Search Results (9)

Ion diffusion, the precipitation of hydration products, and interactions between different reactive particles are critical for optimizing the design of low-carbon cementitious systems. However, at the sub-micron scale, the complex spatial and chemical interactions among diverse components at an early age remain challenging to quantify. In this study, a machine learning-assisted BSE-EDS analytical method was applied to quantify both the phase assemblage and the spatial element features of cement–fly ash–slag ternary systems. The equidistant strip delineation of single-particle and rectangular inter-particle path methods were employed to quantify ionic diffusion gradients in the ternary systems. Single-particle strip analysis quantified the hydration front of clinker, slag and fly ash, while inter-particle analysis identified a persistent calcium-starvation zone at slag–fly ash interfaces. This region is characterized by exceptionally high Si/Ca ratios and a lower average atomic number and material density due to ionic diffusion limitations. These findings identify the slag–fly ash interface as the primary microstructural weak link, providing a robust methodology for capturing the chemical heterogeneities and optimizing the design of sustainable cementitious materials. Full article

This study systematically investigates the influence of grain refinement on the microstructural evolution and mechanical properties of recycled Al-7Si-0.3Mg-1Fe alloy through the addition of varying concentrations (0–1.25 wt.%) of Al-5Ti-2B master alloy. The synergistic effects of Al-5Ti-2B on the α-Al phase, eutectic Si, and Fe-rich intermetallics were characterized using metallographic analysis, XRD, SEM-BSE imaging, and EDS. In the unrefined alloy, the microstructure consisted of an α-Al solid solution with coarse plate-like eutectic Si, while Fe primarily formed needle-like β-Al₅FeSi phases that either surrounded or penetrated the eutectic Si. Increasing the Al-5Ti-2B addition refined both the α-Al dendrites and eutectic Si, while the β-Al₅FeSi phase transitioned from coarse to fine needles. The optimal refinement was achieved at a 1% Al-5Ti-2B addition, yielding a tensile strength of 149.4 MPa and elongation of 4.3%. However, excessive addition (1.25%) led to eutectic Si aggregation and β-Al₅FeSi coarsening, resulting in mechanical property deterioration and brittle fracture behavior. These findings provide insights into optimizing grain refinement for enhancing the performance of recycled Al-Si-Mg-Fe alloys. Full article

This study delved into exploring microstructural states in a Ti–7Ag alloy to achieve targeted functional and structural properties. Specifically, the focus was on attaining a homogeneously precipitated state and a solid solution, known for their potential to combine functional traits like corrosion resistance and antibacterial activity with structural properties such as mechanical strength. However, obtaining these optimized microstructures presents challenges due to kinetic considerations. A key finding of this study was the crucial role of a pre-deformation stage, prior to heat treatment, to create an even distribution of fine Ti₂Ag precipitates. Moreover, we demonstrated that starting from this precipitated state, a controlled dissolution step could yield a single-phase solid solution with similar grain size. Therefore, a tailored set of thermomechanical treatments was developed to achieve both microstructures, and these metallurgical states were fully characterized combining SEM (BSE imaging and EDS analysis), TEM, and XRD. Associated mechanical properties were also assessed by tensile testing. In addition, the process was proven to be robust enough to overcome potential industrial problems, such as slow cooling rates when water-quenching large ingots. Considering the limited existing documentation on microstructural features in Ti–Ag alloys, this work on this model alloy significantly advanced our current understanding of the broader Ti–Ag alloy system by providing new data and showcasing a tailored approach involving thermomechanical treatments. Full article

There are several influencing factors in the preparation of MK (metakaolin)-GGBS (ground granulated blast furnace slag)-based geopolymer repair mortars, including the MK-GGBS ratio, the alkalinity of the alkali activator solution, the modulus of the alkali activator solution, and the water-to-solid ratio. There are interactions between these factors, such as the different alkaline and modulus requirements of MK and GGBS, the interaction between the alkaline and modulus of the alkali activator solution, and the influence of water throughout the process. The effect of these interactions on the geopolymer repair mortar is not fully understood, making optimization of the MK-GGBS repair mortar ratio difficult. Therefore, in this paper, the response surface methodology (RSM) was used to optimize the preparation of the repair mortar, with GGBS content, SiO₂/Na₂O molar ratio, Na₂O/binder ratio, and water/binder ratio as influencing factors and 1 d compressive strength, 1 d flexural strength, and 1 d bond strength as evaluation indices. Additionally, the repair mortar’s overall performance was assessed in terms of setting time, long-term compressive and bond strength, shrinkage, water absorption, and efflorescence. The results show that RSM was successful in establishing a relationship between the repair mortar’s properties and the factors. The recommended values of the GGBS content, Na₂O/binder ratio, SiO₂/Na₂O molar ratio, and water/binder ratio are 60%, 10.1%, 1.19, and 0.41, respectively. The optimized mortar meets the standard’s requirements for set time, water absorption, shrinkage values, and mechanical strength, with minimal visual efflorescence. The back-scattered electron (BSE) images and energy dispersive spectroscopy (EDS) analysis show that the geopolymer and cement have good interfacial adhesion, and a denser interfacial transition zone exists in the optimized proportion. Full article

Air plasma spray technique (APS) is widely used in the biomedical industry for the development of HA-based biocoatings. The present study focuses on the influence of powder homogenization treatment by high-energy ball milling (HEBM) in developing a novel hydroxyapatite-barium titanate (HA/BT) composite coating deposited by APS; in order to compare the impact of the milling process, powders were homogenized by mechanical stirring homogenization (MSH) too. For the two-homogenization process, three weight percent ratios were studied; 10%, 30%, and 50% w/w of BT in the HA matrix. The phase and crystallite size were analyzed by X-ray diffraction patterns (XRD); the BT-phase distribution in the coating was analyzed by backscattered electron image (BSE) with a scanning electron microscope (SEM); the energy-dispersive X-ray spectroscopy (EDS) analysis was used to determinate the Ca/P molar ratio of the coatings, the degree of adhesion (bonding strength) of coatings was determinate by pull-out test according to ASTM C633, and finally the nanomechanical properties was determinate by nanoindentation. In the results, the HEBM powder processing shows better efficiency in phase distribution, being the 30% (w/w) of BT in HA matrix that promotes the best bonding strength performance and failure type conduct (cohesive-type), on the other hand HEBM powder treatment promotes a slightly greater crystal phase stability and crystal shrank conduct against MSH; the HEBM promotes a better behavior in the nanomechanical properties of (i) adhesive strength, (ii) cohesive/adhesive failure-type, (iii) stiffness, (iv) elastic modulus, and (v) hardness properties. Full article

Geothermal process equipment and accessories are usually manufactured from low-alloy steels which offer affordability but increase the susceptibility of the materials to corrosion. Applying erosion-corrosion-resistant coatings to these components could represent an economical solution to the problem. In this work, testing of two newly developed laser metal deposited high-entropy alloy (LMD-HEA) coatings—CoCrFeNiMo_0.85 and Al_0.5CoCrFeNi, applied to carbon and stainless steels—was carried out at the Hellisheidi geothermal power plant. Tests in three different geothermal environments were performed at the Hellisheidi site: wellhead test at 194 °C and 14 bar, erosion test at 198 °C and 15 bar, and aerated test at 90 °C and 1 bar. Post-test microstructural characterization was performed via Scanning Eletron Microscope (SEM), Back-Scattered Electrons analysis (BSE), Energy Dispersive X-ray Spectroscopy (EDS), optical microscopy, and optical profilometry while erosion assessment was carried out using an image and chemical analysis. Both the CoCrFeNiMo_0.85 and Al_0.5CoCrFeNi coatings showed manufacturing defects (cracks) and were prone to corrosion damage. Results show that damage in the CoCrFeNiMo_0.85-coated carbon steel can be induced by manufacturing defects in the coating. This was further confirmed by the excellent corrosion resistance performance of the CoCrFeNiMo_0.85 coating deposited onto stainless steel, where no manufacturing cracks were observed. Full article

Cast Ni-Si-B alloys have the potential for high-temperature applications because of their high resistance to wear, impact, corrosion, and oxidation at elevated temperatures due to an appropriate balance of hard phases and austenite that ensures a good compromise between toughness and hardness. In this work, NiSi3B2 specimens, fabricated by the lost-wax casting process, were investigated. Given the complex multiphase cast microstructure, a differential scanning calorimeter (DSC-TGA) analysis was employed to characterize the reactions that occur during solidification and the resulting phases were characterized using scanning electron microscopy (SEM), with energy-dispersive microanalysis (EDS) and backscattered electron (BSE) image and X-ray diffraction (XRD). Due to the presence of hard phases, machining of the Ni-Si-B components can pose additional difficulties. Therefore, the conditions of the solution heat treatment, which might lead to the homogenization of the microstructure, consequently improving its machinability, were also investigated. The results of the heat-treated samples indicated that the dissolution of the eutectic constituent is accompanied by a significant decrease in the hardness (approximately 17%). It is important to emphasize that the solution heat treatments carried out reduced the hardness without affecting the percentage of borides, which will allow improving the machinability without adversely affecting the alloy performance in service. Full article

Scanning electron microscopy based automated mineralogy (SEM-AM) is a combined analytical tool initially designed for the characterisation of ores and mineral processing products. Measurements begin with the collection of backscattered electron (BSE) images and their handling with image analysis software routines. Subsequently, energy dispersive X-ray spectra (EDS) are gained at selected points according to the BSE image adjustments. Classification of the sample EDS spectra against a list of approved reference EDS spectra completes the measurement. Different classification algorithms and four principal SEM-AM measurement routines for point counting modal analysis, particle analysis, sparse phase search and EDS spectral mapping are offered by the relevant software providers. Application of SEM-AM requires a high-quality preparation of samples. Suitable non-evaporating and electron-beam stable epoxy resin mixtures and polishing of relief-free surfaces in particles and materials with very different hardness are the main challenges. As demonstrated by case examples in this contribution, the EDS spectral mapping methods appear to have the most promising potential for novel applications in metamorphic, igneous and sedimentary petrology, ore fingerprinting, ash particle analysis, characterisation of slags, forensic sciences, archaeometry and investigations of stoneware and ceramics. SEM-AM allows the quantification of the sizes, geometries and liberation of particles with different chemical compositions within a bulk sample and without previous phase separations. In addition, a virtual filtering of bulk particle samples by application of numerous filter criteria is possible. For a complete mineral phase identification, X-ray diffraction data should accompany the EDS chemical analysis. Many of the materials which potentially could be characterised by SEM-AM consist of amorphous and glassy phases. In such cases, the generic labelling of reference EDS spectra and their subsequent target component grouping allow SEM-AM for interesting and novel studies on many kinds of solid and particulate matter which are not feasible by other analytical methods. Full article

The purpose of this study was to liberate gold from sulfide minerals in a gold concentrate through microwave-nitric acid leaching and to separate the light minerals in an insoluble residue using a hydro-separation process. The representative sulfide minerals in the gold concentrate were pyrite with minor galena. Mineralogical characterization was conducted on the gold concentrate using 1715.20 g/t based on lead-fire assays. During the leaching experiment, the effect of nitric acid concentration was studied. The results indicated that the metal leaching rate of the gold concentrate increased with increasing nitric acid concentration. After the microwave-nitric acid leaching, the resulting main feature was consistent with the increased exposure to reactive sulfide minerals and decrease in weight. Characterization techniques such as X-ray diffraction (XRD), scanning electron microscope energy dispersive spectroscopy (SEM-EDS) and scanning electron microscope backscattered electron imaging (SEM-BSE) were performed to characterize the minerals in the insoluble residue using microwave-nitric acid leaching and the hydro-separation process. The XRD patterns of the insoluble residues were compared. The intensities of the pyrite peak decreased and disappeared under different nitric acid concentrations, whereas intensities of the quartz peak increased. The hydro-separation process focused on the separation of heavy (e.g., native gold) and light (e.g., quartz) minerals from the insoluble residues. After the hydro-separation treatment process, the heavy minerals exhibited typical diffraction lines of gold, as obtained using the XRD analysis. Full article