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Molecular Mobility of Thin Films of Poly (bisphenol-A carbonate) Capped and with one Free Surface: From Bulk-like Samples down to the Adsorbed Layer
No full textThe molecular mobility of thin films of poly(bisphenol A carbonate) (PBAC) was systematically investigated using broadband dielectric spectroscopy, employing two distinct electrode configurations. First, films were prepared in a capped geometry between aluminum electrodes employing a crossed electrode capacitor (CEC) configuration, down to film thicknesses of 40 nm. The Vogel temperature, derived from the temperature dependence of relaxation rate of the α-relaxation, increases with decreasing film thickness characterized by an onset thickness. The onset thickness depends on the annealing conditions, with less intense annealing yielding a lower onset thickness. Additionally, a broadening of the β-relaxation peak was observed with decreasing thickness, attributed to the interaction of phenyl groups with thermally evaporated aluminum, resulting in a shift of certain relaxation modes to higher temperatures relative to the bulk material. A novel phenomenon, termed the slow Arrhenius process (SAP), was also identified in proximity to the α-relaxation temperature.
For films with thicknesses below 40 nm, nanostructured electrodes (NSE) were utilized, incorporating nanostructured silica spacers to establish a free surface with air. This free surface causes an enhancement in the molecular mobility for the 40 nm sample, preserving the β-relaxation as a distinct peak. The α-relaxation was detectable in the dielectric loss down to 18 nm, shifting to higher temperatures as film thickness is decreased. Notably, the onset thickness for the increase in Vogel temperature was lower in the NSE configuration compared to the CEC setup, attributed to the presence of the polymer-air interface
Elucidating hierarchical microstructures in high entropy superalloys: An integrated multiscale study
No full textIn this study, we examine a high entropy superalloy (HESA-Y1: Ni49.37Co20Cr7Fe4Al11.6Ti6Re1Mo0.5W0.5Hf0.03 at%), focusing on hierarchical microstructure formation and its effects on mechanical properties. Thermodynamic modeling using Thermo-Calc predicts equilibrium phase fractions, compositions, and transition temperatures,which are validated by experimental data from differential scanning calorimetry (DSC). Transmission electronmicroscopy (TEM) reveals that secondary aging induces nanometer-sized γ particles within γ’ precipitates, forming a hierarchical γ/γ’ microstructure. Atom probe tomography (APT) confirms supersaturation of γ’ precipitates with γ-forming elements (Co, Cr, Fe), driving γ particle formation, and measures interfacial widths between γ’ and γ phases. Partitioning coefficients derived from APT align with Thermo-Calc predictions for most elements. Vickers microhardness testing shows an increase of about 50 HV in the hierarchical microstructure compared to the conventional one. In situ synchrotron X-ray diffraction (XRD) from 25 to 750 ◦C determines a small, negative lattice misfit δ between γ and γ’ phases, suggesting enhanced microstructural stability, consistent with Thermo-Calc calculations. Our methodological approach enables measurement of the unconstrained lattice parameter of phase-extracted γ’ in a single-crystal XRD setup. Due to their small size and low volume fraction, γ particles do not produce distinct reflections in the X-ray diffractogram. Elucidating hierarchical microstructures across multiple scales, we establish that the presence of Re and Hf and controlled aging processes lead to enhanced mechanical properties, offering valuable insights for the design of advanced high entropy superalloys
Effect of fiber surface state on the thermomechanical and interfacial properties of in situ polymerized polyamide 6/basalt fiber composites
No full textThis study investigates the thermomechanical properties and interfacial adhesion of novel in-situ polymerized anionic polyamide 6 (aPA6) composites reinforced with basalt fibers (BF). The impact of different BF surface states - as-received (BFa), ethanol-washed (BFw), and thermally desized (BFu) on composite performance is examined through a comprehensive approach. For the first time, anionic PA6/BF composites with very low residual monomer content were successfully produced via thermoplastic resin transfer molding (tRTM). The PA6/BFw composites exhibited the highest interlaminar/interfacial shear strength in short beam shear test (52 ±8 MPa) and fiber push out test (34 ± 11 MPa) tests. Fiber microdebonding test, performed only on PA6/BFw, yielded a low interfacial shear strength (12 ± 4 MPa), which was attributed to droplet porosity resulting from concurrent polymerization and crystallization. Thermal desizing significantly deteriorated interfacial strength (19.6 ± 1.2 MPa in short beam shear test). This multi-technique characterization provides insights into optimizing the fiber–matrix adhesion in these advanced thermoplastic composites
On-line monitoring of polyhydroxyalkanoate extraction by low-field nuclear magnetic resonance spectroscopy
No full textThe use of low-field nuclear magnetic resonance (NMR) spectroscopy enables real-time reaction monitoring in contrast to time-consuming gas chromatography or off-line high-field NMR measurements. In this study, NMR spectroscopy is demonstrated as a novel process analytical technology (PAT) tool in the downstream processing of polyhydroxyalkanoate (PHA) biopolymers. On-line NMR spectroscopy measurements were performed using a Spinsolve 43 Carbon Ultra instrument in a fully automated mode with a flow-assembly based on PTFE tubing. Single-scan NMR spectra were acquired for real-time monitoring of the extraction process of the PHA copolymer poly(hydroxybutyrate-co-hydroxyhexanoate) with 13.5 mol.% hydroxyhexanoate [P(HB-co-13.5 mol.%HHx)] from Ralstonia eutropha biomass using chloroform or acetone as PHA solvents at lyophilized cell loadings of 20–120 g L 1. The reproducibility and reliability of low-field NMR spectroscopy was comparable to high-field NMR spectroscopy, with superior performance in terms of time. The correlation between the results of on-line monitoring using low-field NMR spectroscopy and off-line analysis using gas chromatography (GC) showed a correlation coefficient of >94 %. The versatility of low-field NMR spectroscopy for elucidating reaction kinetics, facilitating endpoint determination and accelerating extraction processes by maximizing solubility is highlighted as plateau values were reached within 6–10 min for chloroform and acetone, respectively. This novel low-field NMR spectroscopy application promotes a new monitoring approach for downstream PHA processing and supports process development and optimization
Investigation of resistance to gaseous hydrogen of a longitudinal weld seam in a X65 pipeline using the hollow specimen technique
No full textThe constantly increasing demand for renewable energy sources leads to the necessity of transporting large amounts of hydrogen. Since pipelines enable a cost-effective way for the distribution of gaseous hydrogen, the interaction of hydrogen and the pipeline materials must be carefully investigated as hydrogen can cause a degradation of the mechanical properties under certain conditions. Especially welds, which are assumed to be more susceptible to the degradation enhanced by hydrogen, are of great interest. The aim of this study is to investigate the effect of gaseous hydrogen on the mechanical properties of an X65 pipeline, and the longitudinal submerged arc welding (SAW) welded joint. The tests are conducted using the hollow specimen technique on two types of specimens: one extracted from the base material (BM) and the other extracted as a cross-weld (CW) specimen consisting of BM and weld seam. The specimens are charged in situ under a pressure of 60 bar and tested using slow strain rate (SSR) tensile tests with a nominal strain rate of 10−5 s−1. The properties obtained of specimens tested in hydrogen atmosphere are compared to the properties of comparable specimen in inert argon atmosphere as a reference. The performed tests showed a decrease of the reduction of area (RA) from 72% in inert atmosphere to 52% in hydrogen atmosphere for the CW specimen and a decrease from 73% in inert atmosphere to 51% for the BM. Metallographic analyses showed the crack initiation between fine-grained heat-affected zone (FGHAZ) and BM for the specimens tested in hydrogen atmosphere as well as for the reference specimens. This leads to the conclusion that the location of the crack initiation does not change due to the presence of gaseous hydrogen
Modal and Wave Propagation Analysis of Vibration Tests on a Laboratory Building Model Before and After Damage
No full textWeakened structural stiffness is often a consequence of building damage, particularly after severe events such as earthquakes, where compromised structural performance can pose significant risks. To prevent immediate structural failure, an early warning system is essential, which requires inspection of local components. This research aims to achieve that by exploring the wave propagation analysis method, specifically seismic interferometry. Previous studies have applied this method to building structures, treating them as homogeneous layers of grouped floors. By analyzing the wave travel time along the height of these layers, the fundamental period of the building was estimated. However, this approach did not account for local damage or the variability of structural components, similar to the limitations of vibration‐based damage detection methods, which mainly identify global changes. Thus, the goal of this paper is to improve structural health monitoring by examining the sensitivity of wave screening, bridging the gap between nondestructive testing and vibration‐based damage detection. A half‐scale, seven‐story building model, characterized by vertical stiffness irregularity and transverse plan asymmetry, was tested in a laboratory setting. Two vertical sensor arrays were placed near corner columns of different sizes, representing both strong and weak structural areas. These arrays recorded floor accelerations in three directions. The study confirmed the effectiveness of wave propagation analysis for detecting damage along the sensor arrays before and after the earthquake. A transmissibility damage indicator was used to correlate changes in wave velocity, providing a quantitative assessment of damage levels along the wave propagation path
Eine Machbarkeitsstudie zur Skalierung von Sprengversuchen an Stahlbetonbauteilen
No full textSprengversuche sind erforderlich, um Explosionsereignisse auf Grund von Unfällen oder Anschlägen zu untersuchen und um das Schutzniveau für Menschen und Anlagen in kritischen Infrastrukturen zu bewerten. Die Durchführung von Feldversuchen in großem Maßstab für komplexe Szenarien ist sehr ressourcenintensiv. Verlässliche Experimente im kleinen Maßstab sind eine vielversprechende Alternative. Die Skalierungsgesetze für die Bemessung von Stahlbetonkonstruktionen unter Explosionsbelastung sind jedoch nicht hinreichend etabliert.
Die Forschungsarbeit fokussiert sich auf Stahlbetonstrukturen, die für die Standardisierung von skalierten Sprengversuchen in Frage kommen. Im Rahmen der Machbarkeitsstudie wurden auf dem TTS-Gelände Sprengversuche an Probekörpern unterschiedlicher Größe durchgeführt. Dabei wurden verschiedene horizontal gelagerte Stahlbetonplatten getestet und unterschiedlichen Explosionsbelastungen ausgesetzt. Die Sprengversuche umfassten verschiedene Messtechniken zur Quantifizierung der Explosionslast sowie des Verhaltens der Stahlbetonplatten. Die Explosionslast wurde mit bündig eingebauten piezoelektrischen Druckmessern gemessen, während Beschleunigungssensoren und flächig applizierte verteilte faseroptische Sensorik verwendet wurden, um das dynamische Verhalten der Platte unter Explosionsbelastung zu charakterisieren. Darüber hinaus wurden Schädigungsmerkmale ebenfalls mit verteilter faseroptischer Sensorik ermittelt. Die Anwendung solcher Messtechniken sowie die Nutzung verschiedener numerischer Softwaretools bieten die Möglichkeit die Skalierungsgesetze zu verifizieren bzw. anzupassen
Turbulence effect on the determination of powders safety characteristics — A review on the experimental findings and simulation approaches
No full textSafety characteristics are widely used in the process industry to design facilities in a safe way. For powders, they are normally investigated under turbulent conditions inside a spherical test vessel, the so called 20L-sphere, to disperse the dust in air. This has been the target of many researchers to either investigate the turbulence that is present during the standardized test conditions, to compare it to quiescent conditions or to manipulate it for the comparison to other conditions. The approaches have been numerous and while the focus used to be on obtaining different experimental results it has shifted more and more to different kinds of simulations. This review gives an overview about different simulation approaches and how they can be compared. It is also an overview over the experimental findings and compares it to data obtained for three different dusts while changing the pre-ignition turbulence level in a very fine way
Challenges of SEC and the necessity of round robin tests
No full textSize exclusion chromatography (SEC) is still the method of choice for determining the molar mass and molar mass distribution of macromolecules. It is a liquid chromatographic technique that separates molecules based on their size, respectively their hydrodynamic volume using a porous stationary phase that allows smaller molecules to pass through the pores while excluding larger molecules. The chromatogram from the size separation can be calibrated using polymers of known molar mass resulting in a relative molar mass distribution curve. From this distribution curve molar mass averages and the oligomer content (percentage of peak area smaller than 1000 g/mol and 500 g/mol) of polymers can be derived.
The determination of oligomer content is important, because it is often used in regulatory contexts as a measure of small, mobile and potentially more toxic parts of the polymer. Polymer regulations are of increasing political and societal importance. Regulations often strive for narrow limits. But SEC has rather large error margins of 10-20% for the molar mass determination performed in different laboratories or on different instruments. These variances are well known to all experts and users and have been investigated in several round robin tests in the past. These resulted in DIN and ISO standards which, in our opinion, no longer meet today's requirements. Gaps have been identified that require further harmonization. Different polymer types or classes require different methods.
On the other hand, as far as we know, the margins of error in determining oligomer content have not yet been investigated. It is expected that the variation will be rather high. This is because it depends on many factors related to the experimental conditions (column sets used, solvent, temperatures, sample preparation) on the one hand, and the data evaluation mechanisms (choice of baseline and peak limits) on the other. In order to actually measure the error margins and to support this with actual data a round robin test has been performed from June to November 2024 with approx. 40 participating laboratories. Three different solvents were selected, namely THF, DMAc or DMF and water. The samples were selected taking into account a wide range of practical aspects far from narrowly distributed standards: e.g higher distribution range, reduced solubility, included side components, copolymers and dispersions with gel content.
In this contribution we will present the detailed concept of this round robin test and first impressions
Master Curve-Auswertungen und fraktographische Analysen zum Bruchmechanismus – neue Ergebnisse zur Untersuchung des Master Curve Konzepts für ferritisches Gusseisen mit Kugelgraphit bei dynamischer Beanspruchung (Projekt MCGUSS)
No full textIn diesem Beitrag werden erste Master Curve (MC)-Auswertungen und fraktographische Analysen zum Bruchmechanismus aus dem laufenden Kooperationsprojekt MCGUSS zwischen der BAM Berlin und der MPA Stuttgart diskutiert. Für zwei SE(B)140-Großprobenversuchsserien mit je 6-8 Versuchen bei -40 °C bzw. -60 °C und Belastungsraten von 5-8x10^4 MPa√m/s wurden Referenztemperaturen T0 bestimmt. Ergänzt wird dies für erste Versuchsreihen an SE(B)25-Kleinproben, die bei -60 °C und Belastungsraten von ca. 2x10^5 MPa√m/s geprüft wurden. An ausgewählten Bruchflächen dieser Versuche wurden detaillierte fraktographische REM-Analysen vorgenommen. Im Vordergrund stand die Charakterisierung des Bruchmechanismus in Abhängigkeit von den Einflussfaktoren Temperatur und Probengröße. In Richtung der Zähigkeitstieflage werden die Analysen komplettiert durch die Ergebnisse von zwei SE(B)140-Großprobenversuchen bei -100 °C bzw. -140 °C und Belastungsraten von ca. 5-8x10^4 MPa√m/s