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Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene
(2024)
The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements.
Highlights
- Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques
- Determined growth rates depend on distinction between craze zone and crack
- The ratio of the present crack to the anteceding craze zone is validated theoretically
- The transition from crack propagation to ductile shear deformation is identified
- An already formed craze zone may still fail by ductile mechanisms
The present work addresses powder bed binder jetting additive manufacturing by selective magnesium phosphate cement activation. Despite the potential of this technology to aid the digitalization of the construction industry, the effect of processing parameters on the mechanical performance of printed materials has not yet been studied to generate a guideline for the further development of the technology. Statistical methodologies were used to screen the effect of four printing process parameters (printing speed, layer thickness, raster angle, and build direction on flexural and compressive strength). As the exploited technology works with constant fluid pressure, the physical interpretation of the effect of each factor can be considered taking into account the interactions between the binder materials in the powder bed. Analysis of variance (ANOVA) indicated that printing speed and layer thickness significantly affect mechanical performances. Furthermore, the layout of samples for the printing process is preferable to be parallel the printhead movement. An anisotropic behavior was observed, and the samples subjected to compressive forces parallel to the layer plane possessed lower strength values. This effect can be interpreted as a result of a weak area of low density in between layers, leading to a pronounced delamination under compression. Even though the strength of the printed material is not suitable for a structural concrete, it can be marginally improved by design of experiment and optimized for non-structural applications, such as for porous artificial stone. Design of experiment coupled with ANOVA methods can be used in the future to support the development of novel material mixtures, thus expanding the fields of application of this novel additive manufacturing technology.
A widespread recovery of waste heat requires a cost‐effective production of thermoelectric generators. Thermoelectric oxides are predestined for use at high temperatures. For manufacturing reasons, a multilayer generator design will be easily scalable and cost‐effective. To evaluate the potential of ceramic multilayer technology for that purpose, a multilayer of the promising thermoelectric oxides calcium cobaltite (Ca3Co4O9), calcium manganate (CMO, CaMnO3), and glass–ceramic insulation layers is fabricated. Cracks and reaction layers at the interfaces are observed in the microstructure. The compositions of these reaction layers are identified by energy‐dispersive X‐ray spectroscopy and X‐ray diffraction. Mechanical and thermal properties of all layers are compiled from literature or determined by purposeful sample preparation and testing. Based on this data set, the internal stresses in the multilayer after co‐firing are calculated numerically. It is shown that tensile stresses in the range of 50 MPa occur in the CMO layers. The reaction layers have only a minor influence on the level of these residual stresses. Herein, it is proven that the material system is basically suitable for multilayer generator production, but that the co‐firing process and the layer structure must be adapted to improve densification and reduce the tensile stresses in the CMO.
The current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis.
High‐temperature KCl‐induced corrosion of high Cr and Ni alloys investigated by in‐situ diffraction
(2024)
High‐temperature KCl‐induced corrosion in laboratory air was observed in situ utilizing X‐ray diffraction. High Cr‐containing model alloys (Fe‐13Cr, Fe‐18Cr‐12Ni, and Fe‐25Cr‐20Ni) were coated with KCl and exposed to dry air at 560°C. KCl‐free alloys were studied in the equivalent atmosphere as a reference. After exposure to KCl‐free environments, all alloys showed the formation of very thin oxide layers, indicating good corrosion resistance. In contrast, KCl‐bearing alloys showed distinct damage after exposure.
Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering.
Additive manufacturing of metals – and in particular building with laser-based powder bed fusion – is highly flexible and allows high-resolution features and feedstock savings. Meanwhile, though space stations in low Earth orbit are established, a set of visits to the Moon have been performed, and humankind can send out rovers to explore Venus and Mars, none of these milestone missions is equipped with technology to manufacture functional metallic parts or tools in space. In order to advance space exploration to long-term missions beyond low Earth orbit, it will be crucial to develop and employ technology for in-space manufacturing (ISM) and in-situ resource utilisation (ISRU). To use the advantages of laser-based powder bed fusion in these endeavours, the challenge of powder handling in microgravity must be met. Here we present a device capable of building parts using metallic powders in microgravity. This was proven on several sounding rocket flights, on which occasions Zr-based metallic glass parts produced by additive manufacturing in space were built. The findings of this work demonstrate that building parts using powder feedstock, which is more compact to transport into space than wire, is possible in microgravity environments. This thus significantly advances ISRU and ISM and paves the way for future tests in prolonged microgravity settings.
Objectives
The aim of the study was to investigate the impact of organic additives (binder, plasticizer, and the cross-linking ink) in the formulation of water-based feedstocks on the properties of a dental feldspathic glass-ceramic material developed for the slurry-based additive manufacturing technology “LSD-print.”
Material and methods
Three water-based feldspathic feedstocks were produced to study the effects of polyvinyl alcohol (AC1) and poly (sodium 4-styrenesulfonate) (AC2) as binder systems. A feedstock without organic additives was tested as the control group (CG). Disc-shaped (n = 15) and bar (n = 7) specimens were slip-cast and characterized in the green and fired states. In the green state, density and flexural strength were measured. In the fired state, density, shrinkage, flexural strength (FS), Weibull modulus, fracture toughness (KIC), Martens parameters, and microstructure were analyzed. Disc-shaped and bar specimens were also cut from commercially available CAD/CAM blocks and used as a target reference (TR) for the fired state.
Results
In the green state, CG showed the highest bulk density but the lowest FS, while the highest FS in the green state was achieved with the addition of a cross-linking ink. After firing, no significant differences in density and a similar microstructure were observed for all slip-cast groups, indicating that almost complete densification could be achieved. The CAD/CAM specimens showed the highest mean FS, Weibull modulus, and KIC, with significant differences between some of the slip-cast groups.
Significance
These results suggest that the investigated feedstocks are promising candidates for the slurry-based additive manufacturing of restorations meeting the class 1a requirements according to DIN EN ISO 6871:2019–01.
In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF.
In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as ‘‘electron beam-induced fragmentation’’ or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field 𝐵 = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. 𝐵 = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF.