Microstructural change and precipitation hardening in melt-spun Mg–X–Ca alloys

Mg–Al–Si–Ca and Mg–Zn–Ca base alloys were rapidly solidified by melt spinning at the cooling rate of about a million K/s. The melt-spun ribbons were aged in the range 100–400°C for 1 h. The effect of additional elements on microstructural change and precipitation hardening after heat treatment was investigated using TEM, XRD and a Vickers microhardness tester. Age hardening occurred after aging at 200°C in the Mg–Al–Si–Ca alloys mainly due to the formation of Al₂Ca and Mg₂Ca phases, whereas in the Mg–Zn–Ca alloys mostly due to the distribution of Mg₂Ca. TEM results revealed that spherical Al₂Ca precipitate has the coherent interface with the matrix. Considering the total amount of additional elements, Mg–Zn–Ca alloys showed higher hardness and smaller size of precipitates than Mg–Al–Si–Ca alloys. With the increase of Ca content, the hardness values of the aged ribbons were increased. Among the alloys, Mg–6Zn–5Ca alloy showed the maximum value of age hardening peak(H_v:180) after aging at 200°C for 1 h.     

Development of microstructure in cast Mg–AI–rare earth alloys

Abstract

The microstructures and age hardening behaviours of a series of Mg–Al–rare earth (RE) alloys that had been either pressure die cast or permanent mould cast were investigated by SEM and analytical TEM. Two types of phases, Al₄MM and Al₁₂Mg₁₇, were found in the as cast alloys and no pseudoternary Mg–Al–RE phases were present. The Al₄MM phase was thermally stable during solution treatment at temperatures as high as 500°C, whereas Al₁₂Mg₁₇ partially dissolved in the α-Mg matrix during solution treatment at 420°C. No rare earth containing precipitates formed during heat treatment of the investigated alloys but two types of Al₁₂Mg₁₇ precipitation took place. Colonies of discontinuous precipitation containing alternate lamellae of α-Mg and Al₁₂Mg₁₇ formed preferentially in regions α-Mg with high aluminium content. Spheroidisation and coarsening of the discontinuous precipitates occurred after aging at 200°C. Continuous precipitation of Al₁₂Mg₁₇ also occurred and these precipitates had a rodlike morphology and grew in preferred crystallographic directions.

MST/3382     

Microstructural change and precipitation hardening in melt–spun Mg–X–Ca alloys

Mg–Al–Si–Ca and Mg–Zn–Ca base alloys were rapidly solidified bymelt spinning at the cooling rate of about a million K/s. The melt-spun ribbons were aged in the range 100–400%C for 1 h. The effect of additional elements on microstructural change and precipitation hardening after heat treatment was investigated using TEM, XRD and a Vickers microhardness tester. Age hardening occurred after aging at 200%C in the Mg–Al–Si–Caalloys mainly due to the formation of Al₂Ca and Mg₂Ca phases, whereas in the Mg–Zn–Ca alloys mostly due to the distribution of Mg₂Ca. TEM results revealed that spherical Al₂Ca precipitate has the coherent interface with the matrix. Considering the total amount of additional elements, Mg–Zn–Ca alloys showed higher hardness and smaller size of precipitates than Mg–Al–Si–Ca alloys. With the increase of Ca content, the hardness values of the aged ribbons were increased. Among the alloys, Mg–6Zn–5Ca alloy showed the maximum value of age hardening peak(H_v:180) after aging at 200%C for 1h.     

Superplastic behavior and microstructural stability of friction stir processed AZ91C alloy

Superplastic behavior of a solution treated and friction stir processed (FSP) AZ91C alloy is studied. These studies are conducted in the temperature range of 300–375 °C and strain rates (SRs) in the range of 1 × 10^?4–3 × 10^?3 s^?1. Microstructural stability of the FSP alloy is also studied in comparison to the AZ31, AZ61, and AZ91 alloys processed by various routes. High SR sensitivity in the range of 0.33–0.39 and grain size stability till 350 °C is observed for the FSP alloy. The FSP AZ91C alloy showed better thermal stability in comparison to AZ31 and AZ61 alloys. Kinetics of superplastic deformation of the FSP alloy is found to be slower as compared to AZ31 and AZ61 alloys processed by various routes, which is due to the presence of significant amount of second phase precipitates, such as, β-Mg₁₇(Al,Zn)₁₂, Mg₂Si, and Al₈Mn₅ in the FSP alloy. However, these precipitates contributed for better thermal stability of the microstructure of FSP AZ91C alloy.     

Development of high-performance quaternary LPSO Mg–Y–Zn–Al alloys by Disintegrated Melt Deposition technique

In the present study, new quaternary MgY_1.65Zn_0.74Al_0.53 and MgY_3.72Zn_1.96Al_0.45 alloys (wt.%) were synthesized employing the Disintegrated Melt Deposition (DMD) casting technique followed by hot extrusion. Microstructural characterization revealed the presence of 14H long-period stacking ordered structure (LPSO) and Mg₄Y₂ZnAl₃ phases aligned along the direction of extrusion in both alloys. Refined grains (⩽5 μm) due to the effect of dynamic recrystallization (DRX) were also observed to co-exist with larger worked grains (⩾20 μm) in the extruded microstructures. Compared to monolithic Mg, significant increase in the microhardness (∼67–88%), tensile yield strength (∼245–290%) and ultimate tensile strength (∼113–144%) were observed in the Mg–Y–Zn–Al alloys. Despite the significant increase in strength of materials, failure strains of both Mg–Y–Zn–Al alloys were comparable to monolithic Mg. Ignition temperatures of both Mg–Y–Zn–Al alloys were found to outperform commercially available AZ31, AZ80 and WE43 (high-temperature) Mg alloys, and the highest ignition temperature of 770 °C was achieved in the MgY_3.72Zn_1.96Al_0.45 alloy.     

Microstructure of MgAl5Ca3Sr alloy after creep deformation and high‐temperature heat treatment

The paper presents results of microstructural investigations of MgAl5Ca3Sr magnesium alloys in the as‐cast condition, after creep tests at 180 °C, and after heat treatment at 450 °C for 4.5 hours. The microstructure of MgAl5Ca3Sr alloy is composed of α‐Mg solid solution, irregular shaped (Mg,Al)₂Ca phase with C36 crystal structure, bulky (Mg,Al)₁₇(Sr,Ca)₂ phase, fine lamellar Mg₂Ca phase with C14 structure, needle‐shaped Al₂Ca precipitates with the C15 crystal structure. The precipitation of the needle‐shaped Al₂Ca phase in the α‐Mg grains and spheroidization of the C14 phase were found after heat treatment at 450 °C in argon atmosphere. The (Mg,Al)₂Ca (C36) and (Mg,Al)₁₇(Sr,Ca)₂ phases seems to be stable at 450 °C, however, the increasing of aluminum content in C36 compound was observed suggesting the initial stage of C36 → C15 transformation. After creep deformation at 180 °C precipitates of the Al₂Ca phase were found in α‐Mg phase. The intermetallic compounds are stable at 180 °C. The MgAl5Ca3Sr alloy exhibits good creep resistance up to 75 MPa. Tensile properties are comparable to those of Mg‐RE‐Zn–Zr alloys.     

Structural characteristics and elevated temperature mechanical properties of AJ62 Mg alloy

Structure and mechanical properties of the novel casting AJ62 (Mg–6Al–2Sr) alloy developed for elevated temperature applications were studied. The AJ62 alloy was compared to commercial casting AZ91 (Mg–9Al–1Zn) and WE43 (Mg–4Y–3RE) alloys. The structure was examined by scanning electron microscopy, x-ray diffraction and energy dispersive spectrometry. Mechanical properties were characterized by Viskers hardness measurements in the as-cast state and after a long-term heat treatment at 250 °C/150 hours. Compressive mechanical tests were also carried out both at room and elevated temperatures. Compressive creep tests were conducted at a temperature of 250 °C and compressive stresses of 60, 100 and 140 MPa. The structure of the AJ62 alloy consisted of primary α-Mg dendrites and interdendritic nework of the Al₄Sr and massive Al₃Mg₁₃Sr phases. By increasing the cooling rate during solidification from 10 and 120 K/s the average dendrite arm thickness decreased from 18 to 5 μm and the total volume fraction of the interdendritic phases from 20% to 30%. Both factors slightly increased hardness and compressive strength. The room temperature compressive strength and hardness of the alloy solidified at 30 K/s were 298 MPa and 50 HV 5, i.e. similar to those of the as-cast WE43 alloy and lower than those of the AZ91 alloy. At 250 °C the compressive strength of the AJ62 alloy decreased by 50 MPa, whereas those of the AZ91 and WE43 alloys by 100 and 20 MPa, respectively. The creep rate of the AJ62 alloy was higher than that of the WE43 alloy, but significantly lower in comparison with the AZ91 alloy. Different thermal stabilities of the alloys were discussed and related to structural changes during elevated temperature expositions.     

Grain refinement of Mg–Al alloys with Al4C3–SiC/Al master alloy

A novel Al₄C₃–SiC/Al master alloy for grain refinement of Mg–Al–Zn alloys has been developed in the present work. X-ray diffraction (XRD) and electron probe microanalysis (EPMA) results show the existence of Al₄C₃ and SiC particles in this master alloy. The master alloy presents good grain refining efficiency on both AZ31 and AZ63 alloys, but little effect on AZ91 alloy. After addition of 0.5 wt.% Al₄C₃–SiC/Al master alloy, the average grain size of AZ31 and AZ63 decreased dramatically from 1300 to 225 μm, and from 300 to 200 μm, respectively. However, no further refinement of grain size was achieved with additional amount of Al₄C₃–SiC/Al master alloy exceeding 0.5 wt.% for both AZ31 and AZ63 alloys in the present investigation. Duplex phase of Al₄C₃ and SiC was found to be located at the grain center of α-Mg and is proposed to be the nucleating agent during solidification of α-Mg.     

Influence of neodymium on microstructure and mechanical properties of AZ31B wrought magnesium alloy

Abstract

The influences of rare earth neodymium on microstructure and mechanical properties of as cast and hot rolled AZ31B wrought magnesium alloy were investigated. The results show that the mechanical properties of both as cast and hot rolled AZ31B alloys decrease due to Nd addition. Nd reacts with Al to form Al₂Nd phase when Nd is added. Bulky and brittle Al₂Nd intermetallic degrades the mechanical properties. Moreover, the addition of Nd weakens the grain refining effect of Al on as cast AZ31B alloy, resulting in grain coarsening. Coarse grains also cause the decline of the mechanical properties of as cast AZ31B–Nd alloy. The negative influence of the bulky and brittle intermetallics on mechanical properties of AZ31B alloy can be relieved by large deformation because the intermetallics can be sufficiently broken up during the deformation process.     

Structure and mechanical properties of rapidly solidified magnesium based Mg-Al-Zn-RE alloys consolidated by extrusion

Magnesium based Mg-9Al-lZn-5RE (RE = La or Nd) alloys were rapidly solidified by chill block melt spinning. The resulting ribbons were cold packed into an aluminium alloy can and extruded at temperatures of 230 and 340°C and ratios of 20:1 or 25:1. Tensile and hardness tests of the extruded and heat treated materials were carried out. The tensile strength and elongation to fracture of the as extruded material were 478 MN m^?2 and 6·5% respectively and those of the material heat treated for 2 h at 350° C were 420 MN m^?2 and 20% respectively. The microstructure of these specimens was studied by X-ray diffraction and transmission electron microscopy. Intermetallics of Al₁₁ La₃ or Al₂Nd were found at grain boundaries and in the matrix which had a grain size of between 0–26 and 0–8 μm, while Mg₁₇Al₁₂ precipitates were present in the specimens extruded at a lower temperature (230° C). Yield strengths were consistent with the Hall-Petch relationship with grain size established earlier for this class of material.

MST/3495     

Effects of neodymium rich rare earth elements on microstructure and mechanical properties of as cast AZ31 magnesium alloy

Abstract

The effects of neodymium rich rare earth elements [RE(Nd)] on microstructure and mechanical properties of as cast AZ31 magnesium alloy were investigated. The microstructures of as cast AZ31–xRE(Nd) alloys display a dendrite configuration, and the secondary dendrite spacing of the α-Mg phase was decreased with the increasing Nd content. The addition of RE(Nd) resulted in the formation of Al₂Nd and Mg₁₂Nd phases. Mechanical properties were improved significantly due to grain refinement and precipitation of intermetallic phases. When the amount of RE is 1·0 wt-%,The as cast AZ31 alloy reached its maximum tensile strength of 249 MPa at room temperature, yield strength of 169 MPa and elongation of 9·0%.     

Effect of Homogenization Process on Microstructure of Al–Zn–Mg–Cu Aluminum Alloys

Herein, the best homogenization process of 466.5 °C × 36 h + 490 °C × (14–26.4 h) that can completely eliminate the coarse phases σ[Mg(Zn, Al, Cu)₂] and S(Al₂CuMg) in the Al–Zn–Mg–Cu aluminum alloy is developed. The homogenization process is determined by the method of calculation phase diagram, and the experimental verification. It is shown in the results that, first, in the microstructure of the as-cast alloys, the crystal structure of the σ[Mg(Zn, Al, Cu)₂], Al₇Cu₂Fe, and Mg₂Si phases is determined. Second, during the homogenization process, the σ[Mg(Zn, Al, Cu)₂] phase dissolves and also transforms into the S(Al₂CuMg) phase. Most importantly, the dissolution temperature range of the σ[Mg(Zn, Al, Cu)₂], S(Al₂CuMg), and Al₇Cu₂Fe phases is determined from 472.56 to 476.36 °C, from 484.09 to 485.39 °C, and from 540.18 to 547.23 °C, respectively. At best homogenization process, the residual Al₇Cu₂Fe phase area fraction ranges from 1.28 ± 0.16% to 1.60 ± 0.18%. In addition, dispersed η(MgZn₂) phase precipitates in supersaturated Al-matrix during differential scanning calorimeter heating. And, the concentration differences between the grain center and the eutectic of structure of Zn, Mg and Cu regression equations are established, which can provide some reference for the design of experimental parameters, thus reducing the experimental workload.     

Development of ternary Mg based alloy for soldering of AZ31B magnesium alloy

Abstract

Two kinds of ternary Mg based alloys were designed to join the AZ31B magnesium alloy plates by high frequency induction soldering with argon shielding gas. The microstructures and properties of the filler metals and joints were investigated by SEM, X-ray diffraction, differential scanning calorimetry, spreading test and tensile test. The results have shown that the microstructures of Mg–31·5Al–10Sn filler metal mainly consist of Mg₁₇Al₁₂, Mg₂Sn and a trace amount of α-Mg phases, while the microstructures of Mg–29·5Zn–1Sn filler metal include α-Mg phase and Mg₇Zn₃ with a trace of α-Mg and Mg₂Sn phases. Both of the filler metals have narrow melting zones; however, the spreading area of the Mg–31·5Al–10Sn filler metal is much larger than that of the Mg–29·5Zn–1Sn filler metal on the AZ31B base metal. The average tensile strength of solder joints with Mg–31·5Al–10Sn filler metal is a little higher than that of the latter solder joints with Mg–29·5Zn–1Sn filler metal.     

Comparison of superplastic forming abilities of as‐cast AZ91 magnesium alloy prepared by twin roll casting and WE43 magnesium alloy

This paper describes and compares the superplastic behaviour and microstructural evolution of twin roll cast AZ91 and WE43 rolled sheet alloys. Tests were carried out in uniaxial tension on both alloys across a range of temperatures (300 °C–525 °C) and strain rates (1?10^‐4 s^‐1–1?10^‐1 s^‐1). In the case of WE43 gas bulge testing was employed at 400 °C and 0.6 MPa to offer a better analogy to superplastic forming than uniaxial tensile testing. Elongations of over 400 % were observed within WE43 when tested at 450 °C and 1?10^‐3 s^‐1 strain rate, and over 200 % within AZ91 when tested at 350 °C and 1?10^‐3 s^‐1 strain rate. A peak cone height of 41 mm was achieved with WE43 at a temperature of 400 °C and pressure of 0.6 MPa. Electron back scattered detection technique was employed to analyse the microstructural evolution of the two alloys during the forming process. Both WE43 and AZ91 were observed to undergo dynamic recrystallization during elevated temperature tensile testing and failed at low strain rates mainly by means of coalescence of cavitation, in the case of AZ91 at high strain rates cracking of Al₁₂Mg₁₇ intermetallic particles was the dominating failure mechanism. Both alloys were seen to achieve good levels of superplastic ductility over 200 % elongation, which would be industrially useful in niche vehicle and aerospace manufacturing.     

Phase transformations in Al–Mg–Zn alloys during high pressure torsion and subsequent heating

The structure, phase composition, and their thermal evolution were studied in case of ternary Al–Zn–Mg alloys before and after high-pressure torsion (HPT) in Bridgman anvils. The as-cast non-deformed alloys contained the fine particles of Mg₃₂(Al,Zn)₄₉ (τ phase), MgZn₂ (η phase), AlMg₄Zn₁₁ (η′ phase), and Mg₇Zn₃ phases embedded in the matrix of Al-based solid solution. During heating in differential scanning calorimeter (DSC), all these phases dissolved around 148 °C. The τ nanoparticles coherent with (Al) matrix-formed instead around 222 °C. HPT of the as-cast alloys strongly refined the grains of (Al) solid solution from 500 μm to 120–150 nm. The particles of τ, η, η′, and Mg₇Zn₃ phases fully dissolved in the (Al) matrix. During the following DSC-heating, particles of η phase appeared and grew. Their amount became maximal around 166 °C. The growth of η phase in the fine-grained HPT-treated alloys instead of τ phase in the coarse-grained ones is explained by the shift of the (Al) + η/(Al) + η + τ/(Al) + τ lines in the Al–Zn–Mg ternary phase diagram due to the grain boundary (GB) adsorption. At 166 °C the η phase formed the continuous flat layers in numerous (Al)/(Al) GBs. This corresponds to the complete GB wetting by the η phase. Other (Al)/(Al) GBs contain separated lenticular η particles (incomplete GB wetting). Increasing the temperature from 166 to 320 °C led to the disappearance of the completely wetted (Al)/(Al) GBs. In other words, the transition from complete to the incomplete wetting of (Al)/(Al) GBs by the η phase proceeds between 166 °C and 320 °C.     

Microstructure and mechanical properties of as aged Mg–3Sn–1Al and Mg–3Sn–2Zn–1Al alloy

Effect of Zn on the microstructure, age hardening response and mechanical properties of Mg–3Sn–1Al alloy which is immediately aged at 180°C after extrusion process (T5) was investigated. It was found that the Zn can refine the microstructure, remarkably improve the aging response with the peak hardness increases to 75 HV and the time to peak hardness reduces from ～110 to ～60 h, which is attributed to the solid solution hardening of Al, Zn and an amount of finer Mg₂Sn precipitates. The as aged Mg–3Sn–2Zn–1Al alloy exhibits better mechanical property at room temperature or 150°C than that of Mg–3Sn–1Al alloy, which is ascribed to the fine grained microstructure and thermally stable Mg₂Sn particles dispersed at grain boundaries and in the matrix.     

Non-isothermal aging of a high-Zn-containing Al–Zn–Mg–Cu alloy: microstructure and mechanical properties

The non-isothermal aging behaviour of a newly developed Al–Zn–Mg–Cu alloy containing 17?wt-% Zn was investigated. Hardness and shear punch tests demonstrated that during non-isothermal aging, the mechanical properties of the alloy first increased and then decreased. The best properties were obtained in a sample which was non-isothermally aged upto 250°C with heating rate of 20°C?min^?1, due to the presence of η′/η (MgZn₂) phases. This was confirmed by differential scanning calorimetery. After homogenisation, residual eutectic phases remained at triple junctions or in a spherical form. During aging, these phases transformed into rodlike S (Al₂CuMg)-phase at 400°C, with sizes ranging from 50 to 250?nm. The precipitation sequence in this high-Zn alloy was similar to that for conventional Al–Zn–Mg–Cu alloys.     

Formation of intermetallic compounds in Mg–Ag–Al joints during diffusion bonding

In this study, we conducted the diffusion bonding of Mg and Al alloys using a 30-μm-thick pure silver foil interlayer at median temperatures between 390 and 490 °C. We obtained a multilayered structure across the Mg–Ag–Al joint: Mg/Mg(ss, Ag)/Mg₃Ag/MgAg/Ag/Ag(ss, Al)/Ag₂Al/Al. The silver diffusion barrier prevented the formation of brittle intermetallics between Mg and Al. Intermetallics identified at the joint interface include the more ductile types between Mg and Ag, ε-Mg₃Ag and β′-MgAg, and Ag and Al, δ-Ag₂Al. As the bonding temperature increased, Ag₂Al, followed by MgAg, favored the growth of Mg₃Ag IMC layer. The shear strength of the joints increased with the rising bonding temperature to a maximum value of 11.8 MPa at 470 °C. Fracture failure in the joints mainly occurred in the Ag₂Al layer. The formation mechanism for interfacial layers in the joints is believed to consist of four stages: (1) solid-solution formation, (2) Mg–Ag IMC formation, (3) Ag–Al IMC formation, and (4) growth of Mg–Ag and Ag–Al IMCs.     

Wrapping effect of secondary phases on the grains: increased corrosion resistance of Mg–Al alloys

The discrete secondary phases usually cause severe galvanic corrosion, thereby resulting in rapid degradation for Mg–Al alloys in orthopaedics application. In this study, CaO was introduced into Mg–Al–Zn (AZ61) alloy via selective laser melting (SLM) to ameliorate the characterisations of the secondary phases, with an aim to improve its corrosion behaviour. Results revealed that CaO reacted with Mg and Al in Mg–Al alloys during SLM, suppressing the formation of coarse Mg₁₇Al₁₂ phase and promoting the formation of (Mg, Al)₂Ca phase. Meanwhile, the rapid solidification during SLM promoted the homogeneous precipitation of the second phase. As a result, inert (Mg, Al)₂Ca phase homogeneously wrapped the Mg grains, which effectively protected them from the invasion of corrosion solution. Thus, the degradation rate was remarkably reduced from 0.073 to 0.031?mg?cm^–2?h^–1. Furthermore, AZ61-9CaO exhibited good cytocompatibility. This work suggested that AZ61-9CaO was promising candidates for orthopaedics implants.     

Effects of rare earth additions on structures and properties of rapidly solidified copper alloys

Abstract

Copper based Cu–RE alloys (where RE represents lanthanum, neodymium, or samarium) with alloying content up to 16 wt-% were prepared by chill block melt spinning into ribbons of thickness between 40 and 100 μm. The melt spun ribbons were heat treated isochronally for 2 h at 300, 400, 500, 600, 700, and 800°C, respectively. The melt spun and heat treated ribbons were tested for microhardness and resistivity and were characterised by optical and transmission electron microscopy (TEM) and X-ray diffractometry (XRD). Microstructures were of the typical zone B type for Cu–1RE and Cu–3RE ribbons and of the zone B/zone A type for Cu–5RE, Cu–8RE, and Cu–12RE ribbons. Only microstructures of the zone A type were found in Cu–15La ribbons. The metastable extended solid solubilities of the rare earth elements were evaluated by measurements of the lattice parameters of the supersaturated solid solutions and significant extension from the equilibrium solid solubility was found for all three alloys. The secondary phase was identified by TEM and XRD as Cu₆RE for all ribbons except Cu–15La ribbons in which metastable Cu₅La and Cu₁₃La phases were also found. Observations using TEM and XRD also showed a reduction in the α-Cu grain size of the as spun ribbons with increasing alloying content, producing nanosized α-Cu grains on the chill side of the ribbons. Heat treatment of the ribbons at 400°C for 2 h produced no significant coarsening of α-Cu grains as the size of these grains was still in the nanometer region. Both α-Cu and Cu₆RE grains coarsened as a result of heat treatment for 2 h at temperatures of 600°C and above for all the alloys.