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View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation
(2019)
It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts.
First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized.
Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures.
Subsequently, different examples will be shown how these limitations in some cases could be outsmarted.
First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied.
Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS.
All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra.
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved.
Spray drying based granulation processes aim for flowable granules neither containing voids nor hard shells thus leading to a homogenous microstructure in the green and sinter bodies without strength reducing large pores. The increase of the specific surface area due to the utilization of finer powders as raw materials makes the production of granules of demanded quality more sophisticated. Innovations regarding additives as well as process engineering are therefore required.
While conventional spray granulation processes of ceramic materials are based on rotational, one stream or two stream nozzles for nebulization, the investigations in the ZIM project concentrate on the applicability of an ultra sound atomizer unit. A spray dryer comprised of the aforementioned ultra sound atomization unit implemented in a commercial spray dryer (Niro, Denmark) was used as test system. Potential advantages of the ultra sound nebulization are investigated for model systems of alumina, zirconia and a ZTA composite while focusing on solids content, yield, pressability and granule properties (size, size distribution, flowability, shape and microstructure) as well as the final sinter body properties (density, microstructure and flexural strength).
First ultra sound spray drying experiments yielded granules with excellent processability. Spray drying of identical slurries, as before tested and optimized for a two stream nozzle atomization process, resulted in a more suitable size distribution for dry pressing (less particles below 20 µm) and a higher yield. Furthermore, sinter bodies produced of ultra sound granules seem to have less large pores and a more homogenous microstructure
Synthetic microswimmers mimicking biological movements at the microscale have been developed in recent years. Actuating helical magnetic materials with a homogeneous rotating magnetic field is one of the most widespread techniques for propulsion at the microscale, partly because the actuation strategy revolves around a simple linear relationship between the actuating field frequency and the propeller velocity.
However, full control of the swimmers’ motion has remained a challenge. Increasing the controllability of micropropellers is crucial to achieve complex actuation schemes that, in turn, are directly relevant for numerous applications. However, the simplicity of the linear relationship limits the possibilities and flexibilities of swarm control. Using a pool of randomly shaped magnetic microswimmers, we show that the complexity of shape can advantageously be translated into enhanced control. In particular, directional reversal of sorted micropropellers is controlled by the frequency of the actuating field. This directionality change is linked to the balance between magnetic and hydrodynamic forces. We further show an example of how this behavior can experimentally lead to simple and effective sorting of individual swimmers from a group. The ability of these propellers to reverse swimming direction solely by frequency increases the control possibilities and is an example for propeller designs, where the complexity needed for many applications is embedded directly in the propeller geometry rather than external factors such as actuation sequences.
This work investigates the effect of the tribotesting parameters (temperature, atmosphere, and third body chemical composition) on the coefficient of friction (CoF) during pin-on-disc dry (PoD) sliding tribotests using artificial third bodies. The third body comprised nanometric Fe3O4-based binary to quaternary chemical compositions containing copper, graphite, and zirconia. These mixtures were manually or ball-milled prepared, and pin-on-disc tribotests were conducted at 23 °C and 400 °C under air or nitrogen atmospheres. Combining PoD and artificial third body to create synthetic tribofilms might be useful for testing new formulations of Cu-free friction materials. Microstructural characterisation of the tribofilms was used to study the stability of the Fe3O4, copper, and graphite nanoparticles under different testing conditions to understand their effects on the CoF. For the Fe3O4-C-ZrO2-X systems, the ball milling mixing promoted the formation of turbostratic graphite in the tribofilm, impairing the lubricating effect of the graphite under air atmosphere at 23 °C. The formation of monoclinic CuO in the tribofilms during tribotests at 400 °C under air and N2 atmospheres promoted a lubricating effect.
Trapping in T24 steel weld joints – Effects on activation energy for hydrogen diffusion during TDA
(2017)
Failure cases in the past decade exhibited severe cracking in T24 welds and showed that generally hydrogen-assisted cracking (HAC) occurring up to 200°C cannot be excluded. A basic understanding is necessary on how hydrogen diffusion is influenced by the weld process. In this regard, both weld microstructures HAZ and weld metal have particular influence on hydrogen diffusion compared to the base material. In general, hydrogen diffusion at a certain temperature is described by diffusion coefficients representing an effective value of combined lattice diffusion and effects of reversible hydrogen traps. Those traps are typically precipitates, interstitials, grain boundaries and so on. A common approach to describe the trap character and its effect on diffusion is the determination of so-called activation energy. This can be done by respective thermal desorption analysis (TDA) with linear heating. In the present study, different T24 as-welded microstructures (BM, HAZ, WM) were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by TDA with linear heating using a mass spectrometer for detection of ultra-low hydrogen amounts. The results showed that typically the as-welded HAZ had higher energy traps than the tempered base material. Nonetheless two important effects were ascertained: (1) it is strictly necessary to monitor the sample temperature due to its great impact on the hydrogen desorption peak temperature and (2) the real heating rate in the specimen vs. the applied heating rate has to be considered. Both influence the calculated activation energy, i.e. the assigned hydrogen trap character (moderate or strong trap), which changed up to a factor of two in terms of the calculated activation energy. This effect can be much more important compared to the microstructure effect itself. Hence, suitable experimental boundary conditions should be mandatory for the determination of hydrogen trap kinetics.
The present work describes the shear creep behavior of the superalloy LEK 94 at temperatures between 980 and 1050 °C and shear stresses between 50 and 140 MPa for loading on the macroscopic crystallographic shear system (MCSS) (011)[01-1]. The strain rate versus strain curves show short primary and extended secondary creep regimes. We find an apparent activation energy for creep of Qapp = 466 kJ/mol and a Norton-law stress exponent of n = 6. With scanning transmission electron microscopy, we characterize three material states that differ in temperature, applied stress, and accumulated strain/time. Rafting develops perpendicular to the maximum principal stress direction, gamma channels fill with dislocations, superdislocations cut gamma' particles, and dislocation networks form at gamma/gamma' interfaces. Our findings are in agreement with previous results for high-temperature and low-stress [001] and [110] tensile creep testing, and for shear creep testing of the superalloys CMSX-4 and CMSX-6 on the MCSSs (111)[01-1] and (001)[100]. The parameters that characterize the evolving gamma/gamma' microstructure and the evolving dislocation substructures depend on creep temperature, stress, strain, and time.
The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs.
Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels.