5 Werkstofftechnik
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- 5 Werkstofftechnik (114)
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- 1 Analytische Chemie; Referenzmaterialien (9)
- 6.1 Oberflächen- und Dünnschichtanalyse (9)
- 9 Komponentensicherheit (8)
- 6.3 Strukturanalytik (5)
- 3 Gefahrgutumschließungen; Energiespeicher (4)
- 5.5 Materialmodellierung (4)
- 7 Bauwerkssicherheit (4)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (4)
- 1.6 Anorganische Referenzmaterialien (3)
- 3.1 Sicherheit von Gefahrgutverpackungen und Batterien (3)
- 4 Material und Umwelt (3)
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- 9.0 Abteilungsleitung und andere (3)
- 9.3 Schweißtechnische Fertigungsverfahren (3)
- 1.2 Biophotonik (2)
- 1.4 Prozessanalytik (2)
- 8.4 Akustische und elektromagnetische Verfahren (2)
- 9.4 Integrität von Schweißverbindungen (2)
- 1.8 Umweltanalytik (1)
- 1.9 Chemische und optische Sensorik (1)
- 3.4 Sicherheit von Lagerbehältern (1)
- 3.6 Elektrochemische Energiematerialien (1)
- 5.0 Abteilungsleitung und andere (1)
- 6.4 Materialinformatik (1)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (1)
- 6.6 Physik und chemische Analytik der Polymere (1)
- 6.7 Materialsynthese und Design (1)
- 8.0 Abteilungsleitung und andere (1)
- 8.6 Faseroptische Sensorik (1)
- 9.2 Versuchsanlagen und Prüftechnik (1)
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.
The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed.
Background, Motivation and Objective
Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds.
Statement of Contribution/Methods
Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents.
Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution.
Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum).
Results/Discussion
In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm.
The presence, fate and effects of microplastics (MP) in terrestrial systems are largely unknown. The few existing studies investigated either agricultural or industrial sites. Several techniques were used for analysis, primarly spectroscopic methods such as FTIR or Raman. Sample pretreatments like density separations are common to reduce matrix. A lack of harmonised and standardised sampling instructions for microplastic investigations in the terrestrial area was identified as particular critical, because different studies are barely comparable.
The aim of the project is to develop a proposal for a harmonized procedure for sampling, sample preparation and the detection of microplastics in terrestrial matrices for total content determination. By detecting specific degradation products the thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) allows a direct determination of mass content of MP in environmental samples.
Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductivity/osteoinductivity. Nowadays, hydroxyapatite (HA) and tricalcium phosphate (TCP) are the most widespread ceramics for bone grafting at the market, however, their resorption is reported, in some cases, to be not enough. This is why the search for more soluble ceramics compared to HA and TCP looks rather viable.
A possible way to increase ceramics solubility leads to partial substitution of Ca2+-ions in Ca3(PO4)2 by alkali castions, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy, but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making study of sintering of aforementioned ceramics highly important.
For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide.
Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents.
In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS.
Es wird eine Studie zur Charakterisierung eines anisotropen Stahls vorgestellt, bei der Ultraschalluntersuchungen mit Mikrostrukturanalysen verbunden werden. Das Material weist hohe Festigkeit und Korrosionsbeständigkeit auf, zugleich ist mit anisotropen Eigenschaften die mechanischen und betrieblichen Eigenschaften beeinflussen zu rechnen. Vorläufige Ergebnisse lassen vermuten, dass weitere Untersuchungen notwendig sind, um die Fähigkeiten und Grenzen des Materials genau zu bestimmen. Es wird ein systematischer Ansatz mit Array- Prüfköpfen, Time-of-Flight Diffraction (TOFD) Technik und mikrostrukturellen Untersuchungen angewendet, um die Wechselwirkung zwischen Anisotropie und Mikrostruktur des Stahls zu analysieren. Ultraschallprüfungen mit der TOFD-Technik und in Tauchtechnik liefern Einblicke in das anisotrope Verhalten des Werkstoffes, einschließlich entsprechenden Kornorientierung, Dämpfung und Schallgeschwindigkeitsvariation. Diese Messungen führen in Verbindung mit mikrostrukturellen Analysen zu einem tieferen Verständnis des Materialverhaltens. Unser Hauptziel ist es, ein Framework zu erstellen, welches die Ultraschallantwort anisotroper Materialien mit ihren mikroskopischen Struktureigenschaften verbindet. Die vorgestellte Methodik ermöglicht eine zerstörungsfreie und zügige Bewertung der Materialintegrität, was besonders bei der Anwendung von Hochleistungsmaterialien relevant ist. Durch diesen integrativen Ansatz werden verschiedener Charakterisierungsmethoden kombiniert, um ein umfassenderes Materialverständnis zu erreichen.
The system Na2O.B2O3-SiO2 (NBS) is the basis of many industrial glass applications and therefore one of the most studied systems at all. Glass formation is possible over a wide compositional range, but the system also contains ranges of pronounced phase separation and crystallization tendency. Despite its importance, experimental data are limited to few compositional areas. The general understanding and modelling of glass formation, phase separation, and crystallization in this system would therefore be easier if small step melt series could be studied. The efficient melting of such glass series is now possible with the new robotic glass melting system at the Federal Institute for Materials Research and Testing (BAM, Division Glasses). Using three exemplary joins within this NBS system, the small step changes of glass transition temperature (Tg), crystallization behavior as well as glass density (Roh) was studied. Additionally, experimental Tg and Roh data were compared with their modeled counterparts using SciGlass and a newly developed DFT model, respectively.
The influence of prestraining on the aging response of an Al-Cu-Li alloy is investigated by preparation of different strain states (3 %, 4 %, 6 %) of the initial aging state. The Brinell hardness of the subsequently aged samples (up to 60 h aging time) was measured and it was found that the increasing dislocation concentration in the 3 different initial states leads to faster hardness increases and slightly higher maximum hardness.
The influence of heat treatment and creep loading on the microstructure of an Al-Cu-Li alloy was investigated. Especially the formation of different precipitates (T1 and Theta') were characterized and the microstructural changes under different ageing conditions (with and without external strain) were investigated to determine the effect od stress on the ageing process.
Due to their excellent combination of ductility, strength and corrosive resistance, austenitic stainless steels (ASS) are widely used in many industrial applications. Thus, these steel grades can be found as structural components in the (petro-)chemical industry, in offshore applications and more recent for storage and transport of hydrogen fuel. Steels employed for these applications are exposed to aggressive environments and hydrogen containing media. The ingress and accumulation of hydrogen into the microstructure is commonly observed during service leading to a phenomenon called “hydrogen embrittlement”. A loss in ductility and strength, the formation of cracks and phase transformations are typical features of this hydrogen-induced degradation of mechanical properties.
Although, great efforts are made to understanding hydrogen embrittlement, there is an ongoing debate of the underlying mechanisms. This knowledge is crucial for the safe use and durability of components on the one side and the development of new materials on the other.
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a powerful tool for depicting the distribution of the hydrogen isotope deuterium in the microstructure of austenitic and duplex steels. The combination with imaging techniques such as electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM), delivering structural and morphological information, creates a comprehensive picture of the hydrogen/deuterium-induced effects in the materials. All the gathered data is treated with principal component analysis (PCA) and data fusion to enhance the depth of information.
The mobility of hydrogen and deuterium in a steel microstructure is affected by external mechanical stress. To investigate the behaviour of deuterium in a strained microstructure, a new in situ experimental approach was developed. This gives the possibility of analysing samples in the SIMS instrument simultaneously to four-point-bending-tests.
Specimens made from ASS AISI 304L were electrochemically charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and hydrogen existing in the pristine material or adsorbed from the rest gas in the analysis chamber. Nonetheless, similar diffusion, permeation and solubility data allow to draw qualitative conclusions from the experiments, which are relevant for the application addressed.
The reduction of harmful emissions to the environment is one of the most urgent challenges of our time. To achieve this goal, it is inevitable to shift from using fossil fuels to renewable energy sources. Within this transition, hydrogen can play a key role serving as fuel in transportation and as means for energy storage.
The storage and transport of hydrogen using austenitic stainless steels as the infrastructure, as well as the use of these grades in hydrogen containing aggressive environments, remains problematic. The degradation of the mechanical properties and the possibility of phase transformation by ingress and accumulation of hydrogen are the main drawbacks. Advanced studies of the behaviour of hydrogen in austenite is necessary to fully understand the occurring damage processes. This knowledge is crucial for the safe use of components in industry and transportation facilities of hydrogen.
A powerful tool for depicting the distribution of hydrogen in steels, with high accuracy and resolution, is time-of-flight secondary ion mass spectrometry (ToF-SIMS). We here present a comprehensive research on the hydrogen degradation processes in AISI 304L based on electrochemical charging and subsequent ToF-SIMS experiments. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed afterwards. All the gathered data was treated employing data fusion, thus creating a thorough portrait of hydrogen diffusion and its damaging effects in AISI 304L.
Specimens were charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and traces existing in the material or adsorbed from the rest gas in the analysis chamber. Similar diffusion and permeation behaviour, as well as solubility, allow nonetheless to draw onclusions from the experiments.
Fully automated and decentralized fused filament fabrication of ceramics for remote applications
(2024)
Manufacturing of ceramic components in remote (i.e., geographically isolated) settings poses significant challenges where access to conventional manufacturing facilities is limited or non-existent. Fused Filament Fabrication (FFF) enables the rapid manufacturing of ceramic components with complex geometries. Parts formed by FFF require subsequent debinding and sintering to reach full density. Debinding and sintering are typically executed in separate steps with different equipment, necessitating extensive human handling which hinders process automation and may be challenging for the operator in isolated environments. This poster presents an innovative approach: the integration of all process steps into a single, fully automated system, streamlining the process and minimizing human involvement. Our system combines a dual extrusion filament printer with a porous and heat-resistant ceramic print bed. The porous print bed enables mechanical interlocking of the first printed layers, ensuring adhesion and structural integrity during FFF. Ceramic parts are printed onto thin sacrificial rafts, which are built using an interface material with the same binder as the ceramic filament. After the print is completed, the heat-resistant print bed with all parts is transferred seamlessly with a carrier system into a high-temperature furnace for debinding and sintering. During sintering the sacrificial raft is disintegrated, allowing for unconstrained sintering of the ceramic parts and easy removal of the finished parts. In conclusion, our integrated approach enables significant advancements in the fabrication of complex ceramic components in remote environments with increased efficiency and minimal human handling.
Morphologies of Fresnoite surface crystals of BT0.75S glass under different atmospheric conditions
(2019)
Fresnoite glass-ceramics are characterized by piezoelectric, pyroelectric and non-linear optical properties. These properties can be adjusted by orienting the fresnoite crystals during crystallization. Crystallization begins at the surface. The first surface crystals are not oriented perpendicular and, therfore, produce a surface layer that has not the intended properties. To overcome this issue, the formation of fresnoite surface crystals at different atmospheric conditions was studied.
A heat treated glass that formed crystals under controlled conditions can be a glass ceramic. A proper understanding of crystallization in glassy melts is needed yet still lacking. Involved processes include the mobility of Elements within the glass during heat treatment and the reorganization of atomic bonds during crystallization. This change in coordination number of certain elements is easily observable in bulk glass samples during heat treatment with XAS. Our plan was to monitor these reorganization processes in situ at the immediate surface during heat treatment with PEEM to get time and spatial resolved data.
As the well-known damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) are the major causes for possible failure of polyolefin-based materials, especially for PE-HD, they are highly relevant and need to be considered thoroughly. Furthermore, due to slight but perceptible differences in damaging effect, a differentiation between SCG and ESC is expedient. SCG appears in “inert” or “neutral” media without a decisive influence of the surrounding medium whereas ESC occurs in “active” media, which influence the failure behavior and time to failure crucially.
To characterize the inherent resistance of the material against those damage mechanisms, the well-established Full-Notch Creep Test (FNCT) is used. In this study, the FNCT – usually applied according to ISO 16770 [3] using a few universal model liquid media and mainly for pipe materials – is extended by investigations with appropriate parameters of selected relevant PE-HD container materials also in real media, such as the topical fuels diesel and biodiesel. The investigations were performed using a novel FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation.
Especially, mechanical stress and temperature were varied systematically during FNCT and time to failure values, time-dependent elongation data as well as detailed fracture surface analysis by laser scanning microscopy (LSM) were combined for the first time (Fig. 1). Particularly, the fracture surface analysis provides a sound basis to characterize failure behavior, mainly regarding the balance between brittle crack propagation and ductile deformation. Therefore, fracture surface analysis is an essential tool for a decent assessment of SCG and ESC by FNCT measurements.
The full-notch creep test (FNCT) is a common method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD) container materials . The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of specimens mechanically loaded in a well-defined liquid environment. Since the craze-crack damage mechanism underlying the ESC process is associated with brittle failure, the occurrence of globally brittle fracture surfaces is a prerequisite to consider an FNCT measurement as representative for ESC . Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. Due to the experimental setup, an inevitable increase of the true mechanical stress and the associated appearance of small ductile parts on fracture surfaces is induced in any case. Hence, an FNCT experiment is considered as 'valid', if the corresponding fracture surface is predominantly brittle . Based on laser scanning microscopy (LSM) height data of FNCT fracture surfaces , a universal and easy-to-use phenomenological criterion was developed to assess the validity of distinct FNCT experiments. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing.
Following the new paradigm of materials development, design, and optimization, digitalization is the main goal in materials sciences and engineering (MSE) which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR principles are to be ensured. For storage, processing, and querying of data in contextualized form, Semantic Web technologies (SWT) are used since they allow for machine-actionable and human-readable knowledge representations needed for data management, retrieval, and (re)use.
The project ‘platform MaterialDigital’ (PMD) aims to bring together and support interested parties from both industrial and academic sectors in a sustainable manner in solving digitalization tasks and implementing digital solutions. Therefore, the establishment of a virtual material data space and the systematization of the handling of hierarchical, process-dependent material data are focused. Core points to be dealt with are the development of agreements on data structures and interfaces implemented in distinct software tools and to offer users specific support in their projects. Furthermore, the platform contributes to a standardized description of data processing methods in materials research. In this respect, selected MSE methods are semantically represented on a prototypical basis which are supposed to serve as best practice examples with respect to knowledge representation and the creation of knowledge graphs used for material data.
Accordingly, this poster presentation illustrates demonstrators developed and deployed within the PMD project. Semantically anchored using the mid-level PMD Core Ontology (PMDco), they address data transformation leading to a novel data management which is based on semantic integrated data. The PMD data acquisition pipeline (DAP), which is fueled by traditional, diverse data formats, and a pipeline applying an electronic laboratory notebook (ELN) as data source are displayed. Additionally, the efficient combination of diverse datasets originating from different sources is demonstrated by the representation of a use case dealing with the well-known Orowan relation.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
In this poster presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
In this presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
The interest to additively manufacture Nickel-based superalloys has substantially grown within the past decade both academically and industrially. More specifically, additive manufacturing processes such as laser powder bed fusion (LPBF) offer the ability to produce dense parts within a single manufacturing step. In fact, the exceptional freedom in design associated with the layer-based nature of the processes is of particular interest for the complex shapes typically required in turbine applications. In certain cases, the overall part performance can be achieved by tailoring the microstructure and the crystallographic texture to the specific application. However, these advantages must be paid at a price: the large local temperature gradients associated with the rapid melting and solidification produce parts that inherently contain large residual stress in the as-manufactured state. In addition, the presence of pores in the final part may further affect the in-service part failure. As among Nickel-based alloys Inconel 718 exhibits excellent weldability, this alloy has been widely studied in open research in the domain of LPBF. However, significant microsegregation of the heavier alloying elements such as Niobium and Molybdenum accompanied by dislocation entanglements may preclude the application of conventional heat treatment schedules. Therefore, different post processing heat treatments are required for laser powder bed fused Inconel 718 as compared to conventional variants of the same alloy.
In this study, we investigated two different heat treatment routes for LPBF Inconel 718. In a first routine, the samples were stress relieved and subsequently subjected to hot isostatic pressing (HIP) followed by a solution heat treatment and a two-step age (referred to as FHT). In a second routine, the samples were subjected to a single-step direct age post stress relieving heat treatment (referred to DA). We investigated the consequences of such heat treatment schedules on the microstructure, texture, and mechanical behavior. We show that by applying a DA heat treatment the typical columnar microstructure possessing a crystallographic texture is retained, while an equiaxed untextured microstructure prevails in case of an FHT heat treatment. We further evaluate how these heat treatments affect the mechanical behaviour on the macroscopic and microscopic scale.
High- and medium-entropy alloys (HEAs and MEAs) constitute a new class of materials. Those with a face-centered cubic (fcc) structure from the Cr-Mn-Fe-Co-Ni system have excellent mechanical properties and are considered for high-temperature applications since diffusion in these alloys was reported to be sluggish. However, their corrosion resistance at high temperatures must still be evaluated to further qualify them for such kinds of applications. Various groups studied the oxidation behavior of HEAs and MEAs under (dry) laboratory and artificial air as well as CO2/CO mixtures in different temperature ranges. Adomako et al. carried out oxidation tests in dry air between 800 °C and 1000 °C for 24 h in equiatomic CrCoNi, CrMnCoNi, and CrMnFeCoNi alloys. The authors showed that CrCoNi exhibits the best corrosion resistance at 800 °C due to the formation of a protective Cr2O3 layer. The matrix below the oxide scale was reported to be correspondingly depleted in Cr. It was further shown that the addition of Mn and Fe to CrCoNi changes the phase composition of the oxide scale at 800 °C. A Mn2O3 layer was grown during oxidation on CrMnCoNi and CrMnFeCoNi and a Cr2O3 scale was formed at the matrix/oxide scale interface. Beneath these oxide layers, Mn- and Cr-depleted zones were detected. These phase morphologies demonstrate the inward diffusion of oxygen and outward diffusion of Cr and Mn resulting in the formation of Cr2O3 and Mn2O3. In the present study, the corrosion resistance of CrMnFeCoNi and CrCoNi were confirmed and additionally characterized under further oxidizing atmospheres at 800 °C including Ar-2 Vol.% O2, Ar-2 Vol.% H20, and Ar-2 Vol.% SO2 mixtures.
Currently, calcium manganate CaMnO3 and calcium cobaltite Ca3Co4O9 are being investigated as n-type resp. p-type semiconducting materials as oxidation- and temperature-resistant thermoelectric materials for oxide multilayer thermoelectric generators (TEGs). In order to manufacture multilayer TEGs, pressure-assisted sintering processes at high temperatures are necessary to achieve optimal thermoelectric material properties. To realize TEGs in planar film technology, another method to obtain dense ceramic layers directly from the synthesized starting powders without a subsequent high temperature step is emerging recently: the powder aerosol deposition (PAD) method. In the present work, it is investigated whether PAD is suitable to produce dense ceramic films from Sm-doped CaMnO3 and Ca3Co4O9 powders. The resulting thermoelectric properties are characterized as a function of temperature.
CaMnO3 powder could successfully be processed by PAD with resulting layer thicknesses of 5- 6 µm without any high-temperature sintering steps of the films. The electrical conductivity and the Seebeck coefficient of the films were determined in-plane from room temperature to 600 °C in air. The results show a Seebeck coefficient of around -200 µV/K, which is comparable to results of pressed and sintered bars. At 400 °C, the electrical conductivity corresponds to the conductivity of the bar. At higher temperatures the conductivity is better than with the reference. Below 400°C, the electrical conductivity is somewhat lower than that of the reference sample, a mild thermal treatment of the PAD layer improves it. It is expected that the thermal conductivity of the PAD film will be lower compared to the bars due to the nano-crystalline film morphology. This should result in a significantly increased ZT value for the PAD layers and a higher efficiency of the TEG.
The work shows that both CaMnO3 and Ca3Co4O9 can be successfully processed by PAD, and the PAD films show comparable thermoelectric properties.
Within NFDI-MatWerk (“National Research Data Infrastructure for Material Sciences”/ “Nationale Forschungsdateninfrastruktur für Materialwissenschaften und Werkstofftechnik“), the Task Area Materials Data Infrastructure (TA-MDI) will provide tools and services to easily store, share, search, and analyze data and metadata. Such a digital materials environment will ensure data integrity, provenance, and authorship. The MatWerk consortium aims to develop specific solutions jointly with Participant Projects (PPs), which are scientific groups or institutes covering different domains, from theory and simulations to experiments. The Data Exploitation Methods group of the Karlsruhe Institute of Technology-Steinbuch Centre of Computing, as part of TA-MDI, is developing specific solutions in close collaboration with three PPs.
PP07, together with the University of Stuttgart, aims at the image-based prediction of the material properties of stochastic microstructures using large-scale supercomputers. PP13, in cooperation with the University of Saarland, focuses on tomographic methods at various scales in materials research. PP18, together with the Federal Institute for Materials Research and Testing (“Bundesanstalt für Materialforschung und -prüfung”), aspires to define the criteria for materials reference datasets and usage analytics.
The requirements and goals are comparable for each PP: their research outputs, which are scientific datasets, should conform to the FAIR (Findable, Accessible, Interoperable, Reusable) principles. We aim to shape them from a data management perspective making use of the FAIR Digital Object concept, including structured metadata and storage solutions. The results will be a blueprint which will act as a reference for future datasets. Even though the collaboration is in an early stage, the initial steps already show the added value of this approach.
This research has been supported by the Federal Ministry of Education and Research
(BMBF) – funding code M532701 / the Deutsche Forschungsgemeinschaft (DFG, German
Research Foundation) - project number NFDI 38/1, project no. 460247524.
The aim of the task area Materials Data Infrastructure (TA-MDI) of the consortium Materials Science and Engineering (MatWerk) of National Research Data Infrastructure (NFDI) is to shape scientific datasets obtained through the Participant Projects (PPs) from a data management perspective conforming to the FAIR principles, making use of the FAIR Digital Object (FAIR DO) concept, including structured metadata and storage solutions. As an example, they apply PP18 (BAM) as a use case to demonstrate the proposed technical workflow.
The life time of mechanical components in high temperature applications is basically determined by their workings. Corrosion determines the loss of material corresponding to the loss of the effective load-bearing section and consequently increasing stress levels. To improve the material selection for such applications a numerical life prediction corrosion model for different alloys and environments is needed. Based on the ferritic alloys FeCr and FeCrCo a first quantitative model is to be developed. For this purpose, the alloys are aged at 600°C, 650°C and 700°C in synthetic air under normal pressure for between 10 and 240 hours. The first objective is to establish a quantitative relationship between the oxidation rate as a function of composition and microstructure of the alloys. The influence of the inner interface as an essential parameter for transport by diffusion on the oxidation kinetics is discussed in this presentation.
Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear.
Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield.
In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation.
Due to the advantages of additive manufacturing (AM), it has been increasingly integrated into many industrial sectors.
The application of AM materials for safety-critical parts requires the detailed knowledge about their microstructure stability under thermo-mechanical or mechanical load and knowledge on ageing process mechanisms. Ageing processes are characterized by change of the material microstructure that is to be initially investigated. This work deals with the Investigation of 316L stainless steel manufactured by selective laser melting (SLM). Describing Parameters must be defined and applied on the microstructure of these materials in their initial state and after loads were applied. The findings of this work form the basis for the investigation of AM material ageing.
Der weit verbreitete austenitische Stahl 316L soll auch mittels additiver Fertigung verarbeitet werden (316L-AM). Zur Entwicklung optimaler Aufbauverfahren ist ein detailliertes Verständnis des Gefüges notwendig. Das additiv aufgebaute Gefüge zeigt eine Mikrostruktur, die geprägt ist von sehr hohen Abkühlraten und gerichtetem Kornwachstum. Mittels klassischer Metallographie können die Charakteristika des Gefüges wie Körner, Subkörner und Schmelzlinien sichtbar gemacht werden. Mittels EBSD werden Kristallorientierungen ermittelt und bildhaft aufbereitet. Die Feinstruktur der Körner wird im REM in der Übersicht aufgelöst. Erst im TEM kann bei hoher Vergrößerung die Natur der Zellstruktur quantitativ ermittelt werden.
Additive manufacturing (AM) processes are opening new design possibilities for large scale electrical devices such as power generators. Conventional manufacturing methods use copper rods which are wrapped, vacuum impregnated, bend and welded. These processes are labor-intensive and time-consuming. The introduction of AM methods for manufacturing the copper conductor and electrical insulation can reduce the size of the generator head, the most complex part of the generator.
In this study, the electrical and dielectrical properties of additively deposited ceramic layers are investigated and compared with the properties of conventionally fabricated bulk ceramics. The ceramic layers are thermally deposited by atmospheric plasma spraying of a commercially available alumina powder. Bulk ceramics are fabricated by dry pressing and sintering of the same powder. Microstructure and porosity were analyzed by scanning electron microscopy (SEM). Electrical and dielectrical properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards.
The microstructures of sprayed and sintered alumina show significant differences with respect to grain form and porosity. The density of the bulk ceramic is lower than the density of the sprayed layer due to the coarse particle size (d50 = 33 μm). Therefore, data from dense samples of the same chemical composition but lower particle size alumina powder were used for comparison.
Multilayer thermoelectric generators are a promising perspective to the conventional π-type generators. Ceramic multilayer technology is well established for production of microelectronics and piezo-stacks. Key features of ceramic multilayer technology are full-automation, cost-effectiveness, and the co-firing of all materials in one single step. This requires similar sintering temperatures of all used materials. The development of multilayer thermoelectric generators is a subject of current research due to the advantages of this technology. One of the challenges is the compatibility of the different materials with respect to the specific design.
The presented study compares three different designs of multilayer generators based on a given set of material properties. Dualleg, unileg and transverse multilayer generators are compared to conventional π-type generators., the designs are evaluated regarding the expected maximum output power and power density using analytical calculations and FEM simulations. Additionally, the complexity of the production process and material requirements are assessed and design optimizations to simplify production are discussed.
Besides the theoretical aspects, unileg multilayer generator prototypes were produced by tape-casting and pressure-assisted sintering. These prototypes are compared to other multilayer generators from literature regarding the power factors of the used material system and the power density. Improvements of the power output by design optimizations are discussed
Introduction/purpose:
Multi-principal-element alloys (MPEAs), also known as complex concentrated alloys (CCAs), have recently come to the attention of the scientific community due to some interesting and unexpected microstructures, and their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime.
Methods:
In this contribution, the CALPHAD method is used to calculate phase equilibria for the AlMo0.5NbTa0.5TiZr CCA in the presence and absence of oxygen. Equilibrium phase amount evolution with temperature and Scheil Model for solidification (e.g. Fig.1a and Fig.1b, respectively) are analyzed, which are obtained using the databases TCNI9 and TTNI7 and the Gibbs energy minimizer in the Thermo-Calc software.
Results:
The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed. Results obtained by both databases, as well as discrepancies between property phase and Scheil approaches are discussed on the base of experimental results.
Conclusions:
A modeling tool is used to support alloy characterization and development, providing also the possibility to feedback information to improve existing thermodynamic databases.
Thermodynamic study of a refractory complex concentrated alloy (rCCA) using the CALPHAD method
(2019)
Multi-principal-element alloys (MPEAs), have recently come to the attention of the scientific community due to their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime. The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed.
Molecular orientation has a significant effect on the material properties of polymers. Preferential orientation of the microstructure (polymer chains or crystallites) in a specific direction or plane often enhances the material properties, especially if the high-strength covalent bonds are primarily exposed to loads instead of the weaker van der Waals bonds. However, the orientation-dependent microstructure and its mechanical behavior is in general already well understood by many scientific studies [1-3]. Isotropic materials are frequently required for an intrinsic material characterization without prevailing processing-induced properties, as is the case for Full Notch Creep Test (FNCT) [4] addressing environmental stress cracking (ESC) in high-density polyethylene (PE-HD) [5, 6]. Since ESC is one of the major limiting issues for long-term performance of PE-HD pipes and containers [7], which in contrast have a production-related preferential orientated microstructure due to extrusion or extrusion blow molding, it is important to additionally investigate the ESC resistance of such anisotropic microstructure.
Investigations of the slow crack growth (SCG) with respect to the molecular orientation generally obtain a factor of 1.2 up to 4.7 between crack growth perpendicular to the extrusion direction and crack growth parallel to the extrusion direction 8. Based on FNCT investigations with an aqueous detergent solution as environmental medium, hot pressed sheets with isotropic morphology are compared with extruded sheets from which specimens with different orientation angles are taken. However, the time to failure obtained by FNCT is also significantly influenced by the different cooling conditions under which the final morphology is formed. The tendency of the specimen to fail due to ESC is investigated as a function of environmental medium temperature. For a more detailed analysis of the affecting parameters in the manufacturing process, the ESC resistance is discussed considering the differences in crystallinity as revealed by thermal analysis.
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.
Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Very few observations of crystal orientation were focused on separately growing surface crystals. In conclusion, no systematic studies on initially oriented crystal growth or nucleation from defined active surface nucleation sites exists. Therefore, the main objective of this just is to advance the basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. As a first attempt, we focus on reorientation of separately growing surface crystals during their early growth.
The characterization of really unknown phases typically uses 70 to 150 reflectors for lattice metric calculation. The determination of the lattice parameters follows with 4% accuracy. Including a Z correction up to 1% can be reached. The precision of the lattice parameters ratios (a:b:c) is, however, better than 0.1%.
Fiber reinforced polymers (FRPs) are a well established material in lightweight applications, e.g. in automotive, aerospace or wind energy. The FRP components are subjected to multiaxial mechanical as well as hygrothermal loads. Common operation temperatures are in the range of 213 K and 373 K (-60 °C and 100 °C) at a relative humidity of 10% to 90%. In spacecraft applications, the environmental conditions are even more extreme. However, the correlation between multiaxial mechanical loading and harsh environment conditions have to-date not been investigated in detail. The project aims to investigate the fatigue behavior of FRPs dependent on multiaxial mechanical loading, temperature, and humidity. Extensive experimental testing is performed on flat plate and cylindrical tube specimens, accompanied by numerical and analytical calculations.
Les aubes de turbines à gaz utilisées en particulier pour les turboréacteurs de l’aéronautique sont élaborées par fonderie en superalliage monocristallin à base de nickel. Le procédé de fonderie, ainsi que les traitements thermique d’homogénéisation réalisés à très haute température, induisent la présence de pores au sein des pièces qui affectent les propriétés mécaniques et la durée de vie des aubes. Afin de réduire cette porosité les motoristes effectuent un traitement de compression isostatique à chaud (CIC) au cours duquel la porosité diminue par fermeture des pores. Afin de mieux comprendre les mécanismes impliqués au cours du traitement de CIC, nous avons lancé un programme de recherche dans le cadre du projet ERA-Net MICROPORE. La modélisation par champ de phase des mécanismes en jeu est présentée au cours de ce colloque. Nous présentons dans cette affiche un des volets de la caractérisation expérimentale du projet.
Des échantillons de superalliage CMSX4 sont observés après traitement de mise en solution et CIC sous 103 MPa à 1288°C pour différentes durées. Les pores présents sont caractérisés par microscopie électronique à balayage (MEB) afin de suivre l’évolution du taux de porosité au cours du traitement. Une caractérisation plus détaillée de pores partiellement refermés est menée par MEB et grâce à la diffraction des électrons rétrodiffusés (EBSD). Une vision tridimensionnelle de ces défauts est obtenue par des coupes métallographiques effectuées par découpe ionique (FIB).
Le projet ERA – Net MICROPORE est financé en Allemagne par la DFG (projects EP 136/1-1 and FE933/2-1) et en France par l’ANR (projects ANR15-MERA-000-03 and ANR15-MERA-0003-04).
Für die Erfassung der Verbreitung von Mikroplastik (MP) in der Umwelt ist die zeit- und kostenaufwendige Analysestrategie und der damit verbundene geringe Probendurchsatz eine limitierende Größe. Eine große Zahl verschiedener Studien dokumentriet das Auftreten von MP über den gesamten Globus. Meist sind die Studien aufgrund des großen analytischen Aufwands auf exemplarische, stichpunktartige Untersuchungen kleiner Umweltaliquoten und zahlenmäßig kleiner Probenumfänge begrenzt. Um die Verbreitung, die Eintragspfade und den Verbleib von MP in der Umwelt besser zu verstehen und effektive Vermeidungsstrategien abzuleiten, ist es jedoch notwendig, analytisch mehr Proben erfassen zu können.
Bildgebende mikro-spektroskopische Methoden wie das Raman- und FTIR-Imaging ermöglichen eine zeitaufwendige, umfassende Charakterisierung kleiner Umweltaliquoten. Neben der Partikelanzahl sind zusätzlich Informationen zu Partikelgröße, Größenverteilung und Oberflächenmorphologie zugänglich. Chemische und thermische Extraktionsverfahren sind bereits deutlich schneller und können diese Informationen durch eine Massenbilanz vervollständigen. Die analysierbare Probenmenge ist jedoch auf Milligramm Mengen beschränkt.
Wir schlagen daher vor, die Analyse von Proben auf MP durch ein vorangestelltes Screening mit der Nahinfrarot-Spektroskopie (NIRS) zur komplementieren. In diesem wird bereits eine erste Einschätzung über die Präsenz von MP in einer Probe gefällt und dadurch die wertvolle Messzeit anderer Methoden effizienter genutzt.
NIR zur Analyse von Polymeren wird seit langem eingesetzt, jedoch bisher lediglich im Rahmen einer Studie zur Mikroplastikuntersuchung mittels Hyperspektraler Bildgebung beschrieben. Der NIR Spektralbereich findet sich zwischen dem sichtbaren Licht und dem mittleren Infrarot (MIR). MIR Spektren sind durch klar definierte Banden charakterisiert, welche mehrheitlich von den Grundschwingungen der Moleküle stammen. Die höheren Energien im nahen Infrarot regen hingegen Kombinations- und Oberschwingungen der Streck und Biegeschwingungen an. Die resultierenden Absorptionsbanden sind oft breit und relativ unspezifisch. Erst mit Hilfe einer computergestützten Datenauswertung lassen sich aus diesen Spektren nützliche Informationen gewinnen. Dies erklärt die steigende Popularität der NIR-Spektroskopie in der jüngeren Vergangenheit mit einem Schwerpunkt als prozessanalytische Methode. NIR Spektrometer für das industrielle Prozessmonitoring zeichnen sich durch eine kompakte und robuste Konstruktionsweise aus. Die verfügbaren faseroptischen Reflexionssonden eignen sich gut um pulverförmige Proben zu untersuchen. Der räumlich erfassbare Messbereich kann durch die Sondengeometrie variiert werden. Sind die untersuchten Partikel im Verhältnis zur abgetasteten Fläche klein, wird als spektrale Information die Summe der Absorption aller Partikel im Sichtfeld erfasst. Die Methode ist deshalb nicht für Detailuntersuchungen von MP geeignet, erlaubt es jedoch innerhalb weniger Minuten eine Einschätzung über das Vorkommen von Mikroplastik in einer Probe zu treffen.
Exemplarisch wurden für diese Untersuchungen vier der am weitesten verbreiteten Kunststoffe Polyethylen (PE), Polyethylenterephthalat (PET), Polypropylen (PP) und Polystyrol (PS) gewählt. Aus den additivfreien Polymeren wurden nach einer Kryo-vermahlung und anschließender Siebung (< 125 µm) Modellproben generiert. Die Polymere wurden dafür zu einem Massenanteil von 1 % mit einem Standardboden (LUFA2.3, gesiebt < 125 µm) vermischt. Die Gesamtmenge von 1 g je Probe wurde in Aluminiumbehältern präpariert und 8 Messungen an unterschiedlichen, zufällig gewählten Positionen vorgenommen. Die erhaltenen Spektren wurden zur Kalibrierung chemometrischer Modelle genutzt.
In einem hierarchischen Ansatz wurde anhand der NIR-Spektren eine Klassifizierung vorgenommen:
1. Bestimmung ob eine Probe MP enthält (Ja/Nein).
2. Identifikation der Polymere in der Probe.
Eine aussagekräftige Klassifizierung beruht auf einer Vorbehandlung der Spektren. Hierdurch werden die Unterschiede zwischen den einzelnen Polymerbanden hervorgehoben. Die Eignung der so erstellten Modelle wurde anhand eines Referenzmaterials und am Beispiel von Realproben erfolgreich getestet. Dabei zeigte sich, dass nicht nur in den erstellten Polymer-Bodenmischungen, sondern auch in den Rückständen von fermentiertem Bioabfall und in Filterrückständen einer Waschmaschine, MP richtig erkannt wurde. Weiterhin zeigten Tests mit Mikroplastik-freien Bodenproben unterschiedlicher Herkunft, dass keine falsch-positive Resultate erzeugt wurden. Alle vier untersuchten Polymere, d.h. PE, PET, PS und PP mit einem Massenanteil von 1 % in einer Bodenmatrix werden auch bei einer gemischten Polymerzusammensetzung mit der NIR-Spektroskopie erkannt.
Der kombinierte Einsatz von NIRS und Chemometrie ermöglicht die Entscheidung über ein potenzielles Vorkommen sowie die Zuordnung des Materials der enthaltenen Polymerpartikel für eine Massefraktion ≥ 1 % in einer (trockenen) Probenmenge von 1 g innerhalb von 10–15 min. Der zeitaufwendige Schritt der Methode liegt hier in der Erstellung geeigneter chemometrischer Modelle sowie deren Validierung. Wesentliche Voraussetzung ist dabei, dass bei der Kalibrierung die Varianz der zu erwartenden Partikel und der Matrix realistisch abgebildet wird.
As part of a joint project involving the Fraunhofer Institute for Silicate Research (ISC), the Friedrich Schiller University of Jena, the Clausthal University of Technology and the Federal Institute for Materials Research and Testing (BAM), digital tools are to be created for the development of new types of glass materials. Current processes for the production of glasses with improved properties are usually very cost- and energy-intensive due to the low degree of automation and are subject to long development cycles. The use of robotic synthesis processes in combination with self-learning machines is intended to overcome these problems in the long term. The development of new types of glass can then not only be accelerated considerably, but also be achieved with much less effort.
In this talk, data generation via a robotic high-throughput glass melting system is presented, which should be the experimental basis for the ontology developed within the project GlasDigital.
Premature failure of glass under load is caused by sub-critical crack growth (SCCG) originate from microscopic flaws at the surface. While SCCG is related to the humidity of the ambient atmosphere, leading to stress corrosion phenomena at the crack tip, the detailed mechanism and the effect of different network formers are still not fully understood. For more clarity, various soda silicate glasses with a second network former were investigated by double cantilever beam technique: Na2O*Al2O3*SiO2 (NAS), Na2O*B2O3*SiO2 (NBS), Na2O*PbO*SiO2 (NPbS).
Three effects on the crack growth velocity, v, versus stress intensity, KI, curves were found out. The slope in region I, which is limited by corrosion, increases in the order NAS < NBS ≲ NPbS. The velocity range of region II reflecting the transition between corrosion effected and inert crack growth (region III), varies within one order of magnitude between the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For comparison, crack growth at different humidity in commercial soda lime silicate glass (NCS) was measured.
GlasDigital
(2023)
Der aktuelle Stand des MateriaDigital1 Projektes GlasDigital wird vorgestellt. Hierbei wird allgemein die Problem- und Zielstellung präsentiert, als auch auf 2 separaten Postern die Ergebnisse. Diese beinhalten zum Einen die smarte Gestaltung der robotergestützten Glasschmelzanlage der BAM inkl. Analytik und zum Anderen die Digitalisierungsbestrebungen im Bereich Glas, d.h. ML-gestützte C-S-P-Simulation, Ontologie für den Werkstoff Glas, Digitaler Zwilling des Gießprozesses.
Glass strength and fatigue is limited by surface cracks. As subcritical crack growth (SCCG) is governed by ambient humidity, stress corrosion at the crack tip is widely accepted to be the underlying mechanism. However, as water is known to have decisive effect on glass properties and can rapidly enter the crack tip near glass region, SCCG could be affected by such water related phenomena. We tried to mimic these effects studying water dissolution and speciation, mechanical properties, and SCCG in water-bearing glasses. For this purpose, glasses up to 8 wt% water have been prepared by means of high-pressure melting of glass powder - water mixtures.
As part of this effort, SCCG in dry and hydrous commercial micros¬cope slide glass (CW = 6 wt%) was studied in double cantilever beam (DCB) geometry and sub-Tg relaxation was measured by Dynamic Mechanical Analysis (DMA).
For SCCG in ambient air (24% r.h.), SCCG was promoted by the presence of 6wt% bulk water with respect to the dry glass. On the other hand, stress intensity values, KI, required to cause slow crack growth (v < 10-6 ms-1) resemble literature findings for float glass of similar composition in liquid water, which might represent the maximum possible promoting effect of ambient water on SCCG.
For SCCG in vacuum (10-3 mbar), dissolved bulk water causes even more pronounced effects. Most strikingly, it strongly decreases the slope of the log v(KI)-curve, which is a measure of dissipated energy during fracture. A strong increase of sub-Tg relaxation with increasing water content was confirmed by DMA. As a consequence, slow crack growth occurs at KI values as measured in the dry glass whereas fast crack growth occurs at much larger KI than that of the dry glass. Kinks and shoulders shown by the inert log v(KI)-curve indicate that bulk water does not simply affect bulk mechanical properties.