Microstructure and mechanical properties of melt-grown alumina-mullite/glass composites fabricated by directed laser deposition

Melt-grown alumina-based composites are receiving increasing attention due to their potential for aerospace applications; however, the rapid preparation of high-performance components remains a challenge. Herein, a novel route for 3D printing dense (< 99.4%) high-performance melt-grown alumina-mullite/glass composites using directed laser deposition (DLD) is proposed. Key issues on the composites, including phase composition, microstructure formation/evolution, densification, and mechanical properties, are systematically investigated. The toughening and strengthening mechanisms are analyzed using classical fracture mechanics, Griffith strength theory, and solid/glass interface infiltration theory. It is demonstrated that the composites are composed of corundum, mullite, and glass, or corundum and glass. With the increase of alumina content in the initial powder, corundum grains gradually evolve from near-equiaxed dendrite to columnar dendrite and cellular structures due to the weakening of constitutional undercooling and small nucleation undercooling. The microhardness and fracture toughness are the highest at 92.5 mol% alumina, with 18.39±0.38 GPa and 3.07±0.13 MPa·m1/2, respectively. The maximum strength is 310.1±36.5 MPa at 95 mol% alumina. Strength enhancement is attributed to the improved densification due to the trace silica doping and the relief of residual stresses. The method unravels the potential of preparing dense high-performance melt-grown alumina-based composites by the DLD technology.

Effect of Solute Redistribution on Seeding Process of TiAl Alloys with Limited Convection in a Float Zone

Two different analytic models, in which convection in the float zone is assumed, are developed to understand the solute redistributions during general seeding and quasi-seeding processes of TiAl alloys, respectively. The results suggest that the solute redistribution plays an important effect in the phase selection and microstructural development during the initial stage of seeding processes. In the initial stage of the quasi-seeding process, the interface concentration increases gradually and the solute diffusion boundary forms with the crystal growth of α phase. Correspondingly, a maximum constitutional undercooling with respect to β phase occurs ahead of the solidifying α interface and then decreases gradually. Simultaneously, the position where the maximum constitutional undercooling occurs also moves forward with regard to the interface. While in the initial stage of the general seeding process, the α phase can grow continuously as stable phase when the initial composition of the melt is higher than Al 48.9%. Under the influence of both the constitutional undercooling and Ti5Si3 particles, coarse dendrites form and then are transformed to cellular morphology. Nevertheless, the lamellar microstructure can still be aligned well during the entire seeding process. Besides, it is also found that the thickness of solute diffusion boundary decreases with the increase of convection intensity and thus, the growing interface become more stably correspondingly, which is beneficial to the lamellar alignment of TiAl alloys.

Effects of Solidification Conditions on Grain Refinement Capacity of TiC in Directionally Solidified Ti6Al4V Alloy

In this study, the effects of solidification conditions on the grain refinement capacity of heterogeneous nuclei TiC in directionally solidified Ti6Al4V alloy were investigated using experimental and numerical approaches. Ti6Al4V powder with and without TiC particles in a Ti6Al4V sheath was melted and directionally solidified at various solidification rates via the floating zone melting method. In addition, by using the phase field method, the microstructural evolution of directionally solidified Ti6Al4V was simulated by varying the temperature gradient G and solidification rate V. As the solidification rate increased, the increment of the prior β grain number by TiC addition also increased. There are two reasons for this: first, the amount of residual potent heterogeneous nuclei TiC is larger. Second, the amount of TiC particles that can nucleate becomes larger. This is because increasing the constitutional undercooling ΔTc leads to the activation of a smaller radius of heterogeneous nuclei and a higher nucleation probability from each radius. At a cooling rate R higher than that in the floating zone melting experiment (R = 3 to 1000 K/s), the maximum degree of constitutional undercooling ΔTc,Max has a peak value, which suggests that constitutional undercooling ΔTc has a smaller contribution at higher cooling rates, such as those that occur during electron beam melting (EBM), including laser powder bed fusion (LPBF).

New Grain Formation by Constitutional Undercooling Due to Remelting of Segregated Microstructures during Powder Bed Fusion

A microstructure has significant influence on the mechanical properties of parts. For isotropic properties, the formation of equiaxed microstructures by the nucleation of new grains during solidification is necessary. For conventional solidification processes, nucleation is well-understood. Regarding powder bed fusion, the repeated remelting of previous layers can cause nucleation under some conditions that are not explainable with classical theories. Here, we investigate this nucleation mechanism with an unprecedented level of detail. In the first step, we built samples with single crystalline microstructures from Ni-base superalloy IN718 by selective electron beam melting. In the second step, single lines with different parameters were molten on top of these samples. We observed a huge number of new grains by nucleation at the melt-pool border of these single lines. However, new grains can only prevail if the alignment of their crystallographic orientation with respect to the local temperature gradient is superior to that of the base material. The current hypothesis is that nucleation at the melt-pool border happens due to remelting microsegregations from former solidification processes leading to constitutional undercooling directly at the onset of solidification. This study offers the opportunity to understand and exploit this mechanism for different manufacturing processes.

Effect of Ce Addition and Heat Treatment on Microstructure Evolution and Tensile Properties of Industrial A357 Cast Alloy

The effects of adding different Ce contents (0–0.32 wt.%) on the microstructure, mechanical properties, and fracture morphology of industrial A357 cast alloy in as-cast and T6 heat treatment were studied. The main purpose of this study is to improve the microstructure stability and tensile properties of industrial A357 cast alloy. The microstructural analyses indicate that the addition of Ce causes refinement of the α-Al primary phase for the reason that the formation of intermetallic compounds containing (AlSiCeMg) elements enriches the front of the solid–liquid interface, which causes an increase in constitutional undercooling. Simultaneously, the addition of Ce also affected the characteristics of eutectic Si particles, which make its morphology change from acicular structures into fragmented and spheroidized. This is mainly due to the formation of Ce-rich precipitates during solidification, which increase the constitutional undercooling and suppress the nucleation of the eutectic Si particles, resulting in the change of eutectic Si characteristics. Moreover, the needle-like morphology of a Fe-containing intermetallic is transformed into α(AlSiFeCe) phase containing rare earth Ce when part of the Ce atoms entered β(Al5FeSi) phase compounds. The tensile properties of the modified alloys were improved in the as-cast and T6 heat treatment as a consequence of simultaneous refinement of both secondary dendrite arm spacing and grains and the improvement of eutectic Si particles and Fe-containing intermetallic morphology. The fracture surface of the modified alloy has more dimples than the unmodified alloy, which indicates that the main fracture pattern of the modified alloy is dimple fracture caused by the crack of eutectic Si particles. The optimal percentage of Ce in industrial A357 cast alloy was determined to be 0.16 wt.% according to the change of microstructures structure and mechanical properties. These experimental results provide a new basis for adding rare earth Ce to improve the performance of parts in the actual production of industrial A357 cast alloy.

Multi-Refinement Effect of Rare Earth Lanthanum on α-Al and Eutectic Si Phase in Hypoeutectic Al-7Si Alloy

The effect of La addition on primary α-Al and the eutectic Si phase of Al-7Si alloy is investigated systematically in this work. The results indicate that La addition causes a multi-refining efficiency on the microstructure of Al-7Si alloy, including refinement of α-Al grains and secondary dendrite arm spacing as well as eutectic Si particles. The grain size, secondary dendrite arm spacing and area of eutectic Si particles are decreased by 26.8%, 7.7% and 26.7%, respectively, with the addition of 0.1 wt.% La. It is also found that La-rich phases of Al2Si2La form and distribute in the vicinity of the eutectic Si phase. The crystal structure and lattice parameter of Al2Si2La phase are determined to be hexagonal (a = b = 0.405 nm, c = 6.944 nm) based on the TEM analysis results. The multi-refinement effects are mainly attributed to the increased constitutional undercooling caused by the low solubility of La in Al alloy and the growth-restricting factor caused by the Al2Si2La phase.

Different Influences of Rare Earth Eu Addition on Primary Si Refinement in Hypereutectic Al–Si Alloys with Varied Purity

The effect of alloying the Eu element on primary Si refinement in varied purity Al–16Si alloys was studied by scanning electron microscopy (SEM), thermal analysis, micro x–ray diffraction (μ–XRD), electron probe microanalysis (EPMA), and transmission electron microscopy (TEM). The results indicate that the P impurity element in hypereutectic Al–Si alloys has a great influence on the rare earths’ refinement efficiency of primary Si. Coinstantaneous primary Si refinement and eutectic Si modification by Eu was obtained in high purity (HP) Al–16Si and commercial purity (CP) Al–16Si–0.06P alloys, but the primary Si was gradually coarsened in CP Al–16Si alloys. An excellent integration of ultimate tensile strength (144.8 MPa) and elongation (9.8%) of CP hypereutectic Al–16Si–0.06P alloy was obtained by adding 0.15% Eu. The refinement of primary Si in Eu–modified HP Al–16Si alloys was related to the constitutional undercooling of Eu. There was no sufficient Eu element partition into the primary Si particles, and fewer parallel twins, rather than multiple twins, were observed within them. The refinement of primary Si in CP Al–16Si–0.06P alloys was caused by the overlay of two kinds of mechanisms including the heterogeneous nucleation mechanism of AlP and the constitutional supercooling mechanism of Eu. However, in order to refine the primary Si in CP hypereutectic Al–16Si alloys, the Eu:P weight ratio should not exceed 3.33, otherwise the refinement efficiency of primary Si will be reduced due to mutual poisoning between Eu and P. This work can be used to interpret the controversy concerning the influence of rare earths on the primary Si in hypereutectic Al–Si alloys, thereby elucidating the importance of alloy purity to primary Si refinement by rare earths.

Revealing the Nuclei Formation in Carbon-Inoculated Mg-3%Al Alloys Containing Trace Fe

In this study, Fe-bearing Mg-3%Al alloys were inoculated by combining carbon with or without Ca. Both processes can significantly refine the grain size of Mg-3%Al alloys. The highest refining efficiency can be obtained by carbon combined with Ca. The synergistic grain refining efficiency can be attributed to the constitutional undercooling produced by the addition of Ca. Two kinds of carbon-containing nuclei with duplex-phase particles and cluster particles were observed in the carbon-inoculated alloys. A thermodynamic model was established to disclose the formation mechanisms of the duplex-phase particles and Al4C3 cluster particles. This thermodynamic model is based on the change of Gibbs free energy for the formation of these two kinds of particles. The calculated results show that these two particles can form spontaneously, since the change of Gibbs free energy is negative. However, the Gibbs free change of the duplex-phase particle is more negative than the Al4C3 cluster particle. This indicates that the adsorption process is more spontaneous than the cluster process, and tiny Al4C3 particles are preferred to form duplex-phase particle, rather than gathering to form an Al4C3 cluster particle. In addition, the addition of Ca can reduce the interfacial energy between the Al4C3 phase and the Al–Fe phase and promote the formation of duplex-phase particles.