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The performance of adhesively joined hybrid components relies strongly on the stability of the adhesive-material interface. With the increasing utilization of multi-material structures in the automotive and aerospace industry, it is of great scientific and technical interest to understand the processes leading to adhesive failure and to develop novel strategies to increase corrosion and delamination resistance of adhesive joints.
The aim of this study is to develop thin epoxy based films and their carbon nanofiller loaded composites on aluminium alloy AA2024-T3 and to investigate their interfacial stability under corrosive and coupled corrosive-mechanical load. Spin coating was used for the layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Carbon nanofillers are introduced either by mixing into the coating components or in between individual layers. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) analysis was performed to investigate the porosity and water uptake of the model films, respectively. Atomic force microscopy (AFM) results indicated a very homogeneous and dense film with low surface roughness. The bi-layer thickness ranged between 30 to 40 nm. Electrochemical measurements show a higher corrosion resistance with the increase of the bi-layer number.
The main novelty of this contribution is the in-situ AFM investigations under coupled corrosive-mechanical load. For this purpose, a tensile module capable of uniaxial stretching and compression with up to 5 kN force was integrated into the AFM stage. Stretching experiments were performed to investigate the mechanical properties and adhesion of the films, as well as structural changes of the film morphology during uniaxial deformation. The contribution will provide detailed information on the new AFM setup and summarize our results on the stability of model epoxy and nanocomposite films on AA2024-T3.
Wintzheimer, S. ; Szczerba, Wojciech ; de Oliveira Guilherme Buzanich, Ana ; Kashiwaya, S. ; Klein, A. ; Jaegermann, W. ; Toupance, T. ; Shmeliov, A. ; Nicolosi, V. ; Heuzé, K. ; Mandel, K. ; Dembski, S.
The photocatalytic (PC) performance of titanium dioxide (TiO2) nanoparticles strongly depends on their specific surface, the presence of crystal defects, their crystal phase, and the exposed crystal facets. In order to understand which of these factors contributes most significantly to the PC activity of TiO2 colloids, all of them have to be individually analyzed. This study entails the synthesis of five anatase nanocrystal samples. By maintaining the same reactant ratios as well as hydrothermal sol–gel synthesis route and only varying the autoclaving time or temperature, different crystallite sizes are obtained under comparable experimental conditions. A decrease in PC performance with increase in specific surface area is found. Such an unexpected counterintuitive result establishes the basis for a better understanding of the crucial factors that ultimately determine the PC activity. These are investigated by studying nanocrystals bulk and surface structure and morphology using a selection of complementary analysis methods (X-ray photoelectron spectroscopy (XPS), X-ray absorption fine structure (XAFS), X-ray diffraction (XRD)…). It is found that a change in the nanocrystal morphology from an equilibrium state truncated tetragonal bipyramid to a more elongated rod-like structure accompanied by an increase in oxygen vacancies is responsible for an augmented PC activity of the TiO2 nanocrystals.
A novel stationary phase for affinity separations is presented. This material is based on sintered borosilicate glass readily available as semi-finished filter plates with defined porosity and surface area. The material shows fast binding kinetics and excellent long-term stability under real application conditions due to lacking macropores and high mechanical rigidity. The glass surface can be easily modified with standard organosilane chemistry to immobilize selective binders or other molecules used for biointeraction. In this paper, the manufacturing of the columns and their respective column holders by 3D printing is shown in detail. The model system protein A/IgG was chosen as an example to examine the properties of such monolithic columns under realistic application conditions. Several specifications, such as (dynamic) IgG capacity, pressure stability, long-term performance, productivity, non-specific binding, and peak shape, are presented. It could be shown that due to the very high separation speed, 250 mg antibody per hour and column can be collected, which surpasses the productivity of most standard columns of the same size. The total IgG capacity of the shown columns is around 4 mg (5.5 mg/mL), which is sufficient for most tasks in research laboratories. The cycle time of an IgG separation can be less than 1 min. Due to the glass material’s excellent pressure resistance, these columns are compatible with standard HPLC systems. This is usually not the case with standard affinity columns, limited to manual use or application in low-pressure systems. The use of a standard HPLC system also improves the ability for automation, which enables the purification of hundreds of cell supernatants in one day. The sharp peak shape of the elution leads to an enrichment effect, which might increase the concentration of IgG by a factor of 3. The final concentration of IgG can be around 7.5 mg/mL without the need for an additional nano-filtration step. The purity of the IgG was > 95% in one step and nearly 99% with a second polishing run.
The syntheses and crystal structures of two cerium(IV) phosphonates are presented. Cerium(IV) bis(phenylphosphonate) Ce(O3PC6H5)2 1 can be formed from precipitation and mechanochemical reaction, whereas cerium(IV) bis(carboxymethylphosphonate) monohydrate Ce(O3PCH2COOH)2 H2O 2 is only accessible via ball milling. All reactions proceed very fast and are completed within a short time span. In situ measurements for the syntheses of 1 show that the product occurs within seconds or a few minutes, respectively. The structures were solved from powder X-ray diffraction data.
AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small.
Microplastic reference material is required for validation and harmonization purposes. This includes the analysis of the pure polymer particles and the validation of the respective measurement methods. In addition, there is the harmonization of different laboratories. On the other hand, sample preparation methods must be validated and harmonized with regard to their recovery and subsequent analysis in the respective matrices. For this purpose, we produce reference material candidates in the form of tablets with different mass fractions and particle numbers of polyethelene terephthalate. In the presentation first measurement results by µ-Raman, µ-FTIR, pyrolysis-GC-MS and TED-GC/MS will be presented.
Im der Präsentation werden, neben der Möglichkeit der Mikroplastikquantifizierung, auf weitere Anwendungsfelder der Methode TED-GC/MS eigegangen. Dies beinhaltet die Erfassung von Degradationsprodukten UV/O2 geschädigter Polymere und die Detektion von Additiven. Die Optimierung der Methode betreffend Messzeit und materialspezifischer Messanforderung sind ebenfalls Gegenstand.
Wetzel, Annica ; von der Au, Marcus ; Dietrich, P. M. ; Radnik, Jörg ; Özcan Sandikcioglu, Özlem ; Witt, Julia
This work presents the determination of the corrosion characteristics of CrCoNi (medium entropy alloy) and CrMnFeCoNi (high entropy alloy) in 0.1 M NaCl and 0.1 M H2SO4. The morphology and chemical composition of the oxide layers formed on CrCoNi and CrMnFeCoNi were comparatively analyzed by scanning Kelvin probe microscopy (SKPFM) and scanning electron microscopy (SEM) and supported with chemical analysis by means of inductively coupled plasma mass spectrometry (ICP-MS) and X-Ray photoelectron spectroscopy (XPS). The analysis of the 3p core level peaks showed that the oxide layer (native and after anodic passivation) on CrCoNi consisted mainly of Cr oxides, while the oxide layer on CrMnFeCoNi was primarily composed of a mixture of Cr and Fe oxides. In addition, XPS was utilized to assess the oxide layer thicknesses. These results were compared to the thicknesses obtained by means of electrochemical impedance spectroscopy (EIS), with both approaches yielding values up to about 4 nm depending on the electrolyte and the alloy. Cyclic polarization measurements indicated superior corrosion resistance of CrCoNi in both aqueous environments compared to CrMnFeCoNi, as well as to AISI 304 stainless steel.
Wetzel, Annica ; Morell, Daniel ; von der Au, Marcus ; Wittstock, Gunther ; Ozcan, Ozlem ; Witt, Julia
Multi-principal element alloys (MPEAs) are gaining interest in corrosion and electrocatalysis research due to their electrochemical stability across a broad pH range and the design flexibility they offer. Using the equimolar CrCoNi alloy, we observe significant metal dissolution in a corrosive electrolyte (0.1 M NaCl, pH 2) concurrently with the oxygen evolution reaction (OER) in the transpassive region despite the absence of hysteresis in polarization curves or other obvious corrosion indicators. We present a characterization scheme to delineate the contribution of OER and alloy dissolution, using scanning electrochemical microscopy (SECM) for OER-onset detection, and quantitative chemical analysis with inductively coupled-mass spectrometry (ICP-MS) and ultraviolet visible light (UV-Vis) spectroscopy to elucidate metal dissolution processes. In-situ electrochemical atomic force microscopy (EC-AFM) revealed that the transpassive metal dissolution on CrCoNi is dominated by intergranular corrosion. These results have significant implications for the stability of MPEAs in corrosion systems, emphasizing the necessity of analytically determining metal ions released from MPEA electrodes into the electrolyte when evaluating Faradaic efficiencies of OER catalysts. The release of transition metal ions not only reduces the Faradaic efficiency of electrolyzers but may also cause poisoning and degradation of membranes in electrochemical reactors.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize some of our results on the mechanistical aspects of the observed high corrosion resistance.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in two different electrolyte systems (NaCl and H2SO4 c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively. To analyze the semiconducting properties of the passive film Mott-Schottky analysis was conducted.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX, ICP-MS and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of Chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of Chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
Due to their favorable mechanical and anti-corrosion properties, medium entropy alloys (MEA) are of high academic and industrial interest as novel materials for engineering and catalytic applications. Previous studies on general corrosion behavior indicate high current densities at high anodic potentials for MEAs. Further investigations of the underlying transpassive dissolution and local corrosion behavior remain scarce.
To understand the passivation behavior of MEAs CrCoNi and FeCrNi at high anodic potentials, the mechanisms of transpassive dissolution and the oxygen evolution reaction were investigated in this project. Scanning electrochemical microscopy (SECM) was applied in the interrogative mode for the detection of evolving metal species and oxygen. By means of ICP-MS analysis, dissolved metal species were quantified to provide a fundamental understanding on the transpassive dissolution. As the oxygen evolution reaction (OER) may contribute a large percentile to the observed current at high anodic potentials, SECM measurements were employed to analyze the onset of the OER. Potentiodynamic, potentiostatic and chronoamperometric techniques as well as different electrolytes were used to induce precisely controlled corrosion loads during the SECM experiments and for the ICP-MS analysis. Macroscopic corrosion properties of the alloys, electrical and chemical properties of the passive films were studied by means of potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and X-Ray Photoelectron Spectroscopy (XPS), respectively.
Finally, the analysis of the corrosion morphology and the potential of the surface before, during and after passivity breakdown was carried out by means of in-situ atomic force microscopy (AFM) and scanning Kelvin probe force microscopy (SKPFM). The presentation will summarize our results on the interplay of anodic passivation and oxygen evolution of MEAs in aqueous NaCl electrolytes.
Old materials, new life: Using diffusion-controlled synthesis for discovery of novel alloy systems
(2023)
Multi principal element alloy (MPEAs) concept allows us to rethink how we develop application-tailored, sustainable materials. The vast composition space leads to nearly indefinite material combinations and will facilitate finding Pareto optimal materials with lower CO2 footprint and avoidance of critical minerals as design criteria. To probe this large compositional space efficiently, the use high-throughput screening methods is inevitable. Diffusion-controlled synthesis of gradient materials is the optimal technique for screening complex compositional materials that would otherwise require comprehensive modelling or experimental efforts.
In this study, we have used a series of diffusion couples of pure metals and alloys with the aim to create a materials library with correlated data on composition and microstructure. With future recycling prospects in mind, and possible applications of Cu containing alloys in electrocatalytic carbon dioxide reduction and antimicrobial alloys we have generated diffusion couples of brass (Cu63Zn37) and bronze (Cu89Sn11) with either pure metals (Fe, Ni, etc.) or with binary or ternary alloys (FeNi, FeNiCr etc.). For different diffusion times and temperatures, we calculated diffusion constants for the material combinations. Following a detailed characterisation of the gradient materials, we have investigated general and local corrosion properties, electrocatalytic activity for oxygen evolution reaction (OER) and carbon dioxide reduction reaction (CRR) as well as mechanical properties (hardness, elastic modulus) on single-phase alloys synthesized in bulk by means of vacuum arc-melting based on the selected local compositions.
In most cases, due to the short diffusion times, the contact between the diffusion couples lead to two separate diffusion zones and thus, different alloy families on both sides. Especially with ternary alloys, interesting selective diffusion processes and unexpected repulsion effects were observed. The presentation will provide an overview of the gradient materials with a focus on the functional properties of single-phase alloy families derived from them.
3D coherence scanning interferometry (CSI) is anoptical, non-contact and rapide measurement technique using a defined bandwidth of white light at normal incidence. White light interference microscopy (WLIM) providest here-dimensional surface topometry data up to a resolution of 0.4 µm lateral and 0.1 nm vertical. Three operating modi, surface, films and advanced films, enable measurements of step heights, roughness, wear volume, cone angle, surface pattern and layer thickness. Traceability to SI system is ensured by certified standards (PTB/NIST) within a DAkkS DIN EN ISO/IEC 17025:2018 accredited lab.
Weigert, Florian ; Müller, A. ; Häusler, I. ; Geißler, Daniel ; Skroblin, D. ; Unger, Wolfgang ; Radnik, Jörg ; Resch-Genger, Ute
Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties.
L-lactide (LA) was polymerized in toluene by means of neat tin(II) 2-ethylhexanoate (SnOct2). Concentration, time and temperature were varied. The isothermally crystallized polyLAs (PLA) were characterized in the virgin state with regard to topology, molar mass, melting temperature (Tm), crystal modification, high or low Tm morphology, crystallinity and crystal thickness. Even a small amount of solvent favored cyclization relative to polymerization in bulk, so that cyclic polylactides were obtained at 115 ◦C and even at 95 ◦C. At all temperatures the α-modification of PLA was obtained along with crystallinities up to 90%. With 6 M solution the high Tm morphology with Tm’s > 190 ◦C was obtained at 115 ◦C. The crystal thickness of crystallites grown from solution at 115 ◦C was on the average 10–20% higher than that of PLA polymerized in bulk. At a polymerization temperature of 75 ◦C cyclization was incomplete and fewer perfect crystallites were formed. A new hypothesis for the crystal growth of cyclic polyLAs is proposed.