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The control of stress development in cast ceramics during drying is usually one of critical steps in ceramic processes, which is important also for additive manufacturing technologies using a suspension as feedstock. This work introduces a method based on the cantilever deflection method, to simultaneously quantify the kinetics of solvent evaporation, the shrinkage and the intensity of in-plane stresses developed during drying. Particular attention is given here to the experimental limits of the method and to the optimization of the experimental conditions to suitably measure the intensity of in-planar stress in the coating. The optimized method is applied to
four alumina slurries for the water-based additive manufacturing technology LSD-print. Four stages of drying are identified and discussed in relation with the granulometry and morphology of the alumina ceramic particles.
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 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.
An interlaboratory study, involving eigth international laboratories and coordinated by COMTES FHT (Czech Republic), was conducted to validate tensile measurements obtained using miniature specimens on additively manufactured (AM) components and artifacts. In addition to AM 316L stainless steel (316L SS), a wrought highstrength steel (34CrNiMo6V, equivalent to AISI 4340) was also used. Based on the results, a precision statement in accordance with ASTM E691 standard practice was developed, intended for inclusion in a proposed annex to the ASTM E8/E8M tension testing method. The primary outcomes of the study highlighted the agreement between yield and tensile strength measured from miniature and standard-sized tensile specimens. Furthermore, most tensile properties exhibited similar standard deviations, offering users insight into the efficacy of miniature specimen applications.
Advancements in bulk metallic glass thermoplastic forming unleash the potential to fabricate microscale metallic features with unparalleled precision and durability, i.e. microspine gripping structures for mobility platforms on planetary or in-space robots. Four designs of grippers were fabricated and rigorously tested. Coefficient of friction on four test surfaces were measured and compared to SiC paper and Velcro. The hardness and elasticity of the bulk metallic glasses make them a game-changer in the field, offering a superior alternative to conventional nonmetallic grippers.
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
Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables.
AbstractTwo‐photon polymerization (2PP) additive manufacturing (AM) utilizes feedstocks of ceramic nanoparticles of a few nanometers in diameter, enabling the fabrication of highly accurate technical ceramic design with structural details as small as 500 nm. The performance of these materials is expected to differ from conventional AM ceramics, as nanoparticles and three‐dimensional printing at high resolution introduce new microstructural aspects. This study applies 2PP‐AM of yttria‐stabilized zirconia to investigate the mechanical response behavior under compressive load, probing the influence of smallest structural units induced by the line packing during the printing process, design of sintered microblocks, and sintering temperature and thereby microstructure. We find a dissipative mechanical response enhanced by sintering at lower temperatures than conventional. The pursued 2PP‐AM approach yields a microstructured material with an increased number of grain boundaries that proposedly play a major role in facilitating energy dissipation within the here printed ceramic material. This microplastic response is further triggered by the filigree structures induced by hollow line packing at the order of the critical defect size of ceramics. Together, these unique aspects made accessible by the 2PP‐AM approach contribute to a heterogeneous nano‐ and microstructure, and hint toward opportunities for tailoring the mechanical response in future ceramic applications.
Compared to mechanisms like solid solution strengthening, the stacking fault energy (SFE) should be considered as a further factor that influences the material properties. The effect of SFE of alloys or individual elements on strength and resistance can vary considerably. In the high-temperature regime above 700 ◦C, there are still significant gaps in the knowledge about the effect of the SFE on the mechanical properties of single-phase alloys. The effect of SFE on creep resistance of two face-entered cubic equiatomic medium and high entropy alloys, CrCoNi and CrMnFeCoNi, respectively, is evaluated to fill parts of these gaps. Using the Bridgman solidification process, the alloys were produced as single crystals and crept under vacuum at 700 ◦C up to 1100 ◦C. This work shows a significant impact of the lower SFE of CrCoNi on the creep behavior compared to the results of previous investigations of CrMnFeCoNi. The creep resistance of the former is higher over the complete temperature range. At very high temperatures, the strengthening effect of the stacking faults is significantly present. The formation of tetragonal stacking faults and extended dislocation nodes can be identified as the reason for this effect.
Modern dry pressing of ceramic powders using spray‐dried granulates cannot avoid the occurrence of defects related to persisting inter‐ and intra‐granulate interstitial voids. These constitute the parent defect size population limiting the application of polycrystalline ceramics in high‐stress conditions. The mitigation of such defects could widen the range of application in technical and biomedical engineering, reduce the safety range for design, and extend the lifetime of components. Herein, the Weibull size‐effect on strength in size‐partitioned Yttria‐stabilized zirconias (YSZ) feedstocks is used to explore the viability of changing the density distribution of granulate sizes as an effective strategy to obtain a denser particle packing that could reduce the size distribution of strength‐limiting pressing defects. In a direct assessment of critical defect size using multiscale strength testing with a dataset of ≈1300 values, the success of such an approach in increasing the strength reliability for small volume components is demonstrated, along with its ultimate failure in altering the defect size distribution in sintered YSZ ceramics across several length scales. Finally, it is shown that granule morphology (spherical or dimpled) fails to affect the defect density and size distribution in YSZ ceramics.
The digitalization of materials science and engineering (MSE) is currently leading to remarkable advancements in materials research, design, and optimization, fueled by computer‐driven simulations, artificial intelligence, and machine learning. While these developments promise to accelerate materials innovation, challenges in quality assurance, data interoperability, and data management have to be addressed. In response, the adoption of semantic web technologies has emerged as a powerful solution in MSE. Ontologies provide structured and machine‐actionable knowledge representations that enable data integration, harmonization, and improved research collaboration. This study focuses on the tensile test ontology (TTO), which semantically represents the mechanical tensile test method and is developed within the project Plattform MaterialDigital (PMD) in connection with the PMD Core Ontology. Based on ISO 6892‐1, the test standard‐compliant TTO offers a structured vocabulary for tensile test data, ensuring data interoperability, transparency, and reproducibility. By categorizing measurement data and metadata, it facilitates comprehensive data analysis, interpretation, and systematic search in databases. The path from developing an ontology in accordance with an associated test standard, converting selected tensile test data into the interoperable resource description framework format, up to connecting the ontology and data is presented. Such a semantic connection using a data mapping procedure leads to an enhanced ability of querying. The TTO provides a valuable resource for materials researchers and engineers, promoting data and metadata standardization and sharing. Its usage ensures the generation of finable, accessible, interoperable, and reusable data while maintaining both human and machine actionability.
Extended X-ray absorption fine structure (EXAFS) conducted on an equiatomic MoNbTaW bcc medium-entropy alloy that was annealed at 2273 K reveals unexpectedly small 1st and 2nd shell element-specific lattice distortions. An experimental size-mismatch parameter, δexp, is determined to be ca. 50% lower than the corresponding calculated value. Around W, short-range order (SRO) preferring 4d elements in the 1st and 2nd shells persists. A Nb-W ordering is found, which is reminiscent of ordering emerging at lower temperatures in the B2(Mo,W;Ta,Nb)- and B32(Nb,W)-phases. With high-temperature ordering preferences in fcc also foreshadowing low-temperature phase, these findings suggest a general feature of high-temperature SRO.
Processing and cytocompatibility of Cu-doped and undoped fluoride-containing bioactive glasses
(2024)
Sintered or additive-manufactured bioactive glass (BG) scaffolds are highly interesting for bone replacement applications. However, crystallization often limits the high-temperature processability of bioactive glasses (BGs). Thus, the BG composition must combine high bioactivity and processability. In this study, three BGs with nominal molar (%) compositions 54.6SiO2-1.7P2O3-22.1CaO-6.0Na2O-7.9K2O-7.7MgO (13–93), 44.8SiO2-2.5P2O3-36.5CaO-6.6Na2O-6.6K2O-3.0CaF2 (F3) and 44.8SiO2-2.5P2O3-35.5CaO-6.6Na2O-6.6K2O-3.0CaF2-1.0CuO (F3–Cu) were investigated. The dissolution and ion release kinetics were investigated on milled glass powder and crystallized particles (500–600 μm). All glasses showed the precipitation of hydroxyapatite (HAp) crystals after 7 days of immersion in simulated body fluid. No significant differences in ion release from glass and crystalline samples were detected. The influence of surface roughness on cytocompatibility and growth of preosteoblast cells (MC3T3-E1) was investigated on sintered and polished BG pellets. Results showed that sintered BG pellets were cytocompatible, and cells were seen to be well attached and spread on the surface after 5 days of incubation. The results showed an inverse relation of cell viability with the surface roughness of pellets, and cells were seen to attach and spread along the direction of scratches.
AbstractThis study applies Semantic Web technologies to advance Materials Science and Engineering (MSE) through the integration of diverse datasets. Focusing on a 2000 series age-hardenable aluminum alloy, we correlate mechanical and microstructural properties derived from tensile tests and dark-field transmission electron microscopy across varied aging times. An expandable knowledge graph, constructed using the Tensile Test and Precipitate Geometry Ontologies aligned with the PMD Core Ontology, facilitates this integration. This approach adheres to FAIR principles and enables sophisticated analysis via SPARQL queries, revealing correlations consistent with the Orowan mechanism. The study highlights the potential of semantic data integration in MSE, offering a new approach for data-centric research and enhanced analytical capabilities.
This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters.
Die in dieser Studie vorgestellte 3D-Gefüge-Analyse konzentriert sich auf die Kugelgrafite eines Gusseisens des Typs EN-GJS. Es werden die Form anhand des Formfaktors und des Seitenverhältnisses sowie die durchschnittliche Teilchengröße und -verteilung untersucht.
Die Form der Grafite in Gusseisenwerkstoffen ist mitentscheidend für die mechanischen Eigenschaften dieser Legierungen und ist bei der Charakterisierung des Werkstoffs unumgänglich. Mittels Metallografischen Serienschnittverfahrens wird von dem Schicht für Schicht abgetragenen und lichtmikroskopisch schichtweise dargestellten Werkstoff ein digitaler Zwilling erstellt. Von diesem dreidimensionalen Zwilling lassen sich beliebige Ebenen digital projizieren und analysieren. Eine konventionelle quantitative 3D-Analyse untersucht die Voxelmenge und -zusammensetzung eines Körpers im 3D-Raum. Die hier vorgestellte Analyse wendet stereologische 2D-Analyseverfahren auf drei Raumebenen des Werkstoffs an. Dabei sind zwei der Ebenen digitale Projektionen des Zwillings. Die zwei rekonstruierten Ebenen des Werkstoffs sind so gewählt, dass die Richtungsvektoren aller drei Ebenen einen 90°-Winkel zueinander bilden. Diese Methodik wird eingehend beschrieben sowie Herausforderungen und Möglichkeiten des hier vorgestellten Serienschnittverfahrens diskutiert.
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.
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.
Addressing a strategy for publishing open and digital research data, this article presents the approach for streamlining and automating the process of storage and conversion of research data to those of semantically queryable data on the web. As the use case for demonstrating and evaluating the digitalization process, the primary datasets from low‐cycle‐fatigue testing of several copper alloys are prepared. The fatigue test ontology (FTO) and ckan.kupferdigital data management system are developed as two main prerequisites of the data digitalization process. FTO has been modeled according to the content of the fatigue testing standard and by reusing the basic formal ontology, industrial ontology foundry core ontology, and material science and engineering ontology. The ckan.kupferdigital data management system is also constructed in such a way that enables the users to prepare the protocols for mapping the datasets into the knowledge graph and automatically convert all the primary datasets to those machine‐readable data which are represented by the web ontology language. The retrievability of the converted digital data is also evaluated by querying the example competency questions, confirming that ckan.kupferdigital enables publishing open data that can be highly reused in the semantic web.
This data article presents a set of primary, analyzed, and digitalized mechanical testing datasets for nine copper alloys. The mechanical testing methods including the Brinell and Vickers hardness, tensile, stress relaxation, and low-cycle fatigue (LCF) testing were performed according to the DIN/ISO standards. The obtained primary testing data (84 files) mainly contain the raw measured data along with the testing metadata of the processes, materials, and testing machines. Five secondary datasets were also provided for each testing method by collecting the main meta- and measurement data from the primary data and the outputs of data analyses. These datasets give materials scientists beneficial data for comparative material selection analyses by clarifying the wide range of mechanical properties of copper alloys, including Brinell and Vickers hardness, yield and tensile strengths, elongation, reduction of area, relaxed and residual stresses, and LCF fatigue life. Furthermore, both the primary and secondary datasets were digitalized by the approach introduced in the research article entitled “Toward a digital materials mechanical testing lab” [1]. The resulting open-linked data are the machine-processable semantic descriptions of data and their generation processes and can be easily queried by semantic searches to enable advanced data-driven materials research.