rissspitzenbelastung, des Dehnungsbehinderungszustands und des entsprechenden Spannungsverhältnisses an diesem kritischen Punkt wird eine Kreuzprobe mit einem Durchriss konzipiert, die diese Verhältnisse im Bauteil widerspiegelt. Die Versuche werden unter der Temperatur am Diaphragm der Turbinenscheibe durchgeführt. Die J-R-Kurve und die plastische Kollapsgrenze werden bestimmt. Auch die einachsigen Versuche werden unter der Temperatur am Bore der Turbinenscheibe durchgeführt. Die Zugprobe enthält halbelliptische Oberflächenrisse. Ähnlich wie bei der Auslegung der Kreuzproben werden die Rissspitzenbelastung, der Dehnungsbehinderungszustand und das Spannungsverhältnis vergleichbar mit der Turbinenscheibe eingestellt. Die J-R-Kurve und die plastische Kollapsgrenze werden bestimmt.
Mit den Versuchsergebnissen werden die kritischen Lasten für verschiedene Versagensmechanismen (instabiles Risswachstum, plastischer Kollaps) der bruchmechanischen Proben ermittelt, die der kritischen Überdrehzahl der Turbinenscheibe entsprechen.
Multi-material structures are a promising solution to reduce vehicle weight and save fuel or electric energy in automotive design. However, thermal joining of steel and aluminum alloys is a challenge to overcome due to different material properties and the formation of brittle intermetallic phases. In this study, a new joining approach for producing overlap line-shaped joints is presented. The lower joining partner (EN AW 5754) is melted by a laser beam and this melt is displaced into a line-shaped cavity of the upper joining partner (1.0330) by induced Lorentz forces. The melt solidifies in the cavity to a material and form-fitting joint. This approach needs no auxiliary joining elements or filler materials. Previous investigation to produce spot-shaped joints by using this approach showed that quality and reproducibility were limited by known melt pool dynamics of aluminum alloys (keyhole collapses). For line-shaped joints, the melt displacement can take place behind the keyhole. This allows the displacement process to be spatial uncoupled from the influence of the keyhole collapses. The study shows that this improved the process stability and the quality of the joint. The created line-shaped joints were microstructurally characterized by transversal sections. Intermetallic phases were identified by electron backscatter diffraction (EBSD) and EDX-Analysis. The detected intermetallic phases consist of a 5 µm - 6 µm compact phase seam of Al5.6Fe2 and a needle shaped phase of Al13Fe4. Tensile shear tests were carried out to quantify the load capacity. It was possible to create a joint with a load capacity of about 2 kN.
A comparative analysis is performed by XPS, HAXPES and SEM of industrial functionalised graphene powder of different morphology. The chemical analysis carried out by XPS, which probing depth is around 10nm, and HAXPES, which can reach up to 30nm probing depth. By combining these two techniques is possible to get a rough, non-destructive depth profiling of the sample's surface. The results show a higher concentration of the functionlisation elements on the surface of the sample and the influence of the morphology on the functionalisation process and the C/O ratio.
Chemical bonding and coordination environments are crucial descriptors of material properties. They have previously been applied to creating chemical design guidelines and chemical heuristics. They are currently being used as features in machine learning more and more frequently. I will discuss implementations and algorithms (ChemEnv and LobsterEnv) for identifying these coordination environments based on geometrical characteristics and chemical bond quantum chemical analysis. I'll demonstrate how these techniques helped in testing chemical heuristics like the Pauling rule and thereby improved our understanding of chemistry. I'll also show how these tools can be used to create new design guidelines and a new understanding of chemistry. To use quantum-chemical bonding analysis on a large-scale and for machine-learning approaches, fully automatic workflows and analysis tools have been developed. After presenting the capabilities of these tools, I will also point out how these developments relate to the general trend towards automation in the field of density functional based materials science.
Kern des Projektes KupferDigital ist es, einen Demonstrator für ein digitales Datenökosystem zu erstellen, der der Digitalisierung der Materialforschung und der metallverarbeitenden Industrie als zukunftsfähige Plattform zur Verfügung stehen soll. Das Projekt KupferDigital entwickelt Methoden und Konzepte, um den Lebenszyklus am Beispiel von Kupfer – von der Erzgewinnung bis zum Recycling – digital zu erfassen. Grundlage ist die Entwicklung sogenannter Ontologien. Diese können als eine Art Wissensnetz verstanden werden. Sie dienen als gemeinsame Standards für die Beschreibung von Werkstoffen und technischen Vorgängen. Sie helfen bei der digitalen Erfassung von Prozessschritten sowie von Materialeigenschaften. Parallel dazu werden Konzepte für Datenstrukturen, die Speicherung und den Austausch von Werkstoffdaten über neu zu definierende Schnittstellen erarbeitet.
Über die Bereitstellung digitalisierter Lebenszyklen von Kupfer wird die Industrie bei der Pro-duktentwicklung befähigt, neue Werkstoffentwicklungen frühzeitig zu bewerten, beispielsweise unter dem Gesichtspunkt der Nachhaltigkeit. Kupfer kommt hier eine aktuelle Bedeutung zu, weil es für die digitale Transformation sowie die Energie- und Mobilitätswende von fundamentaler Bedeutung ist und somit von hohem gesellschaftlichem Wert. Die Projektziele sind sowohl auf weitere metallische Struktur- und Funktionswerkstoffe als auch auf andere Industriebereiche übertragbar.
Die Projektergebnisse werden im Rahmen der Aktivitäten der Innovationsplattform MaterialDigital allen Interessierten zur Verfügung gestellt.
Efforts towards digitalization in the material science and technology community have enhanced in the last years. In 2019 the German digitalization initiative platform „MaterialDigital“1 (MD) has been started. Numerous projects concerning digitalization, including the copper related project „KupferDigital“ (copper digital) have been initiated under the umbrella of MD. The initiative strives to
address numerous issues concerning data access, exchange, security, provenance and sovereignty. Heterogeneous data origin, storage and evaluation often result in problems concerning comparability and reproducibility of scientific and technological results. In many cases material data are recorded, but the methods of testing are insufficiently described, or such information is not communicated along with the raw data. The material data can also have numerous different formats such as paper printouts, pdfs, excel sheets or csv-files. Hence, gathering and integrating material data from different sources is challenging for potential users like materials scientists and engineers, especially if there are contradictory data where the reasons for contradictions is not clear due their vague description. In order to address these problems, data should comply to the so called „FAIR“ principle which calls for data to be findable, accessible, interoperable, and reusable (FAIR)2 and hence be accessible via so-called decentralized but interconnected data spaces. By using knowledge representation withontologies, data can be enriched with meaning and the methods of the testing procedures can be accurately provided. In this presentation we want to introduce our approach to such knowledge representation based on a high-throughput alloy development process for Cu-based alloys³ along with characterization techniques such as hardness testing and microstructural characterization (e.g. EBSD – Electron Backscattered Diffraction).
Although the slow crack growth in glass is dominated by stress-corrosion phenomena, it also should reflect the underlaying intrinsic fracture behavior controlled by glass chemistry and structure. To investigate such underlaying phenomena, crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young’s moduli and theoretical fracture surface energy. Data analysis reveals slight correlation with the packing density and significant deviations from the intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture.
XPS of GR2M
(2022)
Der Vortrag stellt nach einer kurzen allgemeinen Einleitung zur additiven Fertigung und des Laser Powder Bed Fusion Verfahrens einige Herausforderungen vor, die derzeitig den Einsatz von AM-Komponenten in sicherheitsrelevanten Anwendungen erschweren. Abschließend werden zwei Beispiele von Arbeiten der BAM gezeigt, die zur Überwindung dieser Herausforderungen beitragen können.
Differential Scanning Calorimetry (DSC) may be used to avoid testing for explosive and self-reactive properties according to the legal regulations of chemicals substances and dangerous goods.
Demonstrated measured exothermic decomposition energy value significantly affected by numerous factors - choice of sample vessel, sample mass, baseline shape, peak shape, heating rate.
Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nano- und Mikrostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet.
The microstructure of most Seljuk and Ilkhanid stucco decorations consists of micrometer-sized crystals of gypsum. The stucco-masters of these periods (neither nowadays stucco-masters) were not able to directly control the properties of these tiny crystals with their hands or centimeter-sized tools. There are, however, traces of chaîne opératoire accumulated in the materialistic body of these pieces, some of which could be explored through an interdisciplinary approach. Such an investigation requires very careful in situ observation of the macrostructure, and scientific analyses of the material to discover part of the production process for each body of stucco. Furthermore, there are deterioration factors, some of which are not yet fully understood, and should be identified using modern analytical instruments. These damaging factors could easily affect the micro and macro structure of a stucco decoration, influencing our interpretation. The concept of chaîne opératoire reframes our questions about the production process and probable dating technique of Seljuk and Ilkhanid stuccoes, while analyses of labmade replicas and historic materials enhance our understanding and interpretation of these materials. Here we present the results of such a study for a large body of Seljuk and Ilkhanid stucco decorations at various sites in Iran, and present the potential of this approach as a new perspective in this field of research.
Laser-Induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any material upon irradiation of solids with intense laser radiation. Nowadays, processing rates of up to m^2/min are enabling new industrial applications in medicine, optics, tribology, biology, etc. Depending on the specific type of LIPSS, their structural sizes typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, however, a controversial and vivid debate has emerged during the last two decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter reorganization processes, i.e. distinctly after the laser irradiation. This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches.
We investigate the molecular dynamics and electrical conductivity for a homologous series of linear shaped guanidinium based cyclic ILCs that vary in alkyl chain length, CLCRs (R = 8, 10, 12, 14, 16) by employing broadband dielectric spectroscopy (BDS), and calorimetry comprised of Fast Scanning Calorimetry (FSC) and temperature modulated FSC (TMFSC). Besides conductivity at high temperatures, the dielectric dispersion reveals two relaxation modes: the fast γ and the slow α1 relaxation. The former is assigned to the localized fluctuations while the latter is due to segmental dynamics of the alkyl chains. The γ mode slows down for long chain length CLCs (12,14,16) compared to their shorter analogues. Calorimetric investigation reveals one process, the α2 process, for all ILCs. The α2 process for CLC10, 12, and 14 has a similar temperature dependence as the dielectric α1 relaxation, while for the CLC8 and 10, it's shifted to a higher temperature. For all CLCRs, the absolute values of DC conductivity increase by 4 orders of magnitude at the transition from the plastic crystalline to hexagonal columnar phase. This increase is due to the change in the underlying conduction mechanism from delocalized electron hopping in the crystalline phase to one-dimensional ion mobility in the columnar phase. The glassy dynamics shifts to higher temperatures with increasing alkyl chain length. Conversely, the DC conductivity drops by 3 orders of magnitude from CLC8 to CLC16.
Thermoelektrische Effekte beschreiben die direkte Verknüpfung von thermischer Energie und elektrischer Energie in Festkörpern. Durch Thermodiffusionsströme entsteht direkt, ohne beweg¬liche Teile, ein elektrisches Feld als Folge einer Temperaturdifferenz. Diese Material-eigenschaft wird durch den Seebeckkoeffizienten beschrieben. Je nach Art der Ladungs¬träger sind die indu¬zierte Spannung und der Seebeckkoeffizient positiv (p-Typ) oder negativ (n-Typ). Thermo¬elek¬trische Effekte lassen sich beispielsweise in Thermo¬elementen zur Temperatur-messung, in Pel¬tierelementen zum Kühlen oder Heizen und in thermo¬elektrischen Generatoren zur Umwandlung von thermischer Energie in elektrische Energie nutzen.
In thermoelektrischen Generatoren werden Schenkel aus p-Typ- und n-Typ-Materialien elek-trisch in Reihe und thermisch parallel verschaltet. Konventionell werden einzelne Schenkel aus Bismut¬tellurid auf ein metallisiertes Substrat gelötet. Man spricht vom π-Typ-Design. Aufgrund auf¬wendiger Fertigung und nicht optimaler Flächennutzung stellt dieses Design nicht die best-mög¬liche Lösung dar. Neben Telluriden gibt es noch andere vielversprechende thermoelektrische Material¬systeme wie die oxidischen Thermoelektrika. Im Temperatur¬bereich oberhalb von 700 °C können oxidische thermoelektrische Materialien mit nichtoxidischen konkurrieren. Zudem sind sie oxidationsbeständig und können aus weniger toxischen und besser verfügbaren Rohstoffen her¬ge¬stellt werden. Da es sich um keramische Materialien handelt, können unter Nutzung der Multi¬layer¬technologie (auch Vielschicht- oder Mehrlagentechnik) Generatoren im Multilayer¬design hergestellt werden. Keramische Multi¬layer¬generatoren sind aufgrund der höheren Leis¬tungs¬dichte, der Möglichkeit der gezielten Texturierung und des hohen möglichen Auto¬mati¬sierungs¬grades des Herstellungs¬prozesses eine viel¬versprechende Alternative zu konven¬tionellen π-Typ-Generatoren. Alle Lagen werden in einem Schritt co-gesintert. Die beiden zum jetzigen Zeit¬punkt wohl viel¬versprechendsten oxi¬dischen Thermoelektrika sind Calcium-cobaltit Ca3Co4O9 als p-Typ und Calciummanganat CaMnO3 als n-Typ. Die Sinter¬tem¬peratur von Ca3Co4O9 ist durch eine Phasenumwandlung bei 926 °C beschränkt. Texturiertes, dichtes Ca3Co4O9 mit einer hohen Festigkeit kann nur über Hei߬pressen hergestellt werden. Das Co-Sintern von Ca3Co4O9 und CaMnO3 war wegen der Tem¬pera¬tur¬differenz von 350 K zwischen den jeweiligen Sinterintervallen bisher nicht möglich. Ziel dieser Arbeit war deshalb die Ent¬wick¬lung von kompatiblen oxidkeramischen Werkstoffen und Folien für thermoelektrische Multilayer-generatoren auf der Basis von Ca3Co4O9 und CaMnO3.
Daraus resultieren vier wesentliche Arbeitspakete. Zunächst die Materialentwicklungen von Ca3Co4O9 (p-Typ) und CaMnO3 (n-Typ) für ein Co-Sintern bei 900 °C mit akzeptablen thermoelek¬trischen Eigenschaften, dann die Entwicklung der weiteren im Generator benötigten Kompo¬nenten wie der Isolationsschicht und abschließend die Fertigung und Bewertung von Demonstra¬toren im Multi¬layer¬design.
Foliengießen und druckunterstütztes Sintern ermöglichen die Herstellung von dichtem, tex-turier¬tem Ca3Co4O9 mit hoher Festigkeit und hohem Leistungsfaktor. Letzterer ist das Produkt der elek¬trischen Leitfähigkeit und dem Quadrat des Seebeckkoeffizienten. Für die elektrische Leit¬fähigkeit zeigte sich in dieser Arbeit ein kombinierter Einfluss von Sinterdichte und Textur. Die thermo¬elektrischen Eigen¬schaften lassen sich somit über die Einstellung der Mikrostruktur gezielt steuern.
Durch die Optimierung der Pulversynthese, die Einführung des Sinteradditives CuO und die Kombi¬nation mit dem druckunterstützten Sintern (7,5 MPa) konnte die Sintertemperatur des CaMnO3 bei gleichbleibendem Leistungsfaktor von 1250 °C auf 950 °C gesenkt werden. Druck-unter¬stütztes Sintern von CaMnO3 ist bei 900 °C möglich, führt aber zu einem Werkstoff mit geringerem Leistungsfaktor, geringerer Dichte und ungenügender Festigkeit.
Zur elektrischen Isolation der beiden thermoelektrischen Materialien wurde ein Glas-Keramik-Kompo¬sit mit hohem Volumenwiderstand und angepasstem Wärmeausdehnungs¬koef¬fizienten ent¬wickelt.
Aus den zu Folien vergossenen thermoelektrischen Materialien, der siebgedruckten Iso¬lations-schicht und der siebgedruckten Metallisierung wurden mittels Multilayertech¬nologie De¬mons-tratoren hergestellt. Neben dem pn-Generator aus Ca3Co4O9 und CaMnO3 wurden auch Unileg-generatoren aus Ca3Co4O9 gefertigt. Bei Unileggeneratoren wird die Komplexität des Aufbaus durch die Verwendung von nur einem thermoelektrischen Material verringert. Die Simulation der Demonstratoren zeigte, dass der pn-Generator aus Ca3Co4O9 und CaMnO3 keine höheren Leis-tungsdichten erbringt als der aus nur Ca3Co4O9 bestehende Unileg¬generator. Auf¬grund des ge-ringen Leistungsfaktors und der geringen Festigkeit des bei 900 °C gesinterten CaMnO3 er¬scheint die Fertigung von pn-Multilayer¬generatoren aus Ca3Co4O9 und CaMnO3 derzeit nicht sinn¬voll. Die Unileg¬generatoren aus Ca3Co4O9 erreichen mit sehr hoher Reproduzier¬barkeit 2 mW/cm² bei einer Temperaturdifferenz von 230 K, dies entspricht 80 % der simulierten elektrischen Leistung. Es handelt sich hierbei um den ersten Machbarkeits¬nachweis zur Herstellung von Multilayer-generatoren auf Basis von texturiertem Ca3Co4O9 mit hohem thermoelektrischem Leistungsfaktor, hoher Dichte und hoher Festigkeit.
Solch thermoelektrische Multilayergeneratoren könnten zukünftig Systeme mit geringen elek-trischen Leistungsanforderungen wie Sensoren autark und nachhaltig mit elektrischer Energie ver¬sorgen.