5 Werkstofftechnik
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Eingeladener Vortrag
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Molecular orientation has a significant effect on the material properties of polymers. Preferential orientation of the microstructure (polymer chains or crystallites) in a specific direction or plane often enhances the material properties, especially if the high-strength covalent bonds are primarily exposed to loads instead of the weaker van der Waals bonds. However, the orientation-dependent microstructure and its mechanical behavior is in general already well understood by many scientific studies [1-3]. Isotropic materials are frequently required for an intrinsic material characterization without prevailing processing-induced properties, as is the case for Full Notch Creep Test (FNCT) [4] addressing environmental stress cracking (ESC) in high-density polyethylene (PE-HD) [5, 6]. Since ESC is one of the major limiting issues for long-term performance of PE-HD pipes and containers [7], which in contrast have a production-related preferential orientated microstructure due to extrusion or extrusion blow molding, it is important to additionally investigate the ESC resistance of such anisotropic microstructure.
Investigations of the slow crack growth (SCG) with respect to the molecular orientation generally obtain a factor of 1.2 up to 4.7 between crack growth perpendicular to the extrusion direction and crack growth parallel to the extrusion direction 8. Based on FNCT investigations with an aqueous detergent solution as environmental medium, hot pressed sheets with isotropic morphology are compared with extruded sheets from which specimens with different orientation angles are taken. However, the time to failure obtained by FNCT is also significantly influenced by the different cooling conditions under which the final morphology is formed. The tendency of the specimen to fail due to ESC is investigated as a function of environmental medium temperature. For a more detailed analysis of the affecting parameters in the manufacturing process, the ESC resistance is discussed considering the differences in crystallinity as revealed by thermal analysis.
The development of refractory CCAs has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy, which resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. The aim of this work is to evaluate the alloy’s mechanical behavior under tension in the temperature range 800-1000°C, by applying creep tests under vacuum (excluding oxidation effects). Some little temperature influence on minimum creep rate @ 1000 and 1100 °C was found and at a first glance, and Norton plots shows that deformation is probably both diffusion and dislocation controlled. However, further work is needed to stablish deformation and degradation micro mechanisms in the studied creep regime.
The refractory chemically complex alloy (rCCA) AlMo0.5NbTa0.5TiZr, with a density of 7.4 g/cm3, shows a compressive ultimate strength of 772 MPa at 1000 °C, comparatively surpassing Ni-base and other rCCAs. Its dual-phase microstructure, with a high volume fraction (≈ 62%) of cuboidal and plate-like particles coherently embedded in a continuous matrix, resembles the well-known pattern of the γ/γ" in Ni-base superalloys. Its developers have thus implied that it could stand as structural alloy for high temperature (HT) applications. Here, we report the HT creep properties and the underlying microstructural changes of the rCCA AlMo0.5NbTa0.5TiZr to propose deformation and degradation micromecanisms for this regime. The material was produced by arc-melting and subsequently heat treated in argon: at 1400 °C for 24 h plus a hot isostatic pressure treatment at 1370 °C and 170 MPa for 4 h, with a cooling rate of 10 K/min. Miniaturized tensile specimens (≈ 28 x 7 x 2 mm) were cut and polished to a quality of 1 μm. Creep tests were conducted in vacuum in the respective temperature and stress range 800-1200 °C and 30-120 MPa. For observation, thin slices were extracted from the gauge length, away from the fracture surface, grinded to a thickness of 100 μm, and electropolished to electron transparency. The microstructure was observed on the electropolished specimens using scanning (S) as well as transmission (T) electron microscopy (EM). The Norton plot gives Norton exponents of about 3.1 and 3.2 for temperatures of 1000 and 1100 °C, respectively. Curiously, creep rate minima are very close for a stress level of 30. The starting microstructure reflects a macroscopically lean coarse grain structure and a microscopically fine-meshed basketweave structure with coherency dislocations only around coarsened particles usually close to subgrain boundaries. Results are discussed on the base of variations of this starting microstructure after interrupted and ruptured creep tests.
Thermal cycling of a Ni-excess NiTi alloy was conducted between 50 °C and liquid nitrogen temperature to induce martensitic transformations and to reverse them after. The starting point was an annealed and slowly cooled state, the end point a sample thermally cycled 1500 times. Positron annihilation lifetime spectra and Coincidence Doppler Broadening profiles were obtained in various states and at various tem- peratures. It was found that the initial state was low in defects with positron lifetimes close to that of bulk NiTi. Cycling lead to a continuous build-up of a defect structure up to 20 0 −50 0 cycles after which saturation was reached. Two types of defects created during cycling were identified, namely pure dislo- cations and vacancies attached to dislocations.
The flow behavior of powders has an essential role in many industrial processes, including powder bed additive manufacturing. The characterization of the flow behavior is challenging, as different methods are available, and their suitability for an application in additive manufacturing is still controversial. In this study, six standardized methods (measurement of bulk density by ISO 60 and by ASTM B329, angle of repose by ISO 4324, discharge time by ISO 6186 and by ASTM B964-16, and Hausner Ratio by ASTM 7481 – 18), the rotating drum method (by GranuDrum) and powder rheometry (Anton Paar powder cell), were applied to five size fractions of a crushed quartz sand powder and compared. A statistical approach is proposed and discussed to correlate the obtained flowability indexes with the packing density of powder beds deposited layer-by-layer, and these correlations are compared between methods. Overall, the measurement of bulk density by ASTM B329 that showed the best correlation with the powder bed density. Advanced methods such as the rotating drum method and powder rheometry did not demonstrate particularly good correlations, however they provided complementary information which can be useful to assess the dynamic behavior of powders.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
Reliable characterization of materials at the nanoscale regarding their physio-chemical properties is a challenging task, which is important when utilizing and designing nanoscale materials. Nanoscale materials pose a potential toxicological hazard to the environment and the human body. For this reason, the European Commission amended the REACH Regulation in 2018 to govern the classification of nanomaterials, relying on number-based distribution of the particle size.
Suitable methods exist for the granulometric characterization of monodisperse and ideally shaped nanoparticles. However, the evaluation of commercially available nanoscale powders is problematic. These powders tend to agglomerate, show a wide particle size distribution and are of irregular particle shape.
Zinc oxide, aluminum oxide and cerium oxide with particle sizes less than 100 nm were selected for the studies and different preparation methods were used comparatively.
First, the nanoparticles were dispersed in different dispersants and prepared on TEM-supported copper grids. Furthermore, individual powders were deposited on carbon-based self-adhesive pads. In addition, the samples were embedded by hot mounting and then ground and polished.
The prepared samples were investigated by scanning electron microscopy (including the transmission mode STEM-in-SEM) and Dynamic Light scattering. The software package ImageJ was used to segment the SEM images and obtain the particle sizes and shapes and finally the number-based particles size distribution with size expressed as various descriptors.
The relaxation of macroscopic residual stresses in laser powder bed fused stainless steel 316L
(2021)
The processing of stainless steel 316L using the additive manufacturing process Laser Powder Bed Fusion (LPBF) can widen its field of application due to a strong increase in Yield strength, without making major compromises on the ductility nor its outstanding corrosion and oxidation properties. Furthermore, improved designs that either reduce the weight or optimise the function of a part can be obtained using LPBF. These benefits are however counterbalanced by the proneness of LPBF to inducing high Residual Stresses (RS) during manufacturing. The characterisation and monitoring of these RS are of paramount importance for the wider acceptance of the LPBF process. This study focuses on the relaxation of the initial macroscopic RS present in an LPBF 316L as-built prism that undergoes various routes of manufacturing steps to achieve different specimen geometries and stress relieving treatments. The RS are determined using Angle-Dispersive (AD) and Time-of-Flight (TOF) neutron diffraction. The results reveal high tensile RS close to the surfaces and compressive RS near the centre of the as-built parts. The reduction in size and change of geometry heavily impact the stress ranges of the remaining RS, with lower stress ranges in cylindrical shaped compared to rectangular shaped specimens. Also, the application of different stress relieving heat treatments showed that heat-treating temperatures above 800 °C are necessary to obtain a strong relaxation in LPBF 316L.
Due to its matrix/γ′ structure, the compositionally complex alloy (CCA) Al10Co25Cr8Fe15Ni36Ti6 has excellent properties that fulfill the requirements for a high-temperature material. This base alloy is alloyed with small amounts of high melting elements to a further improvement of its properties, which results in different shapes, fractions and sizes of the two phases γ′ and Heusler after various homogenization and annealing steps. By correlating this microstructure with time independent and dependent mechanical properties, conclusions can be drawn about the effects of the individual phases. The needle-shaped Heusler-phase leads to bad mechanical behavior if its phase fraction is too high. A fraction below 3 vol% is not critical in tensile tests, but it reduces the creep resistance compared to a purely two-phase matrix/γ′-alloy. Sharp-edged cubic γ′-particles and a coarse Heusler-phase without sharp edges in case of the base alloy with 0.5 at.% hafnium lead to the best tensile and creep properties in the high temperature range. At 750 °C, the Hf-containing alloy clearly outperforms two commercially used alloys in the targeted area of application when it comes to creep resistance.
Signal optimization for transmission Kikuchi diffraction (TKD) measurements in the scanning electron microscope is investigated by a comparison of different sample holder designs. An optimized design is presented, which uses a metal shield to efficiently trap the electron beam after transmission through the sample. For comparison, a second holder configuration allows a significant number of the transmitted electrons to scatter back from the surface of the sample holder onto the diffraction camera screen. It is shown that the secondary interaction with the sample holder leads to a significant increase in the background level, as well as to additional noise in the final Kikuchi diffraction signal. The clean TKD signal of the optimized holder design with reduced background scattering makes it possible to use small signal changes in the range of 2% of the camera full dynamic range. As is shown by an analysis of the power spectrum, the signal-to-noise ratio in the processed Kikuchi diffraction patterns is improved by an order of magnitude. As a result, the optimized design allows an increase in pattern signal to noise ratio which may lead to increase in measurement speed and indexing reliability.