Semisolid processing characteristics of AM series Mg alloys by rheo-diecasting

An investigation has been made into the solidification behavior and microstructural evolution of AM50, AM70, and AM90 alloys during rheo-diecasting, their processibility, and the resulting mechanical properties. It was found that solidification of AM series alloys under intensive melt shearing in the unique twin-screw slurry maker during rheo-diecasting gave rise to numerous spheroidal primary magnesium (Mg) particles that were uniformly present in the microstructure. As a result, the network of the β-Mg₁₇Al₁₂ phase was consistently interrupted by these spheroidal and ductile particles. Such a microstructure reduced the obstacle of deformation and the harmfulness of the β-Mg₁₇Al₁₂ network on ductility, and therefore improved the ductility of rheo-diecast AM alloys. It was shown that, even with 9 wt pct Al, the elongation of rheo-diecast AM90 still achieved (9 ± 1.2) pct. Rheodiecasting thus provides an attractive processing route for upgrading the alloy specification of AM series alloys by increasing the aluminum (Al) content while ensuring ductility. Assessment of the processibility of AM series alloys for semisolid processing showed that high Al content AM series alloys are more suitable for rheo-diecasting than low Al content alloys, because of the lower sensitivity of solid fraction to temperature, the lower liquidus temperature, and the smaller interval between the semisolid processing temperature and the complete solidification temperature.     

Effects of microstructure on the fracture toughness of Ti3Al-based titanium aluminides

The influence of microstructure on the fracture toughness of Ti-23A1-9Nb-2Mo-1Zr-1.2Si (at. pct) and Ti-23A1-11Nb-0.9Si (at. pct) Ti₃Al-based alloys has been investigated. Basket-weave microstructures comprising different volume fractions of α ₂ and retained β phases were produced by systematic heat treatments. Besides the volume fraction of the retained β phase, the average size of the β laths has also been used to characterize these microstructures. The toughness of both alloys was examined at room temperature, and the brittle transgranular fracture modes were found to be controlled by microstructure. However, the toughness is not determined solely by the volume fraction of the retained β phase, and a linear relationship has been obtained between the fracture toughness and the average size of the retained β laths. It appears therefore that the toughness of Ti₃Al-based alloys at room temperature is controlled primarily by the width of retained β laths rather than by the retained β volume fraction.     

Influence of Cu additions on the morphology of GeSi precipitates in an Al-Ge-Si alloy

Combined additions of Ge and Si to Al are known to produce higher precipitation hardening than that which occurs in the constituent binaries, when the total amounts of alloying atoms are the same for all the alloys investigated. In the resultant Al-Ge-Si alloys, the diamond cubic precipitates contain both Ge and Si and are designated as GeSi. During artificial aging at 160 °C, the GeSi precipitates are commonly present in three forms, i.e., equiaxed, 〈100〉_Al lath, and triangular plate. The equiaxed form is the dominant one of the three. This article examines the influence of varying amounts (i.e., 2 to 4 wt pct) of Cu additions on the morphology of GeSi precipitates formed in an Al-2.6 wt pct Ge-1.04 wt pct Si alloy during artificial aging at 160 °C. It is shown that Cu additions have the remarkable effect of maximizing the nucleation frequency of the 〈100〉_Al lath form and simultaneously suppressing the nucleation of the equiaxed and the plate forms of the GeSi precipitates. Increasing Cu additions also increase the homogeneity and cause refinement of the 〈100〉_Al laths. These results are discussed in light of (1) the critical requirement of vacancies for the nucleation and growth of GeSi precipitates having an atomic volume larger than Al and (2) the crystallographic nature of the negative dilation strains that develop locally in the Cu-rich regions of the Al matrix. It is further shown that, in the alloys containing increased levels (i.e., exceeding about 2.5 wt pct) of Cu, the precipitation of ϑ′ (metastable ϑ-Al₂Cu) phase occurs, and that the nucleation of Cu-rich ϑ′ precipitates occurs upon the 〈100〉_Al laths of GeSi. The latter effect is discussed in terms of the attainment of both the nucleation site and the necessary solute supersaturation at the 〈100〉_Al GeSi/α-Al interfaces.     

Surface and Interface Energies of Complex Crystal Structure Aluminum Magnesium Alloys

Alloying Al with Mg can improve its structural properties but also can lead to the formation of grain-boundary precipitates of β-Mg₂Al₃ that lead to failure by intergranular fracture and corrosion. Simulating the properties of the β phase is difficult because it has a complex structure with more than 1000 atoms per unit cell. We approximate the experimental β structure by the β′ structure, which has about 300 atoms per unit cell, and we compute the fracture behavior of the material from density functional theory calculations of relevant surface and interface energies. We report also on experimental measurements of the orientation and fracture properties of the α-Al(Mg)–β-Mg₂Al₃ interface and compare them with the atomistic simulations. We have computed the surface energy of face-centered cubic α-Al with up to 10 at. pct Mg, as well as the decohesion energy of β′-Mg₂Al₃ and the interfacial decohesion energy between β′-Mg₂Al₃ and pure α-Al with geometry similar to that observed experimentally. We find that the β′-Mg₂Al₃ decohesion energy is nearly isotropic and is lower than the pure Al surface energy and the α-Al–β′-Mg₂Al₃ interface decohesion energy. This result is consistent with the experimental observations of fracture within the β phase rather than at the α-Al(Mg)–β-Mg₂Al₃ interface or within the α-Al(Mg) phase.     

Interdiffusion in the Mg-Al System and Intrinsic Diffusion in β-Mg2Al3

Solid-to-solid diffusion couples were assembled and annealed to examine the diffusion between pure Mg (99.96?pct) and Al (99.999?pct). Diffusion anneals were carried out at 573?K, 623?K and 673?K (300?°C, 350?°C and 400?°C) for 720, 360, and 240?hours, respectively. Optical and scanning electron microscopes were used to identify the formation of the intermetallic phases, ??-Mg₁₇Al₁₂, and ??-Mg₂Al₃, as well as the absence of the ??-Mg₂₃Al₃₀ in the diffusion couples. The thicknesses of the ??-Mg₁₇Al₁₂ and ??-Mg₂Al₃ phases were measured and the parabolic growth constants were calculated to determine the activation energies for growth. Concentration profiles were determined with electron microprobe analysis using pure elemental standards. Composition-dependent interdiffusion coefficients in Mg-solid solution, ??-Mg₁₇Al₁₂, ??-Mg₂Al₃, and Al-solid solutions were calculated based on the Boltzmann-Matano analysis. Integrated and average effective interdiffusion coefficients for each phase were also calculated, and the magnitude was the highest for the ??-Mg₂Al₃ phase, followed by ??-Mg₁₇Al₁₂, Al-solid solution, and Mg-solid solution. Intrinsic diffusion coefficients based on Huemann??s analysis (e.g., marker plane) were determined for the ~ Mg-62 at. pct Al in the ??-Mg₂Al₃ phase. Activation energies and the pre-exponential factors for the interdiffusion and intrinsic diffusion coefficients were calculated for the temperature range examined. The ??-Mg₂Al₃ phase was found to have the lowest activation energies for growth and interdiffusion among all four phases studied. At the marker location in the ??-Mg₂Al₃ phase, the intrinsic diffusion of Al was found to be faster than that of Mg. Extrapolations of the impurity diffusion coefficients in the terminal solid solutions were made and compared with the available self-diffusion and impurity diffusion data from the literature. Thermodynamic factor, tracer diffusion coefficients, and atomic mobilities at the marker plane composition were approximated using the available literature values of Mg activity in the ??-Mg₂Al₃ phase.     

The effect of strontium on the Mg2Si precipitation process in 6201 aluminum alloy

A transmission electron microscopy (TEM) study of a 6201 aluminum alloy to which controlled strontium additions were made has revealed important differences compared to the same alloy free of strontium. In the as-cast state, strontium favors the formation of α-AlFeSi (Al₈Fe₂Si) rather than β-AlFeSi (Al₅FeSi) phase, resulting in a greater quantity of excess silicon present in the strontium-treated alloy. During heat treatment, the excess silicon allows a greater density of finer β″-Mg₂Si precipitates to form, leading to increased tensile strength values and increased electrical resistivity. Strontium also retards the growth of the precipitates formed during heat treatment and inhibits formation of the equilibrium β-Mg₂Si phase. As a result, the strontium-treated alloy exhibits a resistance to overaging.     

A thousandfold creep strengthening by Ca addition in die-cast AM50 magnesium alloy

The effect of calcium addition on the microstructure and creep strength of the die-cast AM50 magnesium alloy was investigated. The α-Mg grains with the diameter of 4.9 μm are surrounded by the eutectic phases for the AM50-1.72 mass pct Ca alloy, while the β(Mg₁₇Al₁₂) particles are located mainly on the grain boundaries of the α grains for the AM50 alloy. The minimum creep rates of the AM50-1.72 mass pct Ca alloy are three orders of magnitude lower than those of the AM50 alloy at 423 K typically below 120 MPa. The thousandfold creep strengthening by the Ca addition is ascribed to the thermally stable eutectic phases appearing in the AM50-1.72 mass pct Ca alloy, which is expected to yield effective grain boundary strengthening or to resist the plastic flow of the α-Mg grains.     

The influence of alloy composition on precipitates of the Al-Mg-Si system

To study how changes in solute elements affect precipitation, six Al-Mg-Si alloys aged at 175 °C were investigated by transmission electron microscopy (TEM). In alloys with 1.3 at. pct solute, when the Si/Mg ratio exceeds 5/6, a sharp hardness peak appears after 3 hours that correlates with a high density of fine Guinier-Preston (GP) zones. A second, broader peak correlates with β″ precipitates and U phases. With high Si/Mg ratios, GP zones survive for long aging times. The β″-Mg₅Si₆ phase becomes very stable in the alloy with its Si/Mg ratio closest to 6/5. Deviation from this ratio increases fractions of β′, U-phases and disordered precipitates. In Mg-rich alloys less GP zones form and the first peak is suppressed. A coarse precipitate microstructure of β″ and β′ develops, the volume fraction being much higher than in Si-rich alloys. The Mg-rich alloys overage faster. Reducing the content of solutes causes alloys with high Si/Mg ratios to have a more Mg-rich behavior.     

Comparison of precipitates between excess Si-type and balanced-type Al-Mg-Si alloys during continuous heating

Differential scanning calorimetry (DSC) curves were obtained from Al-1.0 mass pct Mg₂Si (balanced) and Al-1.0 mass pct Mg₂Si −0.4 mass pct Si (excess Si) alloys, and precipitates corresponding to each peak at the DSC curve were interpreted by means of high-resolution transmission electron microscopy (HRTEM) observation in order to understand the precipitation sequence of metastable phases. Five peaks were obtained on the DSC curves, from which four were exothermic (A, C, D, and E) and one endothermic (B). Upon HRTEM observation, the peaks for the excess Si alloy were explained as follows: peak A–B: Guinier-Preston (GP) zones and random-type precipitates; peak B: dissolution of the GP zones and the random-type precipitates, precipitation of the β″ phase; peak C: β″ phase and precipitation of type B; peak D: dissolution of the β″ phase; precipitation of type A and β′ phase; and peak E: dissolution of the type B, type A, and β′ precipitation of the (β+Si) phase. This result is quite different from that in the balanced alloy as follows: peak A–B: GP zones and random-type precipitates; peak B: dissolution of the GP zones and the random-type precipitates, precipitation of the parallelogram-type precipitate; peak C: parallelogram-type precipitate and precipitation of β′ phase; peak D: β′ phase, dissolution of parallelogram-type precipitate; and peak E: the β-(Mg₂Si).     

The role of iron in the formation of porosity in Al-Si-Cu-based casting alloys: Part II. A phase-diagram approach

The mechanism by which iron causes casting defects in the AA309 (Al-5 pct Si-1.2 pct Cu-0.5 pct Mg) may be related to the solidification sequence of the alloy. Superimposing calculated segregation lines on the liquidus projection of the ternary Al-Si-Fe phase diagram suggests that porosity is minimized at a critical iron content when solidification proceeds directly from the primary field to the ternary Al-Si-βAl₅FeSi eutectic point. Solidification via the binary Al-βAl₅FeSi eutectic is detrimental to casting integrity. This hypothesis was tested by comparing the critical iron content observed in the standard AA309 alloy to that of a high-silicon (10 pct Si) variant of this alloy.     

Effects of Zr Additions on the Microstructure and Impression Creep Behavior of AZ91 Magnesium Alloy

The effects of 0.2, 0.6, and 1.0 wt pct Zr additions on the microstructure and creep behavior of AZ91 Mg alloy were investigated by impression tests carried out under constant punching stress (σ _imp) in the range 100 to 650 MPa, corresponding to the modulus-compensated stress levels of 0.007 ￡ s_\textimp \mathord

The effect of Mg on the microstructure and mechanical behavior of Al-Si-Mg casting alloys

The microstructure and tensile behavior of two Al-7 pct Si-Mg casting alloys, with magnesium contents of 0.4 and 0.7 pct, have been studied. Different microstructures were produced by varying the solidification rate and by modification with strontium. An extraction technique was used to determine the maximum size of the eutectic silicon flakes and particles. The eutectic Si particles in the unmodified alloys and, to a lesser extent, in the Sr-modified alloys are larger in the alloys with higher Mg content. Large Fe-rich π-phase (Al₉FeMg₃Si₅) particles are formed in the 0.7 pct Mg alloys together with some smaller β-phase (Al₅FeSi) plates; in contrast, only β-phase plates are observed in the 0.4 pct Mg alloys. The yield stress increases with the Mg content, although, at 0.7 pct Mg, it is less than expected, possibly because some of the Mg is lost to π-phase intermetallics. The tensile ductility is less in the higher Mg alloys, especially in the Sr-modified alloys, compared with the lower Mg alloys. The loss of ductility of the unmodified alloy seems to be caused by the larger Si particles, while the presence of large π-phase intermetallic particles accounts for the loss in ductility of the Sr-modified alloy.     

Role of cold work and SiC reinforcements on the β′/β precipitation in Al-10 pct Mg alloy

Elevated temperature (above 100 °C) precipitation behaviors were studied in A1-10 wt pct Mg alloy and the same alloy reinforced with SiC particles through electrical resistivity, hardness, differential scanning calorimetry (DSC), and microscopy. Two distinct hardness peaks/resistivity drops, as associated with two precipitation events, were identified: (1) α (solid solution) → β′ (metastable hex precipitate) → β (Al₃Mg₂, stable complex cubic precipitate); and (2) α → β. Equilibrium β precipitates, transformed from metastable β′, were observed to possess a wide variet of orientation relationships with the matrix and were often observed to be twinned. A more restricted orientation relationship (only three variants) between β and matrix was observed in direct decomposition of α to β, and β precipitates, within these orientation relationships, were never observed to be twinned. In a predominantly binary Al-Mg system, direct precipitation of β was observed to dominate. However, the presence of trace amounts of boron nitride and/or boron (or a large supply of matrix dislocations) either from cold work, or (as in case of composites) from the thermal mismatch between the SiC and Al matrix, produced both precipitation events with event 1 dominant.     

Deformation and fracture behavior of a directionally solidified β/γ′ Ni-30 At. pct Al alloy

The effect of a ductile γ′-Ni₃Al phase on the room-temperature ductility, temperature-dependent yield strength, and creep resistance of β-NiAl was investigated. Room-temperature tensile ductility of up to 9 pct was observed in directionally solidified β/γ′ Ni-30 at. pct Al alloys, whereas the ductility of directionally solidified (DS), single-phase [001] β-NiAl was negligible. The enhancement in ductility was attributed to a combination of slip transfer from the ductile γ′ to the brittle β phase and extrinsic toughening mechanisms such as crack blunting, deflection, and bridging. As in single-phase Ni₃Al, the temperature-dependent yield strength of these two-phase alloys increased with temperature with a peak at approximately 850 K. The creep strength of the β/γ′ alloys in the temperature range 1000 to 1200 K was found to be comparable to that of monolithic β-NiAl. A creep strengthening phase needs to be incorporated in the β/γ′ microstructure to enhance the elevated temperature mechanical properties.     

A sintering study on the β-spodumene-based glass ceramics prepared from gel-derived precursor powders with LiF additive

Beta-spodumene (Li₂O·Al₂O₃·4SiO₂, LAS) powders were prepared by a sol-gel process using Si(OC₂H₅)₄, Al(OC₄H₉)₃, and LiNO₃ as precursors and LiF as a sintering aid agent. Dilatometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and electron diffraction (ED) were utilized to study the sintering, phase transformation, microstructure, and properties of the β-spodumene glass-ceramics prepared from the gel-derived precursor powders with and without LiF additives. For the LAS precursor powders containing no LiF, the only crystalline phase obtained was β-spodumene. For the pellets containing less than 4 wt pct LiF and sintered at 1050 °C for 5 hours the crystalline phases were β-spodumene and β-eucryptite (Li₂O·Al₂O₃·2SiO₂). When the LiF content was 5 wt pct and the sintering process was carried out at 1050 °C for 5 hours, the crystalline phases were β-spodumene, β-eucryptite (triclinic), and eucryptite (rhombohedral (hex.)) phases. With the LiF additive increased from 0.5 to 4 wt pct and sintering at 1050 °C for 5 hours, the open porosity of the sintered bodies decrease from 30 to 2.1 pct. The grains size is about to 4 to 5 μm when pellect LAS compact contains LiF 3 wt pct as sintered at 1050 °C for 5 hours. The grains size grew to 8 to 25 μm with a remarkable discontinuous grain growth for pellet LAS compact contain LiF 5 wt pct sintered at 1050 °C for 5 hours. Relative densities greater than 90 pct could be obtained for the LAS precursor powders with LiF > 2 wt pct when sintered at 1050 °C for 5 hours. The coefficient of thermal expansion of the sintered bodies decreased from 8.3 × 10⁻⁷ to 5.2 × 10⁻⁷/°C (25 °C to 900 °C) as the LiF addition increased from 0 to 5 wt pct.     

Characteristics of lath martensite: Part I. crystallographic and substructural features

This investigation, using an Fe-20 pct Ni-5 pct Mn (wt pct) alloy, was carried out to provide more detailed and accurate information on the crystallographic features of ferrous lath martensite than is presently available. The martensite observed was typical of that found in low carbon steels, but with the present alloy substantial amounts of retained austenite are found, which can be used as a crystallographic reference basis. Analysis of some twenty laths showe_d_the average austenite-martensite orientation relationship to be (lll)_f ‖ (011)_b: [•101]_f 3.9 deg from [•1•1l]_b, using an electron diffraction method involving an error of only a fraction of a degree. Adjacent laths within a packet of lath martensite were found to exhibit the same variant of the orientation relationship although such laths may be misoriented relative to each other by up to 2 deg. Thick layers of austenite found between adjacent laths indicate that the laths do not form by self-accommodation. The lath martensite habit plane is irrational, close to (575)_f [equivalently (•154)_b], but since the habit plane is of the type hkh, 12 apparent habit planes are observed although 24 variants of the orientation relationship may be found. The martensite-austenite interface on one side of a given lath is relatively planar, while that on the opposite side is irregular, suggesting that the laths thicken mainly in one direction. The martensite laths contain screw dislocations in all four ( 111 )_b directions, but one set of the four with Burgers vector α/2 [•111]_b is clearly dominant as a result of accommodation deformation imposed by the large lath martensite shape strain. Austenite dislocation arrays associated with the straight and irregular lath interfaces are very different, again suggesting that the thickening of a lath takes place mainly in one direction away from the initial straight interface.     

Room-temperature deformation behavior of directionally solidified multiphase Ni-Fe-Al alloys

Directionally solidified (DS) β + (γ + γ′) Ni-Fe-Al alloys have been used to investigate the effect of a ductile second phase on the room-temperature mechanical behavior of a brittle 〈001〉-oriented β (B2) phase. The ductile phase in the composite consisted of a fine distribution of ordered γ′ precipitates in a γ (fcc) matrix. Three microstructures were studied: 100 pct lamellar/rod, lamellar + proeutectic β, and discontinuous γ. The β matrix in the latter two microstructures contained fine-scale bcc precipitates formed due to spinodal decomposition. Room-temperature tensile ductilities as high as 12 pct and fracture toughness (K _Q ) of 30.4 MPa √m were observed in the 100 pct lamellar/rod microstructure. Observations of slip traces and dislocation substructures indicated that a substantial portion of the ductility was a result of slip transfer from the ductile phase to the brittle matrix. This slip transfer was facilitated by the Kurdjumov-Sachs (KS) orientation relationship between the two phases and the strong interphase interface which showed no decohesion during deformation. In microstructures which show higher values of tensile ductility and fracture toughness, 〈100〉 slip was seen in the β phase, whereas 〈111〉 slip was seen in the β phase in the microstructure which showed limited ductility. The high ductility and toughness are explained in terms of increased mobile dislocation density afforded by interface constraint. The effect of extrinsic toughening mechanisms on enhancing the ductility or toughness is secondary to that of slip transfer.     

The morphology and substructure of martensite in maraging steels

Thin foil transmission electron microscopy, X-ray diffraction and dilatometric techniques have been used to study the martensitic γ → α transformation in three steels with nominal contents of 8 pct nickel and 0.2 pct beryllium and chromium contents of 12, 14 and 16 pct. In each case the martensite formed as laths with a habit plane close to {225}_γ. With increasing chromium content and increasing cooling rate greater numbers of the laths were observed to be internally twinned. Detailed analysis of the martensitic transformation suggested that the internally twinned laths are formed by a sequence of γ→ ε or faulted γ→ ά. The orientation relationships between the three phases γ, ε and α, determined from selected area diffraction analysis, corresponded to Kurdjumov-Sachs.