Ingenieurwissenschaften und zugeordnete Tätigkeiten
Filtern
Erscheinungsjahr
Dokumenttyp
- Posterpräsentation (804) (entfernen)
Sprache
- Englisch (669)
- Deutsch (134)
- Französisch (1)
Schlagworte
- Corrosion (36)
- Additive manufacturing (30)
- Mechanochemistry (24)
- Additive Manufacturing (20)
- Glass (20)
- Nanoparticles (19)
- Crystallization (17)
- Fluorescence (15)
- Degradation (14)
- In situ (14)
Organisationseinheit der BAM
- 6 Materialchemie (207)
- 5 Werkstofftechnik (97)
- 8 Zerstörungsfreie Prüfung (97)
- 6.3 Strukturanalytik (65)
- 8.5 Röntgenbildgebung (61)
- 6.6 Physik und chemische Analytik der Polymere (56)
- 9 Komponentensicherheit (54)
- 6.1 Oberflächen- und Dünnschichtanalyse (48)
- 1 Analytische Chemie; Referenzmaterialien (46)
- 4 Material und Umwelt (36)
- 7 Bauwerkssicherheit (34)
- 5.1 Mikrostruktur Design und Degradation (28)
- 6.0 Abteilungsleitung und andere (26)
- 1.2 Biophotonik (25)
- 5.4 Multimateriale Fertigungsprozesse (22)
- 9.4 Integrität von Schweißverbindungen (20)
- 4.1 Biologische Materialschädigung und Referenzorganismen (19)
- 5.2 Metallische Hochtemperaturwerkstoffe (19)
- 5.6 Glas (19)
- 6.2 Material- und Oberflächentechnologien (19)
- 9.3 Schweißtechnische Fertigungsverfahren (19)
- 2 Prozess- und Anlagensicherheit (14)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (14)
- 8.0 Abteilungsleitung und andere (14)
- 7.1 Baustoffe (13)
- 6.7 Materialsynthese und Design (12)
- 3 Gefahrgutumschließungen; Energiespeicher (11)
- 4.2 Material-Mikrobiom Wechselwirkungen (11)
- 7.6 Korrosion und Korrosionsschutz (11)
- 8.3 Thermografische Verfahren (11)
- 9.6 Additive Fertigung metallischer Komponenten (9)
- 1.9 Chemische und optische Sensorik (8)
- 5.3 Polymere Verbundwerkstoffe (8)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (8)
- 8.4 Akustische und elektromagnetische Verfahren (8)
- 1.4 Prozessanalytik (6)
- 9.0 Abteilungsleitung und andere (6)
- 2.5 Konformitätsbewertung Explosivstoffe/Pyrotechnik (5)
- 3.1 Sicherheit von Gefahrgutverpackungen und Batterien (5)
- 4.5 Kunst- und Kulturgutanalyse (5)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (5)
- 9.5 Tribologie und Verschleißschutz (5)
- 1.6 Anorganische Referenzmaterialien (4)
- 2.0 Abteilungsleitung und andere (4)
- 5.5 Materialmodellierung (4)
- 9.2 Versuchsanlagen und Prüftechnik (4)
- 1.5 Proteinanalytik (3)
- 2.1 Sicherheit von Energieträgern (3)
- 4.0 Abteilungsleitung und andere (3)
- 7.2 Ingenieurbau (3)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (3)
- 8.6 Faseroptische Sensorik (3)
- VP Vizepräsident (3)
- VP.1 eScience (3)
- 1.1 Anorganische Spurenanalytik (2)
- 2.2 Prozesssimulation (2)
- 3.2 Gefahrguttanks und Unfallmechanik (2)
- 3.4 Sicherheit von Lagerbehältern (2)
- 1.8 Umweltanalytik (1)
- 3.0 Abteilungsleitung und andere (1)
- 3.3 Sicherheit von Transportbehältern (1)
- 3.6 Elektrochemische Energiematerialien (1)
- 5.0 Abteilungsleitung und andere (1)
- 6.4 Materialinformatik (1)
- 7.4 Baustofftechnologie (1)
- MP Mitglied des Präsidiums (1)
- MP.0 Mitglied des Präsidiums und andere (1)
- P Präsident (1)
- PST Präsidiale Stabsstelle (1)
Eingeladener Vortrag
- nein (1)
Zirconium chloro fluoride as catalyst for C-F bond activation and HF transfer of fluoroalkanes
(2024)
In this work1, we have successfully synthesised amorphous zirconium chloro fluoride (ZCF), which exhibits medium lewis acidity. In addition to investigating the local coordination sphere around the Zr atoms and the material properties, we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present the first heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
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.
Since microplastics (MPs) can be found everywhere and are becoming a problem of high concern, it is necessary to understand their occurrence and fate in the environment. However, to obtain data of high quality is very challenging, since measurement operating procedures differ from laboratory to laboratory. Currently, there are no standardized methods to analyze microplastics. One promissing possibility to adress standardization of the methodology and operating procedures are interlaboratory comparisons (ILCs). In this contribution we report the first results of an ILC on microplastic detection methods organized under the pre-stantdardisation plattform of VAMAS (www.vamas.org/twa45/) as Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods”, within the Technical Working Area TWA 45 “Micro and Nano Plastics in the Environment”. The ILC has gathered 84 participants all over the world representing all continents. BAM, as the project leader, produced a set of reference microplastic materials, which have been distributed to all the participants together with the measurement protocols and reporting data templates.
Monitoring of microplastics in food matrices is crucial to determinate the human exposure. By direct ingestion microplastics could be released in the food during the production, through packaging and by consumer’s use. The absence of standard methods to quantify and detect different size range and type of microplastics has led to difficult and time consuming procedural steps, poor accuracy and lack of comparability. In this work, matrix characterization and laboratory experiments were used to investigate the efficiency of sample preparation in milk powder. This information is crucial to compile a standard procedure for sample preparation and digestion of common milk powder to detect different particle sizes and types of polymers. Charaterisation is done by TGA and TOC measurements.
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.
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.
This paper outlines significant advancements in our previously developed aerial gas tomography system, now optimized to reconstruct 2D tomographic slices of gas plumes with enhanced precision in outdoor environments. The core of our system is an aerial robot equipped with a custom-built 3-axis aerial gimbal, a Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor for CH4 measurements, a laser rangefinder, and a wide-angle camera, combined with a state-of-the-art gas tomography algorithm. In real-world experiments, we sent the aerial robot along gate-shaped flight patterns over a semi-controlled environment with a static-like gas plume, providing a welldefined ground truth for system evaluation. The reconstructed cross-sectional 2D images closely matched the known ground truth concentration, confirming the system’s high accuracy and reliability. The demonstrated system’s capabilities open doors for potential applications in environmental monitoring and industrial safety, though further testing is planned to ascertain the system’s operational boundaries fully.
SWIR luminescent nanomaterials – key chemical parameters for bright probes for in vivo bioimaging
(2024)
A current challenge for studying physio-pathological phenomena and diseaserelated processes in living organisms with non-invasive optical bioimaging is the development of bright optical reporters that enable deep tissue penetration, a high detection sensitivity, and a high spatial and temporal resolution. The focus of this project are nanomaterials, which absorb and emit in the shortwave infrared (SWIR) between ~900–2500 nm where scattering, absorption, and autofluorescence of the tissue are strongly reduced compared to the visible and NIR.
Currently, mandatory requirements and recommendations for the detection of irregularities in laser beam welded joints are based on classic micrographs as set out in the standard ISO 13919-1:2019. Compared to classic micrographs, computed tomography enables a non-destructive, three-dimensional and material-independent mode of operation, which delivers much more profound results. Even in building material testing, methods with limited informative value can be checked and supplemented by CT examinations.
Explosionsverletzungen gehören zu den häufigsten Verletzungen bei militärischen Einsätzen. Während die Auswirkungen von Splittern, die als sekundäre Explosionsverletzungen eingestuft werden, durch die modernen ballistischen Körperschutzsysteme der Polizei und des Militärs minimiert werden konnten, stellen die Auswirkungen der Stoßwellenausbreitung im Körper als Teil des primären Explosionstraumas nach wie vor eine ernsthafte Bedrohung dar. Zusätzlich zu einzelnen einsatzbedingten Lastfällen liegt ein wissenschaftlicher Fokus auf besonders exponiertem Personal, z.B. aus den Einsatzbereichen „Taktische Zugangstechnik“, „Präzisionsschützenwesen“ oder Steilfeuerwaffen (Mörser). Repetitive mild traumatic brain injury (mTBI) können gesundheitliche Langzeitschädigungen wie und chronic traumatic encephalopathy (CTE) erzeugen.
Um einen Beitrag zur Erforschung der primären Explosionswirkungen zu leisten, hat die Bundeswehr in Zusammenarbeit mit dem Bundeswehrkrankenhaus Berlin und der Bundesanstalt für Materialforschung und -prüfung (BAM) ein interdisziplinäres wehrmedizinisches Sonderforschungsvorhaben eingerichtet. Ziel der geplanten Untersuchung ist die Entwicklung einer multidisziplinären Methode zur Analyse des Stoßwellenverhaltens in verschiedenen generischen Gewebesimulanzien, sowie Schutzmaterialien unter möglichst realitätsnahen und reproduzierbaren Bedingungen.
Für die Erzeugung reproduzierbarer Stoßwellen wurde ein Autoklav
(Druckbehälter) entwickelt, mit dem durch die detonative Umsetzung eines Acetylen-Sauerstoff-Gemisches gut reproduzierbare Druckwellen unter Freifeldbedingungen erzeugt werden können. Vorteile dieser Methode sind unter anderem die kurzen Rüstzeiten zwischen Versuchsdurchgängen, die Minimierung störender Einflüsse im Vergleich zu Stoßwellenrohren und die geringeren Sicherheitsanforderungen im Vergleich zur Anwendung von konventionellen Sprengstoffen. Das generische Torso-Modell besteht in seiner einfachsten Form aus einem mit Druck- und Beschleunigungssensoren instrumentierten Gelatineblock, welcher eine Simulanz für organisches Gewebe darstellt. Zur Untersuchung des Stoßwellenverhaltens wurden verschiedene Medien, wie Hohlkörper, Festkörper und Gewebesimulanzien differenter Dichte in das generische Torso-Modell eingebracht. Einen besonderer Untersuchungsschwerpunkt bildeten die Grenzbereiche zwischen den unterschiedlichen Medien. Des Weiteren wurde analysiert, wie sich verschiedene Schutzmaterialien auf das Stoßwellenverhalten auswirken und mit welchen veränderten Eigenschaften die Stoßwelle anschließend in die Gewebesimulanz einkoppelt.
Nowadays, people spend most of their time indoors. Thus, a good indoor air quality is important. Emissions of volatile organic compounds (VOCs) from furniture and building materials can cause health complaints1. Quantitative VOC-emission testing is carried out under standardized conditions in emission test chambers. In the presented project an emission reference material (ERM) is developed that emits a defined mixture of VOCs which is required for quality assurance and -control (QA/QC) measures. Porous materials (e.g zeolites, activated carbons, MOFs or aerogels) are used as reservoir materials and impregnated with VOC. The porous materials are selected, among others, by their pore size, pore size distribution, polarity and availability. Due to their regular pore structure zeolites are tested at first. For a prediction of the emission profile, the ERM is supposed to exhibit a constant emission rate over time. The aim is a stability of ≤ 10 % change in the emission rate over a minimum of 14 days.
Method
For impregnation, the material is placed into an autoclave inside a rotatable basket. The VOC is added and the autoclave is closed. Afterwards, CO2 is inserted. The closed system is then heated to the supercritical point of CO2 (31 °C, 73.75 bar). In this state, the CO2 acts as solvent for the VOC. By rotating the basket, the distribution of the VOC is ensured. After a few minutes, the pressure is decreased slowly and the CO2 is released. For the determination of the emission profile, the impregnated sample is placed into an emission test chamber. These chambers can be operated either with dry or humid air (50 ± 5 % rel. humidity). Every second to third day, air samples are taken and analyzed by gas chromatography. For an ideal impregnation, several different pressures and temperatures as well as impregnation times are tested.
Results
Two zeolite materials tested in dry air conditions reach emission profiles with a decrease of less than 10 % over 14 days (heptane and toluene, respectively). Further it was discovered that smaller pellets of the same zeolite show better results than bigger particles. When the pore size of a zeolite is too small, e.g. 0.3 nm, the VOC cannot be absorbed sufficiently. The main disadvantage of zeolites is their hygroscopicity because it has a large impact on the release of VOC when they are used in emission test chambers under standardized test conditions (23 °C, 50 % rel. humidity). Activated carbons have emission profiles with a larger change over 14 days. However, the high hydrophobicity allows measurements in humid air conditions which was not possible with the before mentioned hygroscopic zeolites. It is possible to impregnate powdered materials as well, and thus powdered non-hygroscopic (n.h.) zeolites were impregnated. Their emission profiles are comparable to those of the activated carbons. The use of methylated hygroscopic zeolites with a decrease in hygroscopicity did not yield successful emission measurements. The change over 14 days is calculated only for the stable phase (~250–300 h).
The desired stability of ≤ 10 % change of the emission rate over 14 days could already be reached under dry testing conditions. Further investigations under humid conditions show that zeolites with high Si/Al-ratios are non-hygroscopic and comparable to activated carbons (20–30 % change). The next step is to reduce the change in the emission rate of these materials to the aimed ≤ 10 % over 14 days.
For a deep process understanding of the laser powder bed fusion process (PBF-LB/M), recording of the occurring surface temperatures is of utmost interest and would help to pave the way for reliable process monitoring and quality assurance. A notable number of approaches for in-process monitoring of the PBF-LB/M process focus on the monitoring of thermal process signatures. However, due to the elaborate calibration effort and the lack of knowledge about the occurring spectral directional emissivity, only a few approaches attempt to measure real temperatures. In this study, to gain initial insights into occurring in the PBF-LB/M process, measurements on PBF-LB/M specimens and metal powder specimens were performed for higher temperatures up to T = 1290 °C by means of the emissivity measurement apparatus (EMMA) of the Center for Applied Energy Research (CAE, Wuerzburg, Germany). Also, measurements at ambient temperatures were performed with a suitable measurement setup. Two different materials—stainless steel 316L and aluminum AlSi10Mg—were examined. The investigated wavelength λ ranges from the visible range (λ-VIS = 0.40–0.75 µm) up to the infrared, λ = 20 µm. The influence of the following factors were investigated: azimuth angle φ, specimen temperature TS, surface texture as for PBF-LB/M surfaces with different scan angles α, and powder surfaces with different layer thicknesses t.
Lithium-ion batteries are a key technology for tackling challenges in energy and climate crisis, but up to 30 % are discarded right after production. Quality is closely related to the homogeneity of the used materials and coatings. Fluorine compounds, both in the polymer and from degradation of the electrolyte, are of special interest for the formation and aging of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) emerged as a fast and convenient method for depth-profiling of battery materials. However, fluorine remains a spectroscopic challenge due to a high excitation energy and only few strong emission lines in the UV/Vis spectral range.
We investigated the partial substitution of argon with neon in the plasma gas. The main emission line at 685.603 nm was monitored by both photo multiplier tube (PMT) with Czerny-Turner monochromator at 20 µm slit-size, and charge-coupled device (CCD) with 1200 lines/mm grating. For calibration, we used a set of hot-pressed copper cylinders with varying calcium fluoride amount fraction, ranging from 1.6 % to 4.4 %. Plasma gas mixtures with a mole fraction of 5 %, 10 % and 20 % neon in argon were used. Sensitivity in comparison to pure argon was increased by factor 4, 7 and 14, respectively. In general, PMT detection was more sensitive than CCD. As expected, sputter rates decreased with higher neon content in the plasma gas. Depth-profiling of the cathodes was performed in pulsed mode at constant voltage and pressure, which resulted in stable plasma conditions. We achieve matrix-independent quantitative information on fluorine distribution by correction based on sputter rates.
This advancement in GD-OES provides a more accurate analytical approach for evaluating the homogeneity of lithium-ion battery materials, potentially leading to more sustainable and cost-effective manufacturing processes.
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.
This poster presents an approach to create and maintain a comprehensive and intuitive MSE-centric terminology by developing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures.
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.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Nanopipettes are a type of solid-state nanopore with needle-like geometry. Their applications range from imaging, sensing, diagnostics, and use as injectors. The response of nanopipette sensors is highly dependent on the size, geometry and chemical properties of the sensing region. As nanopipettes are increasingly tuned and modified for specific analytes, a better understanding of the surface chemistry and morphology of the inner channel is necessary. For exploring these effects, quartz nanopipettes were modified by gas phase silanization, a well-utilised technique in the field to enhance performance of nanopipettes, and further functionalised with a metal bis thiolate complex, to aid in chemical analysis. The inner channel of the sensing region was exposed with focused ion beam (FIB) milling as a dedicated sample preparation method for nanoscale surface analysis. The sample characterisation involved scanning electron microscopy (SEM), Auger electron spectroscopy (AES) and low-energy energy dispersive x-ray spectroscopy (EDX). The results demonstrate the first steps towards full characterisation of nanopipettes at the nanoscale, notably with access to the inner channel. The methods used here can be applied to gain further understanding of the response of these sensors to complex analytes, and allow for the study of different surface functionalisation at the all-important sensing region.
Nanopipettes are a type of solid-state nanopore with needle-like geometry. Their applications range from imaging, sensing, diagnostics, and use as injectors. The response of nanopipette sensors is highly dependent on the size, geometry and chemical properties of the sensing region. As they are increasingly tuned and modified for specific analytes, a better understanding of the surface chemistry and morphology of the inner channel is necessary. With the aim of developing a comprehensive approach for characterisation of such nanopipettes, this research focuses on combining surface-sensitive analysis methods with advanced sample preparation techniques. Quartz substrates were modified by gas phase silanization, a well-utilised technique in the field to enhance performance of nanopipettes, and further functionalised with a metal bis thiolate complex, to aid in chemical analysis. The sample characterisation involved scanning electron microscopy (SEM), low-energy dispersive x-ray spectroscopy (EDX), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Auger electron spectroscopy (AES). Using focused ion beam (FIB) milling under gentle conditions, the inner surface of quartz nanopipettes was exposed whilst preserving the integrity of the overall structure (see figure). Owing to the challenging analysis conditions, modification and analysis of flat quartz substrates has been performed in parallel for optimisation purposes. The results demonstrate the first steps towards full characterisation of nanopipettes at the nanoscale, notably with access to the inner channel. The methods used here can be applied to gain further understanding of the response of these sensors to complex analytes and allow for the study of different surface functionalisations at the all-important sensing region.
Multiphoton lithography (MPL), an emerging microfabrication technique, shows great potential in a variety of applications ranging from tissue engineering to soft micro-robotics. Fabricated micro-objects often are expected to undergo shape morphing or bending. Furthermore, ensuring precise property tuning becomes detrimental for the functionality of MPL microstructures. Herein, we present novel MPL materials based on interpenetrating networks (IPNs), which effectively combine the advantages of acrylate and epoxy thermoset systems. A library of 3D MPL IPN microstructures with high 3D structural stability and tailored thermal and micromechanical properties is achieved. MPL laser velocity and fabrication power can be used to tune the morphology and therefore properties of IPN. New IPN microstructures with materials Young's moduli of 4 to 6 MPa demonstrate susceptibility to deformation with high to fully elastic response. Such soft elastic materials hold immense promise within morphable microsystems, soft micro-robotics and cell engineering applications.
Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer showed a deviation for both poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone.