5 Werkstofftechnik
Filtern
Dokumenttyp
- Vortrag (476)
- Zeitschriftenartikel (417)
- Posterpräsentation (116)
- Beitrag zu einem Tagungsband (76)
- Forschungsdatensatz (27)
- Buchkapitel (11)
- Dissertation (10)
- Forschungsbericht (7)
- Sonstiges (5)
- Sammelband (Herausgeberschaft für den kompletten Band) (3)
Sprache
- Englisch (982)
- Deutsch (160)
- Mehrsprachig (9)
- Französisch (2)
- Russisch (1)
Schlagworte
- Additive Manufacturing (67)
- Additive manufacturing (61)
- Corrosion (57)
- Microstructure (45)
- Glass (41)
- Ontology (40)
- Creep (36)
- Fatigue (30)
- Transmission electron microscopy (30)
- EBSD (28)
Organisationseinheit der BAM
- 5 Werkstofftechnik (1154)
- 5.1 Mikrostruktur Design und Degradation (337)
- 5.2 Metallische Hochtemperaturwerkstoffe (278)
- 5.4 Multimateriale Fertigungsprozesse (218)
- 5.6 Glas (153)
- 5.3 Polymere Verbundwerkstoffe (132)
- 5.5 Materialmodellierung (117)
- 8 Zerstörungsfreie Prüfung (110)
- 9 Komponentensicherheit (98)
- 7 Bauwerkssicherheit (91)
- 5.0 Abteilungsleitung und andere (83)
- 8.5 Röntgenbildgebung (80)
- 6 Materialchemie (68)
- 7.6 Korrosion und Korrosionsschutz (45)
- 9.4 Integrität von Schweißverbindungen (38)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (30)
- 1 Analytische Chemie; Referenzmaterialien (28)
- 6.1 Oberflächen- und Dünnschichtanalyse (28)
- 6.3 Strukturanalytik (26)
- 9.6 Additive Fertigung metallischer Komponenten (26)
- 9.0 Abteilungsleitung und andere (23)
- 4 Material und Umwelt (21)
- 9.3 Schweißtechnische Fertigungsverfahren (19)
- 3 Gefahrgutumschließungen; Energiespeicher (18)
- 8.4 Akustische und elektromagnetische Verfahren (15)
- 6.6 Physik und chemische Analytik der Polymere (12)
- 8.0 Abteilungsleitung und andere (11)
- 4.2 Material-Mikrobiom Wechselwirkungen (10)
- 8.3 Thermografische Verfahren (9)
- 9.2 Versuchsanlagen und Prüftechnik (9)
- 1.2 Biophotonik (8)
- 3.1 Sicherheit von Gefahrgutverpackungen und Batterien (8)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (7)
- 7.4 Baustofftechnologie (7)
- 1.4 Prozessanalytik (6)
- 1.6 Anorganische Referenzmaterialien (6)
- 3.0 Abteilungsleitung und andere (6)
- 4.1 Biologische Materialschädigung und Referenzorganismen (6)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (6)
- 8.6 Faseroptische Sensorik (6)
- 6.2 Material- und Oberflächentechnologien (5)
- 6.7 Materialsynthese und Design (5)
- 7.7 Modellierung und Simulation (5)
- VP Vizepräsident (5)
- VP.1 eScience (5)
- 1.9 Chemische und optische Sensorik (4)
- 2 Prozess- und Anlagensicherheit (4)
- 2.1 Sicherheit von Energieträgern (4)
- 4.3 Schadstofftransfer und Umwelttechnologien (4)
- 6.0 Abteilungsleitung und andere (4)
- 6.4 Materialinformatik (4)
- 9.5 Tribologie und Verschleißschutz (4)
- 1.7 Organische Spuren- und Lebensmittelanalytik (3)
- 3.5 Sicherheit von Gasspeichern (3)
- 7.0 Abteilungsleitung und andere (3)
- 1.0 Abteilungsleitung und andere (2)
- 3.4 Sicherheit von Lagerbehältern (2)
- 4.0 Abteilungsleitung und andere (2)
- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (2)
- 7.1 Baustoffe (2)
- S Qualitätsinfrastruktur (2)
- 1.3 Instrumentelle Analytik (1)
- 1.8 Umweltanalytik (1)
- 2.0 Abteilungsleitung und andere (1)
- 3.6 Elektrochemische Energiematerialien (1)
- 7.2 Ingenieurbau (1)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (1)
- P Präsident (1)
- P.0 Präsident und andere (1)
- S.0 Abteilungsleitung und andere (1)
- S.1 Qualität im Prüfwesen (1)
Paper des Monats
- ja (11)
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
Glasses stand out by their wide and continuously tunable chemical composition and large variety of unique shaping techniques making them a key component of modern high technologies. Glass development, however, is still often too cost-, time- and energy-intensive. The use of robotic melting systems embedded in an ontology-based digital environment is intended to overcome these problems in future. As part of the German research initiative MaterialDigital, the joint project GlasDigital takes first steps in this direction. The project consortium involves the Fraunhofer ISC in Würzburg, the Friedrich Schiller University Jena (OSIM), the Clausthal University of Technology (INW), and the Federal Institute for Materials Research and Testing (BAM, Division Glasses) and aims to combine all main basic components required for accelerated data driven glass development. For this purpose, a robotic high throughput glass melting system is equipped with novel inline sensors for process monitoring, machine learning (ML)-based, adaptive algorithms for process monitoring and optimization, novel tools for high throughput glass analysis and ML-based algorithms for glass design, including software tools for data mining as well as property and process modelling. The talk gives an overview how all these tools are interconnected and illustrates their usability with some examples.
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable
materials data space is therefore crucial in the digital transformation of an industrial branch.
A great challenge in establishing a materials data space lies in the complexity and diversity of materials science and engineering. It must be able to handle data from different knowledge areas over several magnitudes of length scale.
The Platform MaterialDigital (PMD) is expected to network a large number of repositories of materials data, allowing the direct contact of different stakeholders as materials producers, testing labs, designers and end users. Following the FAIR principles, it will promote the semantic
interoperability across the frontiers of materials classes. In the frame of a large joint initiative, PMD works intensively together with currently near 20 research consortia in promoting this exchange (www.material-digital.de).
In this presentation we will describe the status of our Platform MaterialDigital. We will also present in more detail the activities of GlasDigital, one of the joint projects mentioned above dealing with the digitalization of glass design and manufacturing.
(https://www.bam.de/Content/EN/Projects/GlasDigital/glasdigital.html)
Gläser zeichnen sich durch eine breite und kontinuierlich abstimmbare chemische Zusammensetzung sowie einzigartige Formgebungstechniken aus, was sie oft zur Schlüsselkomponente moderner Hochtechnologien macht. Die Glasentwicklung ist jedoch oft noch zu kosten-, zeit- und energieintensiv. Der Einsatz von robotergestützten Schmelzsystemen, eingebettet in eine Ontologie-basierte digitale Umgebung, soll diese Probleme in Zukunft überwinden. Im Rahmen der BMBF Forschungsinitiative MaterialDigital unternimmt das Verbundprojekt GlasDigital „Datengetriebener Workflow für die beschleunigte Entwicklung von Glas“ erste Schritte in diese Richtung. Das Projektkonsortium, an dem das Fraunhofer ISC in Würzburg, die Friedrich-Schiller-Universität Jena (OSIM), die Technische Universität Clausthal (INW) und die Bundesanstalt für Materialforschung und -prüfung (BAM, Fachgruppe Glas) beteiligt sind, will alle wesentlichen Basiskomponenten für eine beschleunigte datengetriebene Glasentwicklung zusammenführen. Zu diesem Zweck wird ein robotergestütztes Hochdurchsatz-Glasschmelzsystem mit neuartigen Inline-Sensoren zur Prozessüberwachung, auf maschinellem Lernen (ML) basierenden adaptiven Algorithmen zur Prozessüberwachung und -optimierung, neuartigen Werkzeugen für die Hochdurchsatz-Glasanalyse sowie ML-basierten Algorithmen zum Glasdesign, Data Mining sowie Eigenschafts- und Prozessmodellierung ausgestattet. Der Vortrag gibt einen Überblick darüber, wie all diese Komponenten miteinander verzahnt sind, und veranschaulicht ihre Nutzbarkeit anhand einiger Beispiele.
lasses stand out by their wide and continuously tunable chemical composition and large variety of unique shaping techniques making them a key component of modern high technologies. Glass development, however, is still often too cost-, time- and energy-intensive. The use of robotic melting systems embedded in an ontology-based digital environment is intended to overcome these problems in future. As part of the German research initiative MaterialDigital, the joint project GlasDigital takes first steps in this direction. The project consortium involves the Fraunhofer ISC in Würzburg, the Friedrich Schiller University Jena (OSIM), the Clausthal University of Technology (INW), and the Federal Institute for Materials Research and Testing (BAM, Division Glasses) and aims to combine all main basic components required for accelerated data driven glass development. For this purpose, a robotic high throughput glass melting system is equipped with novel inline sensors for process monitoring, machine learning (ML)-based, adaptive algorithms for process monitoring and optimization, novel tools for high throughput glass analysis and ML-based algorithms for glass design, including software tools for data mining as well as property and process modelling. The talk gives an overview how all these tools are interconnected and illustrates their usability with some examples.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-1. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
Planning an academic career is a bit like enjoying a box of chocolate – you never know what you are going to get next. In this talk, I will begin with sharing how luck, difficult decisions, fate, and family constraints affected my career path across continents, universities, the private sector, and to becoming a director at a national laboratory. This journey was certainly not planned and highlights how opportunities and compromises together allow you to make much more out of your engineering degree than you ever have dreamed of.
After this unusual journey as a materials scientist, I am transitioning to the technical part of my talk, where we will discuss transport in metallic glasses. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via physical aging. As a function of time, relaxation may indeed constitute significant threads to safe applications, such as a complete loss of toughness.
In the search for a physical understanding of aging, we exploit here the ability to track atomic-scale dynamics with coherent x-ray scattering. Conducted across temperatures and under the application of stress, the results reveal unexpected transport. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of atomic-scale dynamics that underly physical aging of metallic glasses. We find that classical Kohlrausch-Williams-Watts behavior is only suited for the short relaxation-time regime, whereas anomalous diffusion emerges at practically relevant times. We discuss these results in terms of the structural relaxation modes and propose a picture of a true microstructure in metallic glasses.
Plastic deformation in crystals is mediated by the motion of line defects known as dislocations. For decades, dislocation activity has been treated as a homogeneous, smooth continuous process that relies on well-average quantities. However, it is now recognized that plasticity can be determined by long-range correlated and intermittent collective dislocation activity, known as avalanches. These abrupt plastic fluctuations often exhibit pure power-law scaling or truncated power-law scaling, which indicates at least some degree of scale-free dislocation behavior. Intriguingly, such statistical signatures can persist across scales exceeding those of the material’s microstructure, raising the question of what relationship there may be between structure and long-range correlated dislocation activity that underlie power-law scaling.
In this talk, we address this question by highlighting examples in which a transition from scale-free to scale-dependent plastic deformation is observed either due to changing external testing conditions (stress-state or temperature) or by tuning the microstructure. In particular, we will focus on the details of the temperature-driven change, that demonstrates how scale-free intermittent flow in body-centered cubic Nb is progressively quenched out with decreasing temperature. The plastic response of Nb is shown to be bimodal across the studied temperature regime, with conventional thermally-activated smooth plastic flow coexisting with sporadic bursts controlled by athermal screw dislocation activity, thereby violating the classical notion of temperature-dependent screw dislocation motion at low temperatures. An abrupt increase of the athermal avalanche component is identified at the critical temperature of the material. We combine the experimental observations with 3D dislocation dynamics simulations, identify a possible origin to athermal screw activity, and discuss the co-existence scale-free and scale-dependent plasticity.
One contribution of materials science to energy efficiency is the continuous development of novel high-performance structural materials that push the strength-ductility envelope. A prominent example are modern advanced high-strength steels (AHSSs), which have enabled considerable weight reductions in the automotive sector, thereby enabling greenhouse emission reductions. To protect such advanced alloys from property degradation via corrosion, zinc (Zn) coatings are often applied through galvanization. Whilst protective, a Zn-coating comes with problems – the AHSS substrate becomes susceptible for liquid-metal embrittlement (LME) than can be the origin of significant mechanical property degradation when liquified Zn infiltrates into the steel substrate. Being for from understood, we focus here on non-cracked environments to capture the early stages of LME. This approach revealed the nucleation and growth of nano-scale intermetallic phases inside uncracked GBs (Materials Today Advances 13, 100196, 2022), highlighting the complex multi-phase microstructure developing before cracking occurs. To shed further light on the early stages of LME in AHSSs, we also consider the microstructural evolution of interrupted welds. We discuss our findings in the context of the time-resolved substructure evolution right beneath the interface between the AHSS and the Zn-based coating and track how Zn progressively infiltrates the substrate along phase and grain boundaries. The experimental results are further corroborated with thermodynamic simulations.
Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design.
Since the TEM has the capacity to observe the atomic structure of materials, in-situ TEM synthesis methods are uniquely suited to advance our fundamental understanding of the bottom-up dynamics that drive the formation of nanostructures. E-beam induced fragmentation (potentially identified as a manifestation of Coulomb explosion) and electron stimulated desorption (ESD) are phenomena that have received attention because they trigger chemical and physical reactions that can lead to the production of various nanostructures. Here we report a simple TEM protocol implemented on WO2.9 microparticles supported on thin amorphous carbon substrates. The method produces various nanostructures such as WC nanoparticles, WC supported films and others. Nevertheless, we focus on the gradual graphitization and gasification of the C substrate as it interacts with the material expelled from the WO2.9 microparticles. The progressive gasification transforms the substrate from amorphous C down to hybrid graphitic nanoribbons incorporating W nanoparticles. We think these observations open interesting possibilities for the synthesis of 2D nanomaterials in the TEM.
Gypsum (CaSO4∙2H2O) and anhydrite (CaSO4) are among the dominant evaporite minerals in the Atacama Desert [1]. They are distributed ubiquitously, and play a key role in local landscape evolution.
The formation mechanism of especially anhydrite has been a matter of scientific debate for more than a century [2]. To date, there exists no model that can reliably predict anhydrite formation at earth’s surface conditions. While thermodynamics favor its formation [3], it is hardly achieved on laboratory time scales at conditions fitting the Atacama Desert. Long induction times for nucleation have recently been modeled by Ossorio et al. [4]. However, anhydrite can be readily found in the Atacama Desert. Recently, the mineral was synthesized in flow-through reactors as a byproduct of K-jarosite dissolution at high water activity (aw=0.98) and room temperature [5], even-though the thermodynamic stability field begins only under a value of ~0.8. Additionally, recent studies investigated the nano-structure of various calcium-sulfates, which advocate for highly non-classical crystallization behavior [6]. The specific roles of particulates, ionic or organic reagents working as catalysts for the non-classical crystallization pathway remain to be determined.
Here, we present recent results from flow-through experiments as well as analyses of anhydrite samples from the Atacama Desert. Flow-through experiments were performed to systematically explore the domains of flow rate, composition, ionic-strengths and starting materials. Neither primary, nor secondary anhydrite was produced in any of these experiments. Analyses on Atacama samples reveal the existence of at least three distinct anhydrite facies, with differing mineralogy and micro- to nano-structures. The facies are (1) aeolian deposits with sub-µm grain sizes, (2) (sub-)surface nodules that formed from aeolian deposits and (3) selenites with secondary anhydrite rims. Possible mechanisms of their formation will be discussed.
Gypsum (CaSO4∙2H2O), bassanite (CaSO4∙0.5H2O), and anhydrite (CaSO4) are essential evaporite minerals for the evolution of hyper-arid surface environments on Earth and Mars (Voigt et al. 2019; Vaniman et al. 2018). The formation mechanism of especially anhydrite has been a matter of scientific debate for more than a century (van’t Hoff et al. 1903). To date, there exists no model that can reliably predict anhydrite formation at earth’s surface conditions. While thermodynamics favor its formation, it is hardly achieved on laboratory time scales at conditions fitting either the Atacama Desert on Earth, or the surface of Mars (Wehmann et al. 2023). In light of most recent developments (e.g. Stawski et al. 2016), that advocate for a complex, non-classical nucleation mechanism for all calcium sulphates, we present an analysis of natural samples from the Atacama Desert to identify key features that promote the nucleation and growth of anhydrite under planetary surface conditions. Our analyses reveal at least three distinct anhydrite facies, with differing mineralogy and micro- to nano-structures. The facies are (1) aeolian deposits with sub-μm grain sizes, (2) (sub-)surface nodules that formed from aeolian deposits and (3) selenites with secondary anhydrite rims. Possible mechanisms of their formation will be discussed.
Die Nutzung von Sensortechnologien, insbesondere im Bereich der Gasdetektion mit einem Schwerpunkt auf Wasserstoff, spielt eine entscheidende Rolle in verschiedenen Anwendungsbereichen der Wasserstofftechnologie. Sicherheitsüberwachung, Leckdetektion und Prozesskontrolle gehören zu den prominenten Anwendungsgebieten dieser Sensortechnologien. Ein zentrales Ziel ist die Erkennung von freigesetztem Wasserstoff sowie die genaue Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren. Dies ist von entscheidender Bedeutung, um potenzielle Gefahren frühzeitig zu erkennen und angemessene Maßnahmen zu ergreifen.
Ein weiterer Schwerpunkt dieses Beitrags liegt auf der Analytik und der Verwendung zertifizierter Referenzmaterialien in Verbindung mit Metrologie für die Wasserstoffspeicherung. Dies gewährleistet eine präzise und zuverlässige Charakterisierung von Wasserstoff und unterstützt die Entwicklung sicherer Speichertechnologien. Im Rahmen des Euramet-Vorhabens Metrology for Advanced Hydrogen Storage Solutions (MefHySto) wird eine Kurzvorstellung präsentiert.
Der Vortrag stellt zwei zerstörungsfreie Prüfverfahren zum strukturellen Zustandsüberwachung (Structural Health Monitoring, SHM) für Wasserstofftechnologien vor. Insbesondere die Fehlstellenerkennung mittels geführter Ultraschallwellen spielt eine bedeutende Rolle bei der Lebensdauerüberwachung von Wasserstoffspeichern. Ein weiterer Aspekt ist die Anwendung faseroptischer Sensorik zur Schadensfrüherkennung von Wasserstoffspeichern. Diese zerstörungsfreien Prüfverfahren ermöglichen eine präzise und frühzeitige Identifizierung von Schäden, was die Sicherheit und Effizienz von Wasserstoffspeichersystemen entscheidend verbessert.
1. Introduction
A normally unwanted process that can arise when converging an electron beam onto, e.g. microparticles, has been called "damage induced by electric field" (DIEF) [1]. By DIEF, the convergent electron beam (CEB) imparts a high amount of energy to the microparticle locally and strongly interacts with its atoms. At a specific current density J, which can be controlled by the convergence angle α, the irradiated material begins to transform. The phenomenon of expelling nanomaterial from microparticles under the influence of a convergent electron beam (CB) in a transmission electron microscope (TEM) has been largely studied [2]. Several types of nanoparticles (NPs) have been observed for different metallic materials and metal oxides after specific CB protocols (P) in the TEM. Thus, DIEF can be used as a promising synthesis method controlled changes of micrometric material to create new nanometric material compositions and morphologies.
While these reactions have been observed in situ at the high acceleration voltages associated with TEM, it remains unclear whether the SEM can also be used to fabricate NPs via DIEF. In contrast to TEM there is no possibility to statically convert the electron beam to a range of α to reach the needed J as in TEM. Instead, the scanning parameters and the magnification can be manipulated so as to find an integrated J. Considering that the scanning electron microscope (SEM) is easier to use, more accessible and cheaper than a TEM, here we explore the possibility to transfer the concepts of DIEF known to operate in the TEM for in situ NP generation SEM.
2. Objectives
The main goal is to determine whether DIEF can be translated to the SEM perform to controlled in situ fabrication of nanoparticles from microparticles, using gold microparticles on amorphous SiO substrate as precursors. We determine what experimental parameters must be taken into account to create SEM-based CBPs for NP creation in the SEM with these materials.
3. Materials & methods
Gold microparticles with diameter of around 1 to 3 µm were deposited on electron transparent amorphous SiO/SiO2 substrate. Using a convergent electron beam protocol (CBP) in a scanning electron microscope (SEM) at an acceleration voltage of 30 kV, the gold microparticles were irradiated until a production of NPs takes place as shown in figure 1. The beam current varied between 16 and 23 nA.
4. Results
Depending on the CBP parameters, either only Au NPs or a mixture of Au and Si NPs are produced. The particle size ranges from a few nm up to 100 nm, and it depends on the distance of the NP to the initial position of the microparticle. Further beam parameters such as the dwell time, the effective irradiated volume and particle size determine whether NPs are produced or if the microparticles only are expelled from the substrate without reacting.
5. Conclusion
The SEM can be used as an instrument for synthesizing nanomaterials via DIEF. Different CBP protocols can be applied for obtaining either gold nanoparticles or silicon + gold nanoparticles
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.