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Thermal spraying provides a rapid method for additive deposition of various ceramics as electrical insulation in applications where polymers are not suitable. New applications in complex shaped additive manufactured metal parts are emerging for example in large scale electrical devices. Microstructural and dielectric evaluation of coatings is crucial to the employment of such free-form processes. The properties and microstructure of the plasma sprayed alumina coatings are compared with dense reference samples of the same powder produced by spark plasma sintering (SPS). To obtain dense bulk samples from the coarse alumina powder for spray coating, SPS is used.
Samples are fabricated by atmospheric plasma spraying (APS) of commercially available alumina powder (d50 = 33 µm) on copper substrates and by SPS of the same powder. Microstructure and porosity were analyzed by optical microscopy and scanning electron microscopy (SEM). Phase compositions were determined by X-ray diffraction (XRD). Dielectric properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructure and dielectric properties of the coating and bulk material are compared to assess whether the coating is suitable for use in electrical insulation application.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is increasingly used to study the distribution of metal-containing drugs, imaging probes and nanomaterials in connection with disease related changes and therapy progress. Additionally, biomolecules can be detected indirectly by using metal-tagged antibodies.
The extracellular matrix (ECM) is, besides the cells, an important component of all body tissues. The macromolecular network of the ECM consists of structural proteins (e.g., collagen, elastin) and proteoglycans composed of highly negatively charged carbohydrates, the glycosaminoglycans (GAGs), which are covalently linked to a protein core. Many diseases, including inflammatory processes and tumors, are associated with characteristic ECM changes at an early stage. Recent studies have shown that contrast agents for magnetic resonance imaging (MRI), which are based on gadolinium containing chelate complexes or iron oxide nanoparticles, can bind themselves to ECM components.
To elucidate the role of GAGs like keratan sulfate (KS) and its modification state in disease, highly specific tools are necessary. As a complement to conventional immunohistochemistry LA-ICP-MS was applied to investigate the distribution of KS in tissue thin sections using a well characterized anti-KS antibody labelled with metal ions. Furthermore, LA-ICP-MS was used for the detection of MRI contrast agents and the identification of their target cells and molecules in tissue samples from animal models, e.g. for cardiovascular diseases. The results show the possibilities of LA-ICP-MS for the elucidation of pathological tissue changes.
Nanoforms with at least one dimension below 100 nm have an important part to play in more and more areas of our daily life. Therefore, risk assessment of these materials is becoming increasingly important. In this context, the European Chemical Agency (ECHA) considered eleven physico-chemical properties as relevant, of which the following six are essential for the registration: chemical composition, crystallinity, particle size, particle shape, surface chemistry and specific surface area. Four of these priority properties can be obtained with electron microscopy and surface analytics like XPS and ToF-SIMS. The reliability of this data must be ensured, especially for their use for grouping and read across approaches. On the other hand, the “reproducibility” crisis has revealed major shortcomings in the reliability of published data.
In a case study, we show how the quality of the data can be ensured by using existing standards and protocols of each step in the workflow of sample characterization. As exemplary samples, two Al-coated TiO2 samples as nanopowders were selected from the JRC repository, capped either with a hydrophilic or a hydrophobic organic ultrathin shell. SEM results provided the size and shape of the nanoparticles, a first overview about the composition was obtained with EDS. XPS and ToF-SIMS supplied the surface chemistry, especially information about the shell and the coating of the particles. Standards and protocols of all steps of the analytical workflow including preparation and data reduction are discussed regarding reliable and reproducible data. Additionally, uncertainties for the different steps are specified.
Only such a detailed description of all these factors allows a comprehensive physico-chemical characterization of the nanoparticles with understanding of their potential risk assessment.
The recent development of x-ray photoelectron spectroscopy using excitation sources different from the usual lab-source Mg Kα and Al Kα and spectrometers with more sophisticated lens systems requires flexible approaches for determining the transmission function. Therefore, the approach using quantified peak areas (QPA) was refined.1 A new algorithm allows a more precise estimation of the transmission function which could be shown by comparing the results obtained with the new version with former calculations. Furthermore, next to the established reference materials Cu, Ag and Au, ionic liquids can be used for estimating the transmission function at beamlines with variable excitation energies. Comparison between the measured and stoichiometric composition shows that a transmission function was determined which allows a reasonable quantification.
microscopy (AFM), or X-ray reflectometry. For the additional determination of thin film composition, techniques like X-ray photoelectron spectroscopy (XPS) or mass spectrometry-based techniques can be used. An alternative non-destructive technique is electron probe microanalysis (EPMA). This method assumes a sample of homogenous (bulk) chemical composition, so that it cannot be usually applied to thin film samples. However, in combination with the thin film software StrataGEM, the thickness as well as the composition of such films on a substrate can be determined.
This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). These samples were used for an international round robin test.
In 2021, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios).
In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BadgerFilm software package and compared the resulting composition and thickness with the results of the established StrataGEM software and other reference methods. With the current evaluation, the BadgerFilm software shows good agreement with the composition and thickness calculated by StrataGEM and as the reference values provided by the KRISS.
The novel lab-based HAXPES spectrometer (ULVAC-PHI Quantes) gives us the possibility to measure XPS at 1486.6 eV (monochromatic Al Kα source) and HAXPES at 5414.9 eV (monochromatic Cr Kα source) on a sample at the same position. The surface analysis with this spectrometer leads to an information depth of about 10 nm for XPS and in comparison, to an analysis of deeper regions of about 30 nm for HAXPES measurements. This method provides a nondestructive way to distinguish between the near-surface region of the nanoparticles and the whole nanoparticle. Additionally, HAXPES gives access to deeper core levels at higher energy.
An application of this technique is presented using nanoparticles. The results shown were obtained with nanoparticles, that were treated differently by means of sterilization for nanosafety (i.e., before studying their toxicity it is important to establish whether nanomaterials are sterile and, if not, to be treated either via microwave or autoclave sterilisation). As a complementary method, the data is compared with SEM and EDX measurements. All methods demonstrate the influence of sterilization. More specifically, these results show that the sterilization step must be considered in the physical-chemical description of the particles for establishing reliable (quantitative structure-activity) relationships.
Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination.
Verschlussbauwerke sind für die untertägige Endlagerung im Salzgestein als eine wichtige technische Barriere vorgesehen. Diese Bauwerke müssen hohen Anforderungen an Sicherheit und Integrität genügen, weshalb im Projekt SealWasteSafe Werkstofftechnik, Prüfverfahren und Überwachungsmethoden für sichere Verschlussbauwerke verbessert werden. Dabei zeigen die untersuchten alkaliaktivierten Materialien (AAM) langsamere Reaktionskinetik bei der Erhärtung im Vergleich zu Salzbeton, was potenziell geringere Rissbildung erwarten lässt. Die Erhärtung wird an Probekörpern (100-300 l) multisensorisch über einen Zeitraum von mindestens 28 Tagen überwacht. Die Parameter Temperatur und Feuchtigkeit werden einerseits kabelgebunden, andererseits mittels drahtloser Radio Frequency Identification (RFID)-Technik aufgezeichnet. Zusätzlich kommen Schallemissionsmessungen sowie Dehnungsmessungen mittels verteilter faseroptischer Sensorik (FOS) zum Einsatz. Die Überwachung zeigt verschiedene Charakteristika beim Erhärten der Materialien mit geringerer Temperaturentwicklung des AAM. Zusätzlich werden Ultraschallmessungen genutzt, um Einbauteile und Störstellen wie Risse und Delaminationen im Rahmen der Qualitätssicherung am Probekörper und am Verschlussbauwerk zu detektieren. Dafür werden sowohl ein Ultraschallmesssystem mit großer Apertur (LAUS) als auch eine Ultraschall-Bohrlochsonde eingesetzt. Durch Erhöhung des Schalldrucks und Schallfeldbündelung im Beton wird die Aussagekraft der von der Bohrlochsonde aufgezeichneten Messsignale verbessert, was in Modellierungen und ersten Labortests gezeigt werden kann. Die Auswertung der Ultraschallmessungen zeigt das große Potenzial der Methode mit Eindringtiefen bis zu 9 m, wobei anspruchsvolle Abbildungsverfahren zu einer verbesserten Abbildung der internen Strukturen führen. Insgesamt verbessern die im Projekt SealWasteSafe entwickelten Materialien und Methoden die Möglichkeiten für sichere Verschlussbauwerke nuklearer Endlager. Obwohl die Konzepte speziell für Bauwerke im Salzgestein entwickelt werden, sind sie partiell gut auf andere Wirtsgesteine übertragbar.
In the recent years, more and more products in construction and automotive industry are bonded by adhesive tapes instead of mechanical fasteners but there is no sufficient understanding of how these bonded, layered materials behave in fires. Our research project gives an insight of how adhesives and substrates interact with each other in different fire scenarios and how flame retardants function in pressure sensitive adhesive (PSA) tapes. A systematic investigation on the burning behavior of PSA tapes as free-standing films, as top layers on different substrates and as sandwich-like adhesive joints was performed. The burning behavior of free-standing PSA tapes and those used as a coating was significantly improved by using phosphorus-based flame retardants. Furthermore, it was shown that, depending on tape structure and substrate, the PSA tape can lower the fire risk by acting as an intermediate protection layer in bonded materials.
Surface applied corrosion inhibitors (SACI) are widely used to mitigate corrosion process of steel reinforcement in concrete. But they remain controversial as to their effectiveness and the ability to compare materials from different manufacturers
and technologies. They are applied onto the surface of
hardened concrete and penetrate towards steel reinforcement. This paper discusses the corrosion inhibition performances of
dual-phase surface applied corrosion inhibitor and the efficiency of the corrosion inhibitor is assessed by selected testing procedures in BAM laboratories.