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Organisationseinheit der BAM
- 6 Materialchemie (203)
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- 4 Material und Umwelt (36)
Eingeladener Vortrag
- nein (1)
Regelwerke zur zerstörungsfreien Bestimmung des Reinheitsgrades wie das SEP 1927 und die ASTM E588 erreichen ihre Vergleichbarkeit unter Anwendung von - vergleichsweise einfachen - Referenzfehlern. Hinsichtlich Realisierbarkeit wird somit der Kompromiss zwischen Herstellung des Referenzfehlers und der erreichbaren Nachweisgrenze gefunden.
Zur Weiterentwicklung über die Grenzen der SEP1927 hinaus, wurde der Versuch unternommen Fehler kleiner 500 μm herzustellen - welche aufgrund der geringen geometrischen Ausdehnung fertigungsbedingt schwierig zu realisieren sind. Bei den vergleichenden Untersuchungen kristallisierten sich zwei Fertigungsverfahren, Funkenerosion (EDM: electrical discharge maching) und die Fertigung der Bohrungen unter Verwendung eines Hochleistungslasers, als vielversprechend heraus. Zunächst wurden die Fehler mit beiden Verfahren in unterschiedlichen Größen (100, 250 und 100 μm) und Tiefen (1, 1,5 und 2 mm) unter Anwendung von computertomographischen Verfahren der Röntgenprüfung, die Geometrie der eingebrachten Fehlstellen und anschließend durch hochauflösende Tauchtechnikmessungen das Reflektionsverhalten charakterisiert.
Time- and space-resolved in situ LIBS measurements of chemical compositions during TIG-welding
(2017)
An in situ monitoring of chemical compositions in the weld pool and the heat affected zone (HAZ) can enable the control of the welding process through the regulation of the welding parameters, and thus can prevent possible weld defects.
The most critical parameter for hot cracking -from a metallurgical point of view- is the chemical composition of the weld pool.
Chemical composition can be measured and quantified during the welding process with the LIBS technique having the appropriate calibration measurements.
Fluorescence microscopic and spectroscopic monitoring of degradation processes upon polymer ageing
(2017)
The majority of all routinely used methods to assess polymer aging are based on destructive tests and methods. Early indicators for the deterioration of polymer materials are e.g., physical or mechanical properties like tensile strength, adhesion, brittleness, and color. It is well-known, however, that predominantly chemical changes are the underlying process of the physical changes that occur in organic materials upon aging over time. Typical initial steps during polymer degradation are crosslinking or chain breaking, alteration of autofluorescence, “yellowing” or bleaching caused by the formation of new functional groups. A straightforward strategy towards the sensitive detection and monitoring of chemical changes in the course of polymer aging is based on non-destructive optical measurements. Luminescence techniques, one of the most sensitive spectroscopic methods are the method of choice. Here, we present first results of luminescence-based monitoring of polymer degradation induced by different environmentally relevant weathering factors (e.g. humidity and UV exposure). Our studies include fluorescence spectroscopy as well as spectral scanning confocal fluorescence microscopy and clearly demonstrate the possibility to follow accelerate-aging processes by luminescence detection.
Metallic springs undergo oxidation and creep at elevated temperatures and their use is limited to temperature of about 650°C. Therefore, there is a need for stable materials which can easily withstand temperatures up to 1000°C for long periods in different atmospheres. Ceramic materials have been drawing attention due to their excellent properties. This work aimed at investigating the high-temperature stability of zirconia and alumina ceramic springs at elevated temperatures under different atmospheres (air, N2 and H2) in order to determine the limitation of use of these ceramic springs.
The synthesis of hybrid inorganic/organic copolymers, using reversible deactivation radical polymerization (RDRP) techniques, has been an intensively studied research topic over recent years. A plethora of hybrid inorganic/organic copolymers were synthesized, including hybrid inorganic/organic block copolymers as well as random copolymers,[1–4] that showed great potential in fabricating hybrid (nano)materials with tailored properties [5]. Two widely employed RDRP techniques to prepare such hybrid inorganic/organic copolymers are atom transfer radical polymerization (ATRP) [1,2] and reversible addition-fragmentation chain transfer (RAFT) polymerization [3,4]. In order, to afford hybrid inorganic/organic copolymers with narrow dispersity, high conversions and precise structures, it is required to choose proper reaction conditions. Due to the importance of both ATRP and RAFT in the preparation of such hybrid polymers, we aim to compare both RDRP techniques by preparing 2-acetoxyethyl methacrylate (AcEMA) and 3-(triethoxysilyl)propyl methacrylate (TESPMA) based homopolymers. For this purpose, AcEMA and TESPMA were polymerized in 1,4-dioxane at 60 °C mediated by CuBr/N,N,N',N'-pentamethyldiethylenetriamine (PMDETA) and 2-(2-carboxylethylsulfanylthiocarbonyl-sufanyl) propionic acid (TTC) as well as cumyl dithiobenzoate (CDB) to evaluate the suitability and reliability of ATRP and RAFT to prepare such hybrid (co)polymers.
Polyurethanes (PU) are formed by polyaddition reaction between diols and diisocyantes. They can be formed utilizing three building blocks, namely a polyol or long-chain diol, a chain extender or short-chain diol, and a diisocyanate. The derived multi-phase block copolymer has thermoplastic properties and is called thermoplastic PU (TPU). This modular approach allows for a variety of alternations yielding a broad range of structural properties and applications. TPUs are based on three main classes of polyols, i.e. polyethers, polyesters, and polycaprolactones. With these different polyols and the ability of changing the ratio of building blocks a variety of material properties can be obtained thus TPUs find numerous applications in e.g. lightweight construction1, insulation, flame retardants, lacquer and glue, as well as medicine.
Linear, isocyanate terminated, polyurethane prepolymers prepared from non-equivalent amounts of diisocyanate such as methylene diphenyl diisocyanate (MDI) attached to a polyol are widely used as precursors of the correspondent polymers. Chain-extending reactions with low molecular weight compounds bearing different amounts of active hydrogens enable both linear and crosslinked polyurethane to be formed.
Due to TPUs being used in a broad range of applications facing a variety of stress (e.g. mechanical, hydrolytic, thermal, radiative/UV, as well as its combinations) the complexity of possible degradation mechanism is high. A functional group derived from degradation of the bulk matrix can be detected utilizing a suited fluorogenic sensor molecule. There are several fluorogenic dyes known for the application as sensor for amine groups e.g. fluorescamine, pyrylium dyes, deriving a fluorescent signal upon reaction.
One of today’s major problems in many technical plants as well as fuel tanks is Microbial induced corrosion (MIC), leading to considerable damage and huge financial losses. Successful prevention of MIC requires the localization of first signs of corrosion as well as the identification of factors influencing the corrosion process. Hence, there is a growing need for sensitive and preferably inexpensive tools that enable the early detection of MIC. Of utmost importance are methods, which provide spatially and time-resolved information and allow the determination of corrosion rates at sites of interest for possible prevention of MIC.
Experimental study on M23C6 nucleation and growth mechanisms in Ni-base superalloy single crystals
(2017)
The addition of carbon to Ni-base superalloy single crystals has been increasingly carried out to improve low angle grain boundary (LAGB) resistance and castability. Consequently, the precipitation of carbides is highly probable during long-term application of components subjected to higher temperatures (> 1000 °C). While the view on the role of carbides as strengthening or detrimental is polemical, their inevitable increased presence in carbon-doped alloys must be addressed. In the present work, the evolution of M23C6 carbides forming in the commercial grade Ni-base superalloy LEK 94 during high-temperature and low-stress creep exposure is assessed. Although carbon is not intentionally added to the LEK 94 alloy, it admits up to 0.1 at. %, which together with the high content of M23C6-forming transition metals, leads to their precipitation. The precipitation is induced here during creep experiments at 1020 °C and a nominal applied stress of 160 MPa along [001]. The correlation of precipitation and external load is carried out by evaluating the carbides in the gage section of parallel and circularly notched cylindrical samples, as well as in their heads. Characterization is made by transmission electron microscopy (TEM). Although primary MC carbides form mostly in interdendritic regions during casting, high temperature exposure induces M23C6 carbide nucleation especially in the γ phase of dendritic regions, where a stronger partitioning of refractory elements is present. The carbides have a needle shape with their main axis on 〈100〉 and a cube-on-cube orientation relationship. They present incoherent {100} facets along their elongated region and semi-coherent {111} facets at their ends. Their nucleation and growth mechanisms are discussed based on microstructural observation under different experimental conditions.
Zur Vermeidung der schädigenden Alkali-Kieselsäure-Reaktion in Betonbauwerken wird die Alkalireaktivität von Gesteinskörnungen im Vorhinein getestet. Der 60°C-Betonversuch ermöglicht eine vergleichsweise schnelle Einschätzung nach fünf-monatiger Testzeit. Dazu wird die Dehnung von Betonprüfkörpern, die mit der zu testenden Gesteinskörnung hergestellt wurden, manuell alle 28 Tage gemessen. Ein alternatives, an der BAM in den vergangen Jahren entwickeltes Verfahren setzt Dehnungssensoren ein, um kontinuierlich und online zu messen. Die Dehnungskurven sind eine gute Grundlage sowohl für die Prognose vom Expansionsverhalten während des Tests als auch für die Validierung von Expansionsmodellen.
The interest in porous anodic aluminum oxide (AAO) has been rapidly growing due to its numerous applications in separation, catalysis, energy generation and storage, electronics, and sensors. From the scientific point of view, AAO is a topical interest in soft matter fields. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamics, and mobility. Embedding polymers and liquid crystals into nanopores of AAO results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. On the other hand, discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with pore diameter of 10, 20, 25, 40, 80, 120 and 180 nm. The filling degree for each sample was checked by thermogravimetric analysis (TGA) in order to ensure complete filling. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the plastic crystalline-to-hexagonal columnar phase transition in two, which might be interpret as two different phase structures; close to the wall and at the pore center. Moreover, the isotropic-to-columnar transition of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC.
Upconversion nanoparticles are characterized by their ability to convert low energy near-infrared excitation in high energy emissions in the visible range. This is enabled by sequential absorption of two or more photons via energy transfer from the sensitizer lanthanide ion Yb3+ to an activator lanthanide ion, e.g. Er3+. Yb3+ sensitation has the advantage of 980 nm excitation achieved by commercial available low power cw laser modules.
Nevertheless, for some applications, especially in aqueous media, which is predominantely in bioanalytical applications, there is the drawback of a local Absorption maximum of water at this wavelength. Sample heating can occur, and excitation power density is strongly distance dependent.
To overcome this issue, the idea is to shift the excitation wavelength to 808 nm. This can be achieved by a tandem-excitation using Nd3+ and Yb3+ ions. Nd3+ gets excited by 808 nm irradiation and transfers the energy to Yb3+, which triggers the upconversion emission of the Er3+ ions. Therefore, it is mandatory to separate Nd3+ and Er3+ by core-shell architecture for reducing the energy backtransfer from Er3+ to Nd3+.
To further enhance the upconversion luminescence an additional inert shell formed by the host material NaYF4 reduces the quenching effects caused by surface defects and dangling bonds.
By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis Approach (evaporation induced self assembly).
Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases.
While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the Independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies.
Chemical admixtures like superplasticizers or stabilizing agents are of ever increasing importance for modern concrete technology. Although such admixtures have meanwhile become common practice in many applications of concrete technology, the understanding of these highly complex systems is still limited and the relevant parameters, which predominantly control the interaction between the superplasticizer and the cement components, have not been identified yet.
Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules. This encouraged us to assess the potential of these methods, and particularly reflectance and fluorescence measurements, for the study of the interactions that occur at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation. Special emphasis is dedicated to search for and identify differences between commonly used superplasticizers.
Here, we focus on hydration effects using commercial comb shape polycarboxylate ethers (PCEs) with different charge densities, which are known to allow a very low water/cement ratio (w/c of 0.20 or less) while maintaining good workability. Based upon changes of the intensity of the reflectance and fluorescence signal and spectral effects of a dye, acting as optical reporter, a model for the interactions of dye, PCE molecules and cement nanoparticles in the very first phase of cement hydration is derived
The results are based on data1. Figure 3 displays temperatures of the tank wall and of the gas phase over testing time. It can be seen that a complete coating strongly delayed the heating of tank wall and gas phase, whereas the partly coated tanks only had a minor influence on temperature development. There was no significant difference between a half coated and a thirdly coated tank measurable. Figure 4 shows the internal pressure of tanks over testing time. Only the fully coated tank enabled a low pressure over 90 min testing time. Hence, a complete coating is necessary to guarantee the fire safety of hazmat tanks and a partly coating is not sufficient.
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
Additive manufacturing (3D printing) of ceramics and other materials offers significant advantages compared to conventional production processes for several applications. While ceramics have been extensively investigated in this regard, additive manufacturing of geopolymers have received much less attention to date. In the present contribution we study a ‘standard’ metakaolin-based geopolymer, a fly ash-based geopolymer and a silica-based one-part geopolymer regarding their suitability for additive manufacturing via selective laser curing. Model geometries such as bars and cuboids could be produced by this route. After selective laser curing the specimens were additionally cured at 80 °C for 24 h. The specimens were studied by means of scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). SEM showed that the precursors in all geopolymers had reacted partially and geopolymeric gel had formed. XRD confirmed these results and additionally revealed that the crystalline byproducts (zeolites) in the one-part geopolymer differed from the byproducts observed in conventionally produced samples. This indicates that also the geopolymerization reactions differ between the two synthesis routes. The mechanical strength after selective laser curing and 80 °C-curing appeared to be highest for the metakaolin-based geopolymer. However, SEM also showed that a significant volume of macropores remained in most regions of all specimens, while some regions in the metakaolin-based geopolymer appeared to be significantly denser. These preliminary results demonstrate that selective laser curing offers potential for the production of geopolymers, but more research has to be undertaken to optimize the process.
Einfluss des Schwefelgehalts auf die Korrosionsbeständigkeit des nichtrostenden Stahls 1.4404
(2016)
Die Korrosionsbeständigkeit nichtrostender Stähle wird maßgeblich von ihrer chemischen Zusammensetzung bestimmt. Der tendenzielle Einfluss ist für die Hauptlegierungselemente in der wissenschaftlichen Fachliteratur beschrieben. Bei Begleitelement Schwefel gibt es dagegen keine konkreten Untersuchungen die belegen, ab welchem Gehalt mit einer Verringerung der Korrosionsbeständigkeit zu rechnen ist. Im Lichtbogenschmelzofen wurden verschiedene Legierungen mit abgestuftem Schwefelgehalten hergestellt, um den Einfluss dieses Begleitelementes auf die Korrosionsbeständigkeit systematisch zu untersuchen. Die KorroPad-Prüfung und die Bestimmung kritischer Lochkorrosionspotentiale wurden zur Charakterisierung der Legierungen genutzt. Beide Methoden belegen eine zunehmende Verringerung der Lochkorrosionsbeständigkeit mit dem Schwefelgehalt.
Die Korrosionsbeständigkeit geschweißter Konstruktionen aus nichtrostenden Duplexstählen wird von den Schweißparametern und der Nachbehandlung der Oberflächen bestimmt. Eine etablierte Methode der Schweißnahtnachbehandlung ist das Strahlen der Oberfläche mit Glasperlen. Diese Methode soll aus wirtschaftlichen Gründen durch das Strahlen mit Korund ersetzt werden, welches deutliche Zeit- und Kostenvorteile bietet. Besonders bei der Lochkorrosionsbeständigkeit hat sich das Schleifen mit Korund bereits als nachteilig erwiesen, weshalb diese Umstellung auch beim Stahlen kritisch hinterfragt wird. Daher wurden Probeschweißungen bei der Firma Modersohn hergestellt und mit verschiedenen Oberflächenbearbeitungsmethoden (Glasperlenstrahlen, Korundstrahlen, Beizen, Elektropolieren, Schleifen) nachbehandelt. Diese verschiedenen Oberflächenzustände wurden analytisch (REM, Rauheit) charakterisiert und hinsichtlich ihrer Lochkorrosionsbeständigkeit vergleichend untersucht werden, um die Eignung des Strahlens mit Korund zu beurteilen.