Search Results (21)

Immiscible Al–Sn–Cu alloys may offer attractive properties, attaining superior tribological and mechanical properties when Sn-rich soft particles are homogeneously distributed in the reinforced Al–Cu matrix. In this paper, the solidifications of both Al-10 wt.% Cu-10 wt.% Sn and Al-10 wt.% Cu-20 wt.% Sn alloys were investigated to analyze the successive stages that occur during the controlled cooling of these alloys, from the initial formation of the α-Al dendritic array to the final eutectic reaction. In particular, we focus on the liquid-phase demixing occurring during the solidification path, which leads to the formation of Sn droplets in the melt through a nucleation-growth process. Horizontal directional solidifications were performed on thin samples in a Bridgman-type furnace, with in situ and real-time observations using X-ray radioscopy. Two different behaviors have been found concerning liquid separation: for the low-Sn-content alloy, liquid demixing occurs in one single step, whereas for the high-Sn-content alloy, it is a two-step process, with first the nucleation of a few small Sn droplets followed by a sudden formation of a large amount of wide Sn droplets. The possible causes of these different behaviors are discussed in relation to the literature, namely, either a switch from immiscible to miscible liquids or a transition from the binodal region to the spinodal region. Full article

Al–Zn–Mg–Si alloy coatings have been developed to inhibit the corrosion of cold-rolled steel sheets by offering galvanic and barrier protection to the substrate steel. It is known that Fe deposited from the steel strip modifies the microstructure of the alloy. We cast samples of Al–Zn–Mg–Si coating alloys containing 0.4 wt% Fe and directionally solidified them using a Bridgman furnace to quantify the effect of this Fe addition between $600 °\mathrm{C}$ and $240 °\mathrm{C}$. By applying a temperature gradient, growth is encouraged, and by then quenching the sample in coolant, the microstructure may be frozen. These samples were analysed using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) to determine the morphological effects of the Fe distribution across the experimental temperature range. However, due to the sub 1 wt% concentration of Fe, synchrotron X-ray fluorescence microscopy (XFM) was applied to quantitatively confirm the Fe distribution. Directionally solidified samples were scanned at 7.05 keV and 18.5 keV using X-ray fluorescence at the Australian Synchrotron using the Maia array detector. It was found that a mass nucleation event of the Fe-based τ₆ phase occurred at $495 °\mathrm{C}$ following the nucleation of the primary α-Al phase as a result of a peritectic reaction with remaining liquid. Full article

During the solidification process, microstructures are affected by the experimental conditions, the thermophysical characteristics of the alloy, and the type of grain-refining particles. Unidirectional solidification experiments were performed in a vertical Bridgman-type furnace to investigate the effect of the solidification front velocity on the solidified microstructure of a non-refined and refined Al-20%Cu alloy. The samples were solidified by rapidly increasing the sample velocity (v) range from 0.02 mm/s to 0.2 mm/s while maintaining an almost constant temperature gradient (~5 K/mm). As a result, despite changes in the solid/liquid front velocity along the sample, the microstructure of the non-refined alloys remained columnar. In the refined alloy, the columnar structure changed into an equiaxed structure at two different front velocities. Full article

Oriented magnesium bicrystals with a 45°$⟨10\overline{1}0⟩$ asymmetrical tilt boundary were produced by directional solidification in a vertical Bridgman furnace. Employing a partition in the cylindrical mold led to unwanted crystallization on the contact surface with the growing interface, disrupting the desired growth conditions for the boundary. A modified setup with seed crystals placed side by side in a conical mold addressed the former issue and enabled the production of high-quality 56 mm × $\mathrm{\varnothing }$ 34 mm bicrystals. Due to the asymmetrical character of the boundary, the adjacent growing crystals witnessed unequal growth rates, with the basal-oriented crystal dominating the growth process. Plane strain compression experiments were carried out on bicrystalline samples extracted from the prepared bicrystal. The panoramic orientation mapping of large areas of several mm² revealed low-angle boundaries (5° misorientation) associated with the curved segments of the original asymmetrical tilt boundary. It also depicted heterogeneous lattice rotation near the grain boundaries. Full article

Crystal materials are prone to cracking during growth, which is a key problem leading to slow growth and difficulty in forming large-size crystals. In this study, based on the commercial finite element software COMSOL Multiphysics, the transient finite element simulation of the multi-physical field, including fluid heat transfer—phase transition—solid equilibrium—damage coupling behaviors, is performed. The phase-transition material properties and maximum tensile strain damage variables are customized. Using the re-meshing technique, the crystal growth and damage are captured. The results show the following: The convection channel at the bottom of the Bridgman furnace greatly influences the temperature field inside the furnace, and the temperature gradient field significantly influences the solidification and cracking behaviors during crystal growth. The crystal solidifies faster when it enters the higher-temperature gradient region and is prone to cracking. The temperature field inside the furnace needs to be properly adjusted so that the crystal temperature decreases relatively uniformly and slowly during the growth process to avoid crack formation. In addition, the crystal growth orientation also significantly affects the nucleation and growth direction of cracks. Crystals grown along the a-axis tend to form long cracks starting from the bottom and growing vertically, while crystals grown along the c-axis induce the laminar cracks from the bottom in a horizontal direction. The numerical simulation framework of the damage during crystal growth, which can accurately simulate the process of crystal growth and crack evolution and can be used to optimize the temperature field and crystal growth orientation in the Bridgman furnace cavity, is a reliable method to solve the crystal cracking problem. Full article

The single-crystal lithium hydride (LiH) generally grows in a gradient temperature region with the Bridgman method. A stable and appropriate temperature gradient is crucial in the crystallization process. In this paper, the temperature variation of single-crystal LiH growth is calculated by the finite element method (FEM). It is shown that the LiH compact melted entirely after heating to 750 °C at 10 °C/min in a dual-temperature furnace and holding for 2.4 h. The crystallization margin was 46.5 °C after holding for 5 h. The crystallization margin of LiH at the cone point, respectively, decreased to 33.7 °C, 28.6 °C, 25.6 °C, and 16.5 °C when the upper furnace was maintained at 750 °C, and lower furnace was cooled to 680 °C, 650 °C, 630 °C, and 550 °C, respectively. The optimal conditions for obtaining large size and high-quality LiH single crystals were predicted to be 630 °C at a lower-temperature-zone, 200 mL/min (cooling water flux), and 20 mm/h rise rate of the furnace. Based on the parameters of the above simulation, we synthesized LiH single crystal. X-ray diffraction (XRD) patterns showed that the LiH single crystal exhibited a (2 0 0) crystallographic plane at 44.5° with good chemical stability in air. Full article

Using magnetic stirring during solidification provides a good opportunity to control the microstructure of alloys, thus controlling their physical properties. However, magnetic stirring is often accompanied by a change in local concentrations, and new structures form which could harm the physical properties. This research paper investigated the effect of forced melt flow by a rotating magnetic field (RMF) on the macrostructure of an Al-Si eutectic alloy. To serve this purpose, Al-12.6 wt% Si alloy samples were solidified in a vertical Bridgman-type furnace equipped with a rotating magnetic inductor to induce the flow in the melt. The diameter and length of the sample are 8 mm and 120 mm, respectively. The solidification parameters are a temperature gradient (G) of 6 K/m, and the solid/liquid front velocity (v) of 0.1 mm/s. These samples were divided into parts during the solidification process, where some of these parts are solidified under the effect of RMF stirring while others are solidified without stirring. The structure obtained after solidification showed a distinct impact of stirring by RMF; new phases have been solidified which were not originally present in the structure before stirring. Besides the eutectic structure, the new phases are the primary aluminum and the primary silicon. The Si concentration and the volume fraction of each phase were measured using Energy-Dispersive Spectroscope (EDS)and new image processing techniques. The experimental results reveal that applying the RMF during the solidification has a distinct effect on the macrostructure of Al-Si eutectic alloys. Indeed, the RMF provokes macro-segregation, reduces the amount of eutectic structure, and changes the sample’s Si concentration distribution. Full article

During ground-based solidification, buoyancy flow can develop by the density difference in the hypoeutectic type of the alloys, such as Al-7 wt% Si alloy. Buoyancy flow can affect the thermal field, solute distribution in the melt, and the position and amount of the new grains. As solidification is a very complex process, it is not very easy to separate the different effects. Under microgravity conditions, natural convection does not exist or is strongly damped due to the absence of the buoyancy force. Therefore, experiments in microgravity conditions provide unique benchmark data for pure diffusive solidification conditions. Compared to the results of the ground-based and microgravity experiments, it is possible to get information on the effect of gravity (buoyancy force). In the framework of the CETSOL project, four microgravity solidification experiments were performed on grain refined (GF) and non-grain refined Al-7 wt% Si alloy onboard the International Space Station in the Materials Science Laboratory. These experiments aimed to study the effect of the solidification parameters (solid/liquid front velocity v_SL, temperature gradient G_SL) on the grain structure and dendritic microstructures. The microgravity environment eliminates the melt flow, which develops on Earth due to gravity. Four ground-based (GB) experiments were performed under Earth-like conditions with the same (similar) solidification parameters in a vertical Bridgman-type furnace having four heating zones. The detailed analysis of the grain structure, amount of eutectic, and secondary dendrite arm spacing (SDAS) for different process conditions is reported and compared with the results of the microgravity experiments. GB experiments showed that the microstructure was columnar in the samples that do not contain GF material or in case the solid/liquid (v_SL front velocity was slow (0.02 mm/s)). In contrast, in the sample which contained GF material, progressive columnar/equiaxed transition (PCET) was observed at v_SL = 0.077 mm/s and G_SL = 3.9 K/mm. The secondary (SDAS) dendrite arm spacing follows the well-known power law, $SDAS=K{[t_0]}^{\frac{1}{3}}$, where K is a constant, and t₀ is the local solidification time for both GB and µg experiments. Full article

Al–Si eutectic alloys are industrially important; they play a significant role in the casting-manufacturing of most materials. The properties of the materials are governed by their microstructure, which can be tuned by adjusting the solidification process parameters. Herein, the effect of forced melt flow on the microstructure of an Al–Si eutectic alloy during unidirectional solidification was investigated experimentally. Al–12.6-wt%-Si alloy samples were solidified in a vertical Bridgman-type furnace equipped with a rotating magnetic inductor to induce flow in the melt. The samples were subjected to different magnetic induction conditions during the solidification experiments. The diameter of the samples was 8 mm, and their length was 120 mm. The eutectic alloy samples were solidified unidirectionally at a growth rate of v ≈ 0.1 mm/s and a temperature gradient of G ≈ 6 K/mm. The inter-lamellar distances (λ), lengths, and orientation angles of the Si lamellae were investigated using new measurement methods. The experimental results reveal that applying the rotating magnetic field (RMF) during the solidification has a distinct effect on the microstructure of Al–Si eutectic alloys. Indeed, the RMF refines the eutectic structure, reduces the interlamellar distances, and increases the diversity of the Si lamella angle’s orientations. However, the successive stirring process has a negligible effect on the lengths and angles of Si lamellae. Full article

The relationship between the angles of misorientation of macroscopic low-angle boundaries (LABs) and changes in the lattice parameter of the γ′-phase around the LABs in the root of single-crystalline (SX) turbine blades made of CMSX-4 superalloy were studied. The blades with an axial orientation of the [001] type were solidified using an industrial Bridgman furnace with a 3 mm/min withdrawal rate. X-ray diffraction topography, the EFG Ω-scan X-ray diffraction method, scanning electron microscopy, and Laue diffraction were used to study the thin lamellar samples with a thickness of 0.5 mm and orientation of the surface perpendicular to the [001] direction. It is found that in the areas with a width of a few millimetres around LABs, decreases in the lattice parameter of the γ′-phase occur. These lattice parameter changes are related to the internal stresses of the γ′-phase caused by local changes in the concentration of alloying elements and/or to the dendrite bending near the LABs. X-ray topography used on two surfaces of thin lamellar samples coupled with the lattice parameter measurements of the γ′-phase near the LAB allows separating the misorientation component of LAB diffraction contrast from the component and visualising the internal stresses of the γ′-phase. Full article

Various alloy compositions were cast as single crystals in a Bridgman vacuum induction furnace and creep tested at 980 °C: pure Ni, the equiatomic alloys CoCrNi and CrMnFeCoNi (Cantor alloy), single-phase fcc (Ni) solid solution alloys (with the composition of the matrix-phase of CMSX-3 and CMSX-4), and two-phase Ni-based superalloys CMSX-3 and CMSX-4. Due to the single-crystal state, grain size effects, grain boundary sliding, and grain boundary diffusion can be excluded. The results identify two major strengthening mechanisms: solid solution strengthening and other mechanisms summarized as precipitation hardening. Configurational entropy does not increase creep strength: The Cantor alloy, with the highest configurational entropy of all alloys tested, shows a weak and similar creep strength at 980 °C in comparison to pure Ni with zero configurational entropy. The element Re is a very effective strengthener, both in single-phase fcc (Ni) solid solution alloys as well as in two-phase superalloys. Quantitative estimations of different strengthening mechanisms: internal back stress, misfit stresses, Orowan bowing, and γ′-phase cutting (in the case of two-phase superalloys) are presented. Finite element simulations allow estimating the influence of solid solution strengthening of the matrix on the creep behavior of the two-phase superalloys. Full article

The areas located near the cooling bores of single-crystalline cored turbine blades made of nickel-based CMSX-4 superalloy were studied. The blades were solidified by the vertical Bridgman technique in the industrial ALD furnace. Longitudinal sections of the blades were studied by Scanning Electron Microscopy, X-ray diffraction topography, X-ray diffraction measurements of the γ′-phase lattice parameter a, and the α angle of the primary crystal orientation. The local changes in α were analyzed in relation to the changes of the dendrite’s growth direction near the cooling bores. It was found that in the area approximately 3 ÷ 4 mm wide around the cooling bores, changes of α and a, both in the blade root and in the airfoil occurred. The local temperature distribution near the cooling bores formed a curved macroscopic solidification front, which caused changes in the chemical composition and, consequently, changes in the a value in a range of 0.002 Å to 0.014 Å. The mechanism of alloying elements segregation by tips of the dendrites on the bent solidification front was proposed. The multi-scale analysis that allows determining a relation between processes proceed both on a millimeter-scale and a micrometric and nanometric scale, was applied in the studies. Full article

Quaternary semiconductor materials of the Pb₄Ga₄GeS(Se)₁₂ composition have attracted the attention of researchers due to their possible use as active elements of optoelectronics and nonlinear optics. The Pb₄Ga₄GeS(Se)₁₂ phases belong to the solid solution ranges of the Pb₃Ga₂GeS(Se)₈ compounds which form in the quasi-ternary systems PbS(Se)−Ga₂S(Se)₃−GeS(Se)₂ at the cross of the PbGa₂S(Se)₄−Pb₂GeS(Se)₄ and PbS(Se)−PbGa₂GeS(Se)₆ sections. The quaternary sulfide melts congruently at 943 K. The crystallization of the Pb₄Ga₄GeSe₁₂ phase is associated with the ternary peritectic process L_p + PbSe ↔ PbGa₂S₄ + Pb₃Ga₂GeSe₈ at 868 K. For the single crystal studies, Pb₄Ga₄GeS(Se)₁₂ were pre-synthesized by co-melting high-purity elements. The X-ray diffraction results confirm that these compounds possess non-centrosymmetric crystal structure (tetragonal symmetry, space group P–42₁c). The crystals were grown by the vertical Bridgman method in a two-zone furnace. The starting composition was stoichiometric for Pb₄Ga₄GeS₁₂, and the solution-melt method was used for the selenide Pb₄Ga₄GeSe₁₂. The obtained value of the bandgap energy for the Pb₄Ga₄GeS₁₂ and Pb₄Ga₄GeSe₁₂ crystals is 1.86 and 2.28 eV, respectively. Experimental measurements of the spectral distribution of photoconductivity for the Pb₄Ga₄GeS₁₂ and Pb₄Ga₄GeSe₁₂ crystals exhibit the presence of two spectral maxima. The first lies in the region of 570 (2.17 eV) and 680 nm (1.82 eV), respectively, and matches the optical bandgap estimates well. The locations of the admixture maxima at about 1030 (1.20 eV) and 1340 nm (0.92 eV), respectively, agree satisfactorily with the calculated energy positions of the defects vs. and V_Se. Full article

The roots of cored single-crystalline turbine blades made of a nickel-based CMSX-4 superalloy were studied. The casts were solidified by the vertical Bridgman method in an industrial ALD furnace using the spiral selector and selector continuer situated asymmetrically in the blade root transverse section. Scanning electron microscopy, the Laue diffraction and X-ray diffraction topography were used to visualize the dendrite array and the local crystal misorientation of the roots. It has been stated that heterogeneity of the dendrite array and creation of low-angle boundaries (LABs) are mostly related to the lateral dendrite branching and rapid growth of the secondary and tertiary dendrites near the surface of the continuer–root connection. These processes have an unsteady character. Additionally, the influence of the mould walls on the dendrite array heterogeneity was studied. The processes of the lateral growth of the secondary dendrites and competitive longitudinal growth of the tertiary dendrites are discussed and a method of reducing the heterogeneity of the root dendrite array is proposed. Full article

Cast iron exhibits a wide range of mechanical properties, depending on its microstructural features. The microstructure of cast iron consists of several microconstituents with different elastic-plastic behavior, making the strain non-uniform across the bulk material. To understand the individual effects of these microconstituents on the overall mechanical behavior, local strain analysis using digital image correlation analysis was carried out. Samples with two different compositions (varying cerium, magnesium and silicon) were processed at different solidification velocities in a Bridgman furnace. Sections of the directionally solidified samples were loaded under uniaxial compression to measure global and local strain behavior. Despite the variability of the microstructure, the stress–strain curves obtained by digital image correlation (DIC) were found to react in a well-controlled way to changes in solidification velocity. It was observed that high-strain failure (greater than 15%) was accompanied by local straining of the softer ferritic phase, but during low-strain failure, local straining was not prominent. Higher nodularities, due to higher solidification velocities, raised the compressive strength without affecting the toughness significantly. Higher percentages of carbides led to higher compressive strengths with corresponding losses in ductility. The continuity of the matrix was also found to play an important role in the behavior during compression. Full article