5 Werkstofftechnik
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The creep behavior of single-crystals of the nickel-base superalloy CMSX-4 was investigated at 1288°C, which is the temperature of the hot isostatic pressing (HIP) treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no Gamma’-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g. the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-section area psi of [001] crystals reached nearly 100%, while for a [111] crystal psi=62%. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals didn’t not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. From the shape of deformed specimens and TEM investigations it was concluded that the main strain contribution resulted from <011> {111} octahedral slip.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized.
For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotronand the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates the dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation.
Efficient energy provision using fuel cells requires effective hydrogen storage capacities. Glass is a material of low intrinsic hydrogen permeability and is therefore a promising material for hydrogen storage containers or diffusion barriers. Pioneer work on oxidic glasses seems to indicate a correlation between glass composition and hydrogen permeation, which was mainly derived from the behavior of silica glass. In this study, we focus on the relationship between topologic (free volume; network polymerization) and thermodynamic (configurational entropy) glass parameters. Experiments were performed well below the glass transition temperature, which excludes significant structural relaxation and chemical dissolution of hydrogen. The compositional dependence of seven glasses on the SiO2-NaAlO2 join pointed out that in fully polymerized glasses the H2 permeability cannot be solely derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen diffusion and solubility. Additionally, results indicate that hydrogen permeability of the glasses is affected by the configurational heat capacity ΔCp at Tg.
Effective hydrogen storage capacities are prerequisite for an efficient energy provision using fuel cells. Since glass has low intrinsic hydrogen permeability, it is a promising material for hydrogen storage containers as well as hydrogen diffusion barriers. Previous studies on oxidic glasses suggest a correlation between the glass composition and hydrogen permeation that was derived mainly from silica glass. In the present study, we concentrate on the relationship between thermodynamic (i.e., configurational entropy) and topologic (i.e., free volume, network polymerization) parameters. Experimental data were gathered well below the glass transition temperature, excluding significant effects caused by structural relaxation and chemical dissolution of hydrogen. The results of seven analysed glasses on the SiO2-NaAlO2 joint showed that the hydrogen permeability in fully polymerized glasses cannot solely be derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen solubility and diffusion. Additionally, the results indicate that the configurational heat capacity ΔCp at Tg affects the hydrogen permeability of the investigated glasses.
PE-HD as a polymeric fuel storage tank material: Photooxidation, fuel sorption and long-term storage
(2018)
High-density polyethylene (PE-HD) is a commodity thermoplastic polymer which is typically used for packing of dangerous goods. Its good resistance against photooxidation, fuels, chemicals and other environmental factors in addition to low production costs makes PE-HD attractive for fuel storage applications. Typical engine fuels stored in polymer tanks are petrol, diesel and biodiesel that receives increasing attention as proper alternative to fossil fuels. One of the major problems with biodiesel is its susceptibility to oxidize due to its chemical composition of unsaturated fatty acids which also can cause polymer degradation.
The aim of this study is to investigate the influence of different environmental factors, UV radiation and commonly stored fuels, on the mechanical, physical and chemical properties of two types of PE-HD polymers (stabilized and non-stabilized). The influence on the mechanical properties was tested by Charpy and tensile tests, chemical and physical properties were evaluated by Fourier-transform infrared spectroscopy (FTIR) and by dynamical mechanical analysis (DMA) tests. Samples were characterized after varying exposure time of UV radiation and after fully and partially immersion in biodiesel. In addition, similar experiments were conducted using diesel for comparison.
The first documentation of fuel biodeterioration dates back to the late 19th century. However, extensive studies concerning the microbial fuel contamination started in 1980’s. Polymeric fuel storage tanks containing diesel and biodiesel provide environmental conditions for microbial growth. Several studies demonstrated that bacteria, which were found in contaminated fuel systems, can use fuels as macronutrient; but such bacteria can also cause microbiologically influenced corrosion and fouling.
The aim of this study is to investigate the initial attachment behavior of bacteria, isolated from a diesel contamination, on neat and photooxidized high-density polyethylene (PE-HD). Two common PE-HD’s, less- and biodiesel-stabilized, were radiated to UV light representing a tank exposed to sunlight. The effect of photooxidiation on PE-HD’s surface were characterized chemically by Fourier-transform infrared spectroscopy (FTIR). The attached bacteria Pseudomonas aeruginosa and Bacillus subtilis on the polymer surface were evaluated by fluorescence microscopy and colony-forming unit tests (CFU).
Glass-fibre-reinforced plastics (GFRP) are commonly used for the construction of pressure vessels and tanks for example in automotive and aerospace industries. Especially for pressure vessels used for the storage of natural gas or hydrogen with operation pressures up to 700 bar, an early material fatigue detection is of great interest. Measuring the distributed strain profile of GFRP structures helps to understand and detect material fatigue. In this article, we demonstrate the great potential of swept wavelength interferometry (SWI) based distributed strain sensing for the monitoring of pressure vessels made from GFRP. A resin transfer molding (RTM) process was used to manufacture GFRP-tube specimens. Commercial optical fibres with polyimid coating were glued to the surface externally in circumferential and axial direction. A cyclic load of up to 150 bar was applied to the samples using a servo-hydraulic test bench. Comparing the loaded and unloaded test conditions, we determined up to 2 % elongation in circumferential direction. We demonstrate reliable distributed strain measurements with sub-centimetre spatial resolution. By monitoring these high-resolution strain profiles, we were able to detect local material degradation that manifested itself as localized strain changes. Crucially, the material Degradation could be detected already after 75 % of dat the fatigue life before a crack appeared that led to leakage.
Lock-in- and flash thermography are standard methods in active thermography. They are widely used in industrial inspection tasks e.g. for the detection of delaminations, cracks or pores. The requirements for the light sources of these two methods are substantially different. While lock-in thermography requires sources that can be easily and above all fast modulated, the use of flash thermography requires sources that release a very high optical energy in the very short time.
By introducing high-power vertical cavity surface emitting lasers (VCSELs) arrays to the field of thermography a source is now available that covers these two areas. VCSEL arrays combine the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination range of flash lamps or LEDs and can thus potentially replace all conventional light sources of thermography.
However, the main advantage of this laser technology lies in the independent control of individual array areas. It is therefore possible to heat not only in terms of time, but also in terms of space. This new degree of freedom allows the development of new NDT methods. We demonstrate this approach using a test problem that can only be solved to a limited extent in active thermography, namely the detection of very thin, hidden defects in metallic materials that are aligned vertically to the surface. For this purpose, we generate destructively interfering thermal wave fields, which make it possible to detect defects within the range of the thermal wave field high sensitivity. This is done without pre-treatment of the surface and without using a reference area to depths beyond the usual thermographic rule of thumb.
In Germany spent nuclear fuel and high level radioactive waste is stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. The used metal seals consist of three components as can be seen in the cross-sectional view in Figure 1. The innermost part is a helical spring that is surrounded by an inner jacket made of stainless steel. The outer jacket that is made of a softer material which in case of assembly in the aforementioned storage containers is silver or aluminum (i.e. Al 99.5). During application the seal is compressed and due to the restoring force of the helical spring, the outer jacket is plastically deformed and adapts to the sealing surface. Hence, leakage paths are closed and the sealing function is generated. In Germany the above-mentioned containers are licensed for up to 40 years of interim storage, which in case extended storage becomes necessary before a final repository is available will have to be extended to even longer periods. Therefore, the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads as well.
At Bundesanstalt für Materialforschung und –prüfung (BAM) long-term investigations are being conducted in which seals are assembled in test flanges and aged at temperatures ranging from room temperature to 150°C for accelerated aging. The aged seals are tested semi-annually (after the first 6 months in which the seals are tested more frequently) regarding the sealing performance, the remaining seal force, and the useable resilience upon decompression. Results of these investigations have been published over the past years (e.g. Grelle, Wolff, Probst, Jaunich, & Völzke, 2017; Völzke, Wolff, Probst, Nagelschmidt, & Schulz, 2014). It was found that the seal force and the useable resilience decrease with time and temperature, which is in agreement with the result of other studies (Sassoulas et al., 2006; Wataru et al., 2016) as well. Geometry change of the outer jacket has been identified as the main reason for this seal behavior. At the prevailing operating temperatures and stresses the aluminum is subjected to creep deformation leading to a thinning of the outer jacket. Since the seal groove depth remains unchanged the helical spring expands, which in turn leads to a decrease of the generated spring and seal force.
Although the main reason for the change of seal parameters over time and temperature is known, a detailed characterization of the seal behavior and a reliable prediction of the parameter development for aging times that exceed the experimental time frame have not been possible, yet.
For deeper understanding of the aging processes, an Investigation program, which is covered in this contribution, is conducted at Bundesanstalt für Materialforschung und –prüfung (BAM) that focusses on the behavior of the aluminum jacket and its influence on the long-term sealing performance. The program investigates properties of material samples as well as the behavior of the seal as a component.
Original sheet material of the same aluminum that is used for manufacturing of the seals is investigated in compression creep tests. For this, a DMA (dynamic mechanical analysis) machine is employed (here used for static tests) that allows for a measurement of the specimens deformation under forces of up to 500 N. The advantage of this method is that the original material can be tested in the same shape as used for the seals which is 0.5 mm thick sheet material. For investigation of tensile creep standard specimens are used, that were machined from surrogate material of the same composition and annealing condition.
Furthermore, aluminum seals that are cut into smaller segments are assembled in flanges and placed in heating chambers at temperatures ranging from 23°C to 150°C. After different periods of time from 3 days to 300 days the segments are taken out of the flanges and are investigated, thus giving information on different states of aging. Measurements of the development of the seal contact width and the aluminum jacket thickness are done with an optical microscope. Further investigations on the segments will include metallography and hardness measurements.
From the detailed material and component behavior including the results of the long-term seal force and useable resilience investigations a better understanding of the overall seal behavior can be gained. The aim is to contribute to the development of material models and analytical approaches for the prediction of the sealing behavior in dependence of time and temperature.