TY - CONF A1 - Stargardt, Patrick A1 - Junge, P. A1 - Greinacher, M. A1 - Kober, D. A1 - Mieller, Björn T1 - Dielectric properties of plasma sprayed coatings for insulation application N2 - 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. T2 - Ceramics in Europe 2022 CY - Krakow, Poland DA - 10.07.2022 KW - Dielectric characterization KW - Atmospheric plasma spraying KW - Spark plasma sintering KW - Electrical insulation PY - 2022 AN - OPUS4-55328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Ciornii, Dmitri A1 - Kersting, R. A1 - Hagenhoff, B. A1 - Hodoroaba, Vasile-Dan T1 - Reliable, and reproducible physico-chemical data of nanomaterials for risk assessment N2 - 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. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Reference data KW - Risk assessment KW - Nanomaterials KW - Titania PY - 2022 AN - OPUS4-54961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Knigge, Xenia A1 - Guo, Z. A1 - Valsami-Jones, E. A1 - Radnik, Jörg T1 - Characterization of sterilized nanoparticles by lab-based XPS and HAXPES N2 - 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. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - XPS KW - HAXPES KW - Nanoparticles PY - 2022 AN - OPUS4-54968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roveda, Ilaria A1 - Serrano Munoz, Itziar A1 - Madia, Mauro T1 - Investigation of residual stresses and microstructure effects on the fatigue behaviour of a L-PBF AlSi10Mg alloy N2 - 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. T2 - 43rd Materials Mechanics Seminar CY - Sani, Chalkidiki, Greece DA - 05.06.2022 KW - AlSi10Mg KW - Fatigue KW - Neutron diffraction KW - X-ray diffraction PY - 2022 AN - OPUS4-55090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D imaging and residual stress analysis of AM materials at BAM N2 - 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). T2 - Seminar at Chalmers University and Centre for Additive Manufacture (CAM2) CY - Gothenburg, Sweden DA - 19.05.2022 KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Computed tomography KW - Synchrotron X-ray diffraction KW - X-ray refraction PY - 2022 AN - OPUS4-55019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Kai A1 - Mirabella, Francesca A1 - Mezra, Marek A1 - Weise, Matthias A1 - Wasmuth, Karsten A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Bonse, Jörn A1 - Hodoroaba, Vasile-Dan T1 - ToF-SIMS as a new tool for nano-scale investigation of ps-laser generated surface structures on Titanium substrates N2 - 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 T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Laser-induced periodic surface structures KW - Time of Flight - Secondary ion mass spectrometry KW - White light interferometric microscopy KW - Titanium alloy PY - 2022 AN - OPUS4-54992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Serrano Munoz, Itziar T1 - Multiscale residual stress analysis and synchrotron X-ray refraction of additively manufactured parts N2 - 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. T2 - Seminar at Grenoble INP, Science et Ingénierie des Matériaux et Procédés (SIMaP) CY - Grenoble, France DA - 01.07.2022 KW - Additive manufacturing KW - Residual stress KW - X-ray refraction KW - Computed tomography PY - 2022 AN - OPUS4-55232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blasón Gonzalez, Sergio A1 - Chaudry, M. A1 - Elorriaga, A. A1 - Madia, Mauro A1 - Zerbst, Uwe A1 - Llavori, I. A1 - Hilgenberg, Kai T1 - Design methodology of vessel produced by L PBF stainless steel using representative specimens N2 - 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. T2 - ECF23, European Conference on Fracture 2022 CY - Funchal, Portugal DA - 27.06.2022 KW - Additive manufacturing KW - Steel 316L KW - Fracture Mechanics PY - 2022 AN - OPUS4-55240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute T1 - Quantification of the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials N2 - 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. T2 - Nanotech France CY - Paris, France DA - 15.06.2022 KW - Optical assays KW - Functionalized nano- and microparticles KW - Particle surface analysis KW - Surface group quantification KW - Terminal functional groups PY - 2022 AN - OPUS4-55208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönherr, J. A. A1 - Duarte, Larissa A1 - Madia, Mauro A1 - Zerbst, Uwe A1 - Geilen, M. B. A1 - Klein, M. A1 - Oechsner, M. T1 - Robust Determination of Fatigue Crack Propagation Thresholds from Crack Growth Data N2 - 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. T2 - ECF23 (European Conference on Fracture 2022) CY - Madeira, Portugal DA - 27.06.2022 KW - Fatigue crack propagation threshold KW - ISO 12108 KW - ASTM E647 KW - Data evaluation methods KW - Experimental determination PY - 2022 AN - OPUS4-55252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Wolf, Jakob A1 - Emmerling, Franziska T1 - Smart Machines, New Materials, Automated Future N2 - 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. T2 - Analytica 2022 CY - Munich, Germany DA - 21.06.2022 KW - Automated synthesis KW - Nanoparticles PY - 2022 AN - OPUS4-55198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Serrano Munoz, Itziar A1 - Roveda, Ilaria A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Synchrotron x ray refraction detects microstructure and porosity evolution during in situ heat treatments in an LPBF ALSI10MG alloy N2 - 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). T2 - ICTMS 2022 CY - Grenoble, France DA - 27.06.2022 KW - Synchrotron refraction KW - In situ heating KW - AlSi10Mg alloy KW - Additive manufacturing KW - Microstructural evolution PY - 2022 AN - OPUS4-55199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fabry, Cagtay A1 - Hirthammer, Volker A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - WelDX - a file format for processing and archiving welding research data N2 - 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. T2 - International Workshop on FAIR Data in Plasma Science CY - Online meeting DA - 16.05.2022 KW - WelDX KW - Open science KW - Research data management KW - Arc welding KW - Digital transformation PY - 2022 AN - OPUS4-55153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit A1 - von Hartrott, P. T1 - Interlinking Structured Data about Aging and Fattigue of an Aluminum Alloy N2 - 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. T2 - LCF9 CY - Berlin, Germany DA - 21.6.2022 KW - Data management KW - Data linking KW - Thesaurus PY - 2022 AN - OPUS4-55159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Babutzka, Martin T1 - New findings on the formation of corrosion product layers on zinc in the atmosphere N2 - 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. T2 - 26th International Galvanizing Conference and Exhibition CY - Rome, Italy DA - 20.06.2022 KW - Atmospheric Corrosion KW - Corrosion KW - Corrosion products KW - Gel-type electrolytes KW - Zinc PY - 2022 AN - OPUS4-55113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis Alexander A1 - Rehmer, Birgit A1 - Graf, B. A1 - Ulbricht, Alexander A1 - Skrotzki, Birgit A1 - Rethmeier, Michael T1 - Low cycle fatigue behavior of DED-L Ti-6AL-4V N2 - 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. T2 - Ninth International Conference on Low Cycle Fatigue (LCF9) CY - Berlin, Germany DA - 21.06.2022 KW - AGIL KW - Additive Manufacturing KW - Ti-6Al-4V KW - Low-Cycle-Fatigue KW - Microstructure PY - 2022 AN - OPUS4-55123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Han, Ying A1 - Kruse, Julius A1 - Madia, Mauro A1 - Radners, Jan A1 - von Hartrott, Philipp A1 - Skrotzki, Birgit T1 - The influence of aging and mean stress on fatigue of Al-alloy EN AW-2618A N2 - 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. T2 - LCF9 CY - Berlin, Germany DA - 21.06.2022 KW - Fatigue KW - Aluminium alloy KW - EN AW-2618A KW - Damage Behavior PY - 2022 AN - OPUS4-55125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duarte, Larissa A1 - Madia, Mauro A1 - Zerbst, Uwe T1 - Fracture mechanics fatigue life assessmente based on effective crack propagation data obtained at closure-free conditions N2 - The use of effective crack propagation data, i.e. not affected by the crack closure mechanisms, is proposed as a reliable and robust alternative for the fatigue life assessment of cyclically loaded components. T2 - 43rd Materials Mechanics Seminar CY - Sani, Greece DA - 05.06.2022 KW - Effective crack propagation data KW - Crack-closure KW - Component assessment PY - 2022 AN - OPUS4-55044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - George, Janine T1 - Data-driven chemical understanding N2 - 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. T2 - Materials Project Seminar Series CY - Online meeting DA - 18.05.2022 KW - DFT KW - Chemical heuristics KW - Crystal Orbital Hamilton Populations KW - Machine learning KW - Phonons PY - 2022 UR - https://www.youtube.com/watch?v=e7zYrz6fgog UR - https://next-gen.materialsproject.org/community/seminar AN - OPUS4-55008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Han, Ying A1 - Radners, J. A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Aluminium High Temperature Fatigue N2 - 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. T2 - FVV Frühjahrstagung 2022 CY - Würzburg, Germany DA - 31.03.2022 KW - High Cycle Fatigue KW - Aluminium Alloy KW - EN AW-2618A PY - 2022 AN - OPUS4-54886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Florian, Camilo A1 - Mezera, Marek A1 - Wasmuth, Karsten A1 - Richter, Anja A1 - Schwibbert, Karin A1 - Krüger, Jörg A1 - Müller, F. A. A1 - Gräf, S. T1 - A brief survey on open questions about laser-induced periodic surface structures N2 - 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. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Industrial applications KW - Biofilm growth PY - 2022 AN - OPUS4-54929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Anja A1 - Buchberger, G. A1 - Stifter, D. A1 - Duchoslav, J. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Heitz, J. A1 - Schwibbert, Karin T1 - Reducing Escherichia coli adhesion to PET by modulating spatial periods of laser-induced surface nanoripples N2 - 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. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Bacterial adhesion tests KW - Bacteria repellent surfaces KW - Polymer foils KW - E. coli PY - 2022 AN - OPUS4-54930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Mirabella, Francesca A1 - Mezera, Marek A1 - Weise, Matthias A1 - Sahre, Mario A1 - Wasmuth, Karsten A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Chemical and structural changes at the surface of titanium materials upon irradiation with near-infrared ultrashort laser pulses N2 - 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. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - ToF-SIMS KW - Chemical analysis KW - Titanium PY - 2022 AN - OPUS4-54931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhu, Jiangchao A1 - Madia, Mauro T1 - Burst behaviours of aero-engine turbine disk at overspeed conditions N2 - 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. T2 - 43rd Materials Mechanics Seminar CY - Sani, Chalkidiki, Greece DA - 06.06.2022 KW - Structural integrity KW - Fracture mechanics KW - Turbine disk KW - Overspeed PY - 2022 AN - OPUS4-55081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhu, Jiangchao A1 - Madia, Mauro T1 - Fracture mechanics-based structural integrity assessment of aero-engine turbine disks under overspeed conditions N2 - 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. T2 - Turbo Expo 2022 CY - Rotterdam, Netherlands DA - 13.06.2022 KW - Structural integrity KW - Fracture mechanics KW - Turbine disk KW - Overspeed PY - 2022 AN - OPUS4-55082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelking, Lorenz A1 - Eissel, A. A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas A1 - Wesling, V. T1 - Optimisation of surface residual stresses using hybrid milling processes for additive manufactured Ni alloy components N2 - 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. T2 - ICRS11, 11th International Conference on Residual Stresses CY - Nancy, France DA - 27.03.2022 KW - Surface integrity KW - Ultrasonic-assisted milling KW - Additive manufacturing KW - Ni alloy KW - Alloy 36 PY - 2022 AN - OPUS4-54904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelking, Lorenz A1 - Eissel, A. A1 - Schröpfer, Dirk A1 - Treutler, K. A1 - Kannengießer, Thomas A1 - Wesling, V. T1 - Optimisation of surface residual stresses using hybrid milling processes for additive manufactured Nickel alloy components N2 - 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. T2 - Bachelor-, Master-, Doktoranden-Kolloquium, Otto-von-Guericke-Universität Magdeburg CY - Magdeburg, Germany DA - 18.05.2022 KW - Surface integrity KW - Ultrasonic-assisted milling KW - Additive manufacturing KW - Ni alloy KW - Alloy 36 PY - 2022 AN - OPUS4-54908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten A1 - Wilbig, Janka A1 - Müller, Ralf A1 - Nawaz, Q. A1 - Boccaccini, A.R. T1 - 3D printing of crystallizing bioactive glasses N2 - 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. T2 - ICG Berlin 2022 CY - Berlin, Germany DA - 03.07.2022 KW - Bioactive Glass KW - Crystallization KW - Sintering KW - 3D printing PY - 2022 AN - OPUS4-55253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vecchiato, Luca A1 - Meneghetti, Giovanni A1 - Moda, Giovanni A1 - Madia, Mauro T1 - Fatigue limit estimation of welded joints under constant amplitude uniaxial loading adopting the cyclic R-curve analysis N2 - 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. T2 - European Conference on Fracture 2022 (ECF23) CY - Funchal, Portugal DA - 27.06.2022 KW - Welded Joints KW - Fatigue Limit KW - Cyclic R-curve PY - 2022 AN - OPUS4-55254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander A1 - Bruno, Giovanni A1 - Mishurova, Tatiana A1 - Serrano Munoz, Itziar A1 - Roveda, Ilaria A1 - Fritsch, Tobias A1 - Ulbricht, Alexander A1 - Sprengel, Maximilian A1 - Schröder, Jakob T1 - Residual stresses and micromechanical properties of additively manufactured metals: why do we need a paradigm shift? N2 - An overview of the challenges and successes in the methodology to characherise residual stresses and micromechnical properties in additively manufactured metals T2 - CAM2 Annual Seminar 2022 - 5-year journey CY - Gothenburg, Sweden DA - 24.10.2022 KW - Additive Manufacturing KW - Residual stress KW - AGIL KW - MANUFACT KW - Micromechnical properties PY - 2022 AN - OPUS4-56466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Berger, Anka T1 - BAM Research Programm - SAPT Related to the safe transport of polymerizing substances N2 - 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). T2 - IGUS EOS ad hoc working groups - "Testing of solid oxidizers" / "Classification of energetic substances" / "Revision of test series H" CY - Frankfurt am Main, Germany DA - 21.11.2022 KW - SAPT KW - Prüfserie-H KW - Polymerisierende Stoffe KW - Zeitlicher Abbau von Stabilisatoren KW - Thermisches Verhalten KW - Transport KW - TAM IV PY - 2022 AN - OPUS4-56474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Driessche, A. E. S. T1 - Particle-mediated origins of mesocrystalline disorder in calcium sulfate single crystals N2 - 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. T2 - Granada Münster Discussion Meeting (GMDM) CY - Granda, Spain DA - 30.11.2022 KW - Anhydrite KW - Mesocrystals KW - Calcium sulfate KW - Bassanite KW - Gypsum PY - 2022 AN - OPUS4-56476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beygi Nasrabadi, Hossein A1 - Chen, Yue A1 - Hanke, T. A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Domain-level ontology formulation based on the Platform Material Digital (PMD) ontology: case study Brinell hardness N2 - 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. T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Copper KW - Materials Science KW - Ontology KW - Platform MaterialDigital (PMD) KW - Brinell hardness PY - 2022 AN - OPUS4-56092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - 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. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andresen, Elina A1 - Frenzel, Florian A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Upconversion for security tags and future applications N2 - 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. T2 - SHIFT 2022 CY - La Laguna, Tenerife, Spain DA - 10.10.2022 KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence PY - 2022 AN - OPUS4-56229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Sobol, Oded T1 - Additive manufacturing for components in hydrogen technologies N2 - 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. T2 - MPA-Workshop Hydrogen CY - Online meeting DA - 10.11.2022 KW - Additive manufacturing KW - Hydrogen KW - Technologies KW - Overview KW - Component PY - 2022 AN - OPUS4-56233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI-ToF mass spectrometry for the characterization of biobased polymers suitable for depollution N2 - 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. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - MALDI TOF MS KW - Biobased polymers KW - Depollution PY - 2022 AN - OPUS4-56237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Driessche, A. T1 - Particle-mediated origins of mesocrystalline disorder in calcium sulfate single crystals N2 - 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. T2 - ECCG: European Conference on Crystal Growth 7 CY - Paris, France DA - 25.07.2022 KW - Anhydrite KW - SAXS KW - Single crystal KW - Mesocrystal PY - 2022 AN - OPUS4-56276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Dreissche, A. T1 - Particle-mediated origins of mesocrystallinity in calcium sulfate single crystals N2 - 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. T2 - GeoMinKöln 2022 CY - Cologne, Germany DA - 11.09.2022 KW - Anhydrite KW - Mesocrystals KW - Calcium sulfate PY - 2022 AN - OPUS4-56277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kilo, M. A1 - Diegeler, A. A1 - Müller, Ralf A1 - Waurischk, Tina A1 - Reinsch, Stefan T1 - Glass Screening for the systematic development of new glasses N2 - Die technischen Möglichkeiten der robotischen Glasschmelzanlage der BAM werden vorgestellt. T2 - 26th International Conference on Glass CY - Berlin, Germany DA - 04.07.2022 KW - Material Digital PY - 2022 AN - OPUS4-56280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abderrazak, H. A1 - Marestin, C. A1 - Ibtissem, J. A1 - Mercier, R. A1 - Casablanca, H. A1 - Souissi, R. A1 - Weidner, Steffen A1 - Jaffrezic, N. A1 - Chatti, Saber T1 - Synthesis of new bio based adsorbent phases N2 - 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. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Organic-inorganic adsorbents KW - Semi-Interpenetrating Network KW - Poly(ether-sulfone) KW - Reversible adsorption. PY - 2022 AN - OPUS4-56286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brirmi, N. A1 - Mercier, R. A1 - Marestin, C. A1 - Weidner, Steffen A1 - Casablanca, H. A1 - Jaffrezic, N. A1 - Ben Romdahne, H. A1 - Chatti, Saber T1 - Effect of the pendant groups on the biobased polymers obtained by click chemistry suitable for the removal of phenolic compounds from water N2 - 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). T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Biobased polymers KW - Phenolic compounds KW - 1,2,3-triazole PY - 2022 AN - OPUS4-56287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Haider, M. B. A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - 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. T2 - AfLS3 CY - Online meeting DA - 14.11.2021 KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved KW - In situ PY - 2021 AN - OPUS4-56256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - 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. T2 - Denver X-ray Conference: DXC 2021 CY - Online meeting DA - 02.08.2021 KW - Dispersive XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2021 AN - OPUS4-56257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - 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. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 27.06.2022 KW - XAS KW - Mechanochemictry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - 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. T2 - Advances X ray Analytics Seminar at TU Berlin CY - Berlin, Germany DA - 14.06.2022 KW - XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Heilmann, Maria T1 - Nanoparticle Populations N2 - 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. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 47th Steering Committee Meeting CY - Turin, Italy DA - 18.10.2022 KW - VAMAS KW - Nanoparticles KW - Inter-laboratory comparison KW - Particle size distribution KW - Nanoparticle concentration PY - 2022 AN - OPUS4-56196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Tielemann, Christopher A1 - Müller, Ralf A1 - Busch, R. A1 - Patzig, C. A1 - Höche, T. T1 - Surface-Initiated Microstructure Formation in Glass Ceramics N2 - 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. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Glass KW - Oriented surface crystallization KW - Surface energy KW - Bond energy KW - Nucleation mode PY - 2022 AN - OPUS4-56070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Meinel, Dietmar A1 - Koptyug, A. A1 - Surmeneva, M. A1 - Khrapov, D. A1 - Paveleva, A. A1 - Surmenev, R. T1 - Procedures for quantitative characterization of periodic minimal surface structures (TMPSS) N2 - 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. T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Surface roughness KW - Additive manufacturing KW - Computed tomography KW - Wall thickness KW - Machine learning KW - Manufacturing defects PY - 2022 AN - OPUS4-56162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Serrano Munoz, Itziar A1 - Fernandez, R. A1 - Gonzalez-Doncel, G. A1 - Garces, G. T1 - A paradigm shift in the description of creep in metals can only occur through multi-scale imaging N2 - 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. T2 - Korrelative Materialcharakterisierung 2022 CY - Dresden, Germany DA - 13.10.2022 KW - X-ray refraction KW - EBSD KW - Alloys KW - TEM KW - SEM PY - 2022 AN - OPUS4-56163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -