Grain refinement of magnesium alloys

The literature on grain refinement of magnesium alloys is reviewed with regard to two broad groups of alloys: alloys that contain aluminum and alloys that do not contain aluminum. The alloys that are free of aluminum are generally very well refined by Zr master alloys. On the other hand, the understanding of grain refinement in aluminum bearing alloys is poor and in many cases confusing probably due to the interaction between impurity elements and aluminum in affecting the potency of nucleant particles. A grain refinement model that was developed for aluminum alloys is presented, which takes into account both alloy chemistry and nucleant particle potency. This model is applied to experimental data for a range of magnesium alloys. It is shown that by using this analytical approach, new information on the refinement of magnesium alloys is obtained as well as providing a method of characterizing the effectiveness of new refiners. The new information revealed by the model has identified new directions for further research. Future research needs to focus on gaining a better understanding of the detailed mechanisms by which refinement occurs and gathering data to improve our ability to predict grain refinement for particular combinations of alloy and impurity chemistry and nucleant particles. This article is based on a presentation made in the symposium entitled “Phase Transformations and Deformation in Magnesium Alloys,” which occurred during the Spring TMS meeting, March 14–17, 2004, in Charlotte, NC, under the auspices of ASM-MSCTS Phase Transformations Committee.     

Resistance to shape refinement of precipitates in Al-(Si,Ge) alloys during thermal cycling

The present work addresses the response of Si-Ge precipitates in Al-0.5Si-0.5Ge (at. pct) to thermalcycling treatments of the sort known to refine the shapes of Ge precipitates in binary Al-Ge alloys. Alloys aged at 250 °C contained both small, platelet precipitates on {111} planes and larger, equiaxed precipitates that were heavily twinned. Thermal cycling between 250 °C and 360 °C led to partial or complete dissolution of the platelets. However, the equiaxed particles coarsened at an essentially constant shape; the shape refinement that led to untwinned, single-variant octahedral precipitates in binary Al-Ge did not occur. The apparent reason is the heavy twinning of the Si-Ge precipitates, which produces particles with a nearly spherical shape and rounded, incoherent interfaces and is, hence, a viable mechanism for relaxing the large misfit strain of the precipitate structure. The twinned particles undergo normal coarsening at an essentially constant shape. After thermal cycling, the precipitates contain Si and Ge in the approximate ratio of 70Si-30Ge, which is in the composition range expected for the cycling temperature.     

Phase transformation during annealing of rapidly solidified Al- rich Al- Fe- Si alloys

Thermal decomposition of rapidly solidified microstructure of three Al-Fe-Si alloys (Al-10,12, 14Fe-2Si wt pct) has been studied by DTA and TEM. The initial microstructure consists mostly of aluminum and a smaller volume fraction of an amorphous phase. During heating the amorphous phase first transforms to the metastable α(AlFeSi) cubic phase (Im ,a = 1.25 nm) at ∼ 380°C. At higher temperature ∼ 430 °C the α(AlFeSi) phase transforms by ordering to a trigonal phase (two modifications, α′ and α ″,were found). The crystallography of the α′(AlFeSi) and α″(AlFeSi) phases is analyzed using selected area and convergent beam electron diffraction technique.     

Grain refinement in magnetically stirred GTA welds of aluminum alloys

The mechanisms of grain refinement have been examined for magnetically stirred gas tungsten arc (GTA) welds completely penetrating thin sheets of several aluminum alloys. Grain refinement in unstirred welds may be brought about by adding sufficient titanium to produce heterogeneous nucleation by Ti-rich particles. In some alloys magnetic stirring is shown to extend the range of welding conditions which produce a partially equiaxed structure, and to widen the equiaxed fraction of partially equiaxed welds. This is attributed to magnetic stirring lowering the temperature gradient, allowing nucleation and growth of Al-rich grains further ahead of the columnar interface growing in from the fusion boundaries. In alloys with low Ti levels, magnetic stirring may cause refinement by sweeping grains from the partially molten zone ahead of the advancing solidification interface. This mechanism requires that the partially molten zone be sufficiently wide, and that the grain size in this zone remain small.     

Oxidation of Fe-7Cr-12Ni-(0-6)Al-(0-7)Si alloys

A series of Fe-7Cr-12Ni-(0-6)Al-(0-7)Si alloys was oxidized at test temperatures between 800° and 1000 °C. The master alloy, Fe-7Cr-12Ni, had no oxidation resistance at temperatures above 800 °C. Aluminum additions to the master alloy produced a protective A1₂O₃ layer over the substrate metal which prevented rapid oxidation and allowed time for a Cr₂O₃ layer to develop underneath. Silicon addition to the master alloy produced an SiO₂ oxide sublayer at the metal-oxide interface which, when formed, provided an effective barrier to oxidation. A combination of 1.5-pct-Al and 2.0-pct-Si additions provided the best oxidation protection.     

Zr在Mg-9Gd-4Y合金中的晶粒细化机制

研究了不同Zr含量对Mg-9Gd-4Y合金晶粒大小的影响及Zr的晶粒细化机制．结果表明,Zr可以明显细化合金的晶粒,且随Zr含量增加,晶粒变得更细小．微观组织分析表明,在Zr含量较高的合金中,几乎每个晶粒内都含有至少一个富Zr的核;而在Zr含量较低的合金中没有发现这种核．在高Zr含量和低Zr含量的合金中,晶粒细化的机制不同：在低Zr含量合金中,Zr以抑制品粒长大为主;在高Zr含量合金中,Zr以促进异质形核为主．     

The grain refinement of zinc-aluminum alloys by titanium

Abstract

The effect of small additions of titanium in the range 0?0.5 wt% on the primary α′ aluminum grain size in Zn–Al alloys containing 7 and 24 wt% Al has been examined. Marked refinement of the α′. phase was associated with the occurrence of small cubic particles in the microstructure. Electron microprobe and electron diffraction analysis showed that the particles were Al₅Ti₂Zn with a simple cubic symmetry, a = 3.99 ± 0.04Å. In the refined alloys the primary aluminum grains were “non-dendritic” and this morphology has been discussed in relation to the effectiveness of the particles as nuclei and the theory of predendritic solidification.

Additions of not less than 0.04 wt% of titanium to Zn-Al alloys containing 7 to 24 wt% Al are sufficient for complete grain refinement of the primary aluminum phase.

Résumé

Les auteurs ont étudié l'influence de faibles additions de titane (0-0.5% poids) sur la taille des grains d'aluminium (α′ primaire) des alliages Zn–Al. Un affinement marqué de la phase α′. est obtenu lorsqu'il y a présence de petites particules cubiques dans la microstructure. Des analyses à la microsonde et par diffraction électronique révèlent que ces particules sont composées de Al₅Ti₂Zn ayant une structure cubique simple (a = 3.99 ± 0.04Å). Dans les alliages á grains affmés, ces derniers sont “non?dentritiques” et cette morphologie est discutée à la lumiére de l'éfficacité des particules qui agissent comme germes et de la théorie de la solidification pré-dendritique.

Des additions d'au moins 0.04% poids de titane aux alliages Zn-Al, contenant de 7 à 24% poids d'aluminium, sont suffisantes pour obtenir un affinement complet du grain de la phase prima ire riche en aluminium.     

Relationship between fracture toughness and crack extension resistance curves (R curves) for Ti-6Al-4V alloys

The effects of microstructure, impurity content, and testing temperature on the fracture toughness (as measured by the crack tip opening displacement (CTOD)) and microcrack extension resistance curves (R curves) of Ti-6Al-4V alloys were examined. At 0 °C, microstructure is the most influential factor in the toughness-strength relationship. Acicular microstructure specimens have a higher CTOD than specimens with equiaxed microstructures, regardless of strength (0.2 pct proof stress) and impurity content. At −196 °C, impurity content becomes a controlling factor in the toughness-strength relationship. Extra-low impurity (ELI) specimens, which have a lower impurity content, show a higher CTOD, irrespective of microstructure. Microcracks extended from the notch tip before the maximum load was reached during testing were investigated, and crack initiation (δ _i) and extension-resistance properties were evaluated by obtaining exact R curves of the microcracks. At 0 °C, specimens with different microstructures and different impurity contents have almost the same δ _i. But acicular-microstructure specimens with a higher CTOD at a given strength show a greater crack extension resistance. At −196 °C, ELI specimens, which have a higher CTOD, show a larger crack extension resistance. It is concluded that the crack extension-resistance property of the microcracks extended from the notch tip before the maximum load is a controlling factor for the fracture toughness of Ti-6Al-4V alloys.     

Grain refinement of copper by the addition of iron and by electromagnetic stirring

The effect of iron additions in the range of 0.57 to 7.5 wt pet on the grain size of electromagnetically levitated copper-iron alloys was investigated. The samples were solidified while levitated or quenched in water from the molten state. The addition of iron was found to be effective in reducing the grain size of copper, and the average grain size decreased as the iron content was increased up to the peritectic liquid composition of about 2.8 wt pet Fe. Beyond this composition, the grain size of the samples solidified in the levitated state was insensitive to the iron content, whereas that of the quenched samples continuously decreased with increasing iron content. The results indicate that electromagnetic stirring causes fragmentation of copper dendrites in the hypoperitectic region, and hence enhances grain refinement. In the hyperperitectic region, on the other hand, the stirring has a detrimental effect on the grain refinement by agglomerating the primary iron particles which act as heterogeneous nucleation sites for the copper matrix.     

Equal-channel angular pressing of commercial aluminum alloys: Grain refinement, thermal stability and tensile properties

Using equal-channel angular (ECA) pressing at room temperature, the grain sizes of six different commercial aluminum-based alloys (1100, 2024, 3004, 5083, 6061, and 7075) were reduced to within the submicrometer range. These grains were reasonably stable up to annealing temperatures of ∼200 °C and the submicrometer grains were retained in the 2024 and 7075 alloys to annealing temperatures of 300 °C. Tensile testing after ECA pressing through a single pass, equivalent to the introduction of a strain of ∼1, showed there is a significant increase in the values of the 0.2 pct proof stress and the ultimate tensile stress (UTS) for each alloy with a corresponding reduction in the elongations to failure. It is demonstrated that the magnitudes of these stresses scale with the square root of the Mg content in each alloy. Similar values for the proof stresses and the UTS were attained at the same equivalent strains in samples subjected to cold rolling, but the elongations to failure were higher after ECA pressing to equivalent strains >1 because of the introduction of a very small grain size. Detailed results for the 1100 and 3004 alloys show good agreement with the standard Hall-Petch relationship.     

Solidification behavior,microstructure and silicon twinning of Al-10Si alloys with ytterbium addition

The solidification behavior, micro structure and silicon twinning of Al-10 Si alloys with Yb addition were investigated by thermal analysis, optical microscopy, X-ray diffraction. scanning electron microscopy, and transmission electron microscopy. The results indicate that the nucleation temperature, minimum temperature, and growth temperature of Al-lOSi alloys decrease with increasing Yb content. The cooling curves of the Yb-modified alloys exhibit marked recalescence. The recalescence of the modified alloy peaks at 2.3 ℃ when the Yb content is 0.7 wt%. The 3 D morphologies of eutectic Si in Yb-modified alloys change from a coarse plate-like structure to a honeycomb structure with many fine fibrous structures.The Al-Si-Yb intermetallic compound is observed in the 1.0 wt% Yb-modified alloy. Meanwhile, XRD analysis and TEM results indicate that the average twin spacing in the Yb-modified alloys is 18-46.2 nm.The average twin spacing of eutectic Si decreases with increasing Yb content. When the Yb content in the modified alloy is increased to 0.7 wt%, the average twin spacing value of eutectic Si reaches to 18 nm,which promotes the formation of twins and refinement of eutectic Si.     

Al—3B中间合金的加工量对亚共晶Al—Si合金晶粒细化的影响

研究了Al-3B中间合金不同的加入量对亚共晶Al-Si合金晶粒尺寸的影响。该中间合金对所研究全部范围内的Al-Si合金都具有一定的细化效果,但在不同的含硅量下其细化能力并不相同,同时证实对未经细化处理的亚共晶Al-Si合金而言,在含硅量约3%（质量分数,下同）时合金具有最小的晶粒尺寸。随着Al-3B中间合金加入量的提高,出现最小晶粒尺寸的合成成分向高硅方向移动,当加入量达到1%时,在含硅量为6%的Al-Si合金中出现最小的晶粒尺寸。     

Calorimetric evaluation of nonequilibrium state in as-melt spun Al-1.72 and Al-3.12 At. Pct Cu Alloys and Al-6.74, Al-8.48, and Al-11.97 At. Pct Si alloys

Formerly Graduate Student, Graduate School of Engineering, Osaka University, Suita Osaka 565, Japan     

铝合金等通道挤压晶粒细化机制

本文讨论铝合金在等通道挤压过程中的晶粒细化机制。发生的晶粒细化主要通过三种机制完成：1)取向分裂诱发形变带;2)应变集中产生的宏观或微观剪切带;3)高角度晶界随应变增加。形变条件和路径、模具几何及材料参数决定形变组织的演化。亚结构和显微剪切带的取向与模具剪切面一致但在原则上与材料的晶体位错滑移系统无关。形变带的晶体取向倾向接近在路径A下稳定织构的取向。在高应变,由于显微组织的压缩和拉长造成的晶界面积增加成为主要晶粒细化机制。变形至一定应变后,形变进入稳态,晶粒细化不再发生。     

Al-7Si Alloy Directional Solidification With the Application of a Pulsed Magnetic Field

An experiment on the directional solidification of Al-7Si alloys under the influence of a pulsed magnetic field(PMF)is performed.Maximal peak value of PMF intensity up to 0.226 T between two iron cores was generated when a capacitor bank of 120μF capacitance with initial voltage of 1000 V was triggered to a pair of solenoids.The PMF decreases the temperature gradient ahead of the liquidus front and increases the width of the mushy zone.In this paper,using Darcy’s permeability law and Lehrnann’s model,the order of magnitude of the interdendritic liquid flow velocities with the application of PMF is evaluated.     

Microstructure and Properties of the Al-27Si/Cu/Al-50Si Joint Brazed by the Partial Transient Liquid Phase Bonding

Al-27Si and Al-50Si were brazed by using a thin Cu interlayer. The metallurgical bonding without obvious defects is achieved, and a wide brazing seam consisting of fine eutectic structures and coarse Si particles is formed in the Al-27Si/Cu/Al-50Si joint. The deposition of Si element in the liquid phases during solidification results in the formation of the larger Si particles and ultra-small Si particles in the brazing seam. The shear strength of the joint reaches 63 MPa.     

Effect of cooling rate on the solidification Behavior of Al-7 Pct Si-SiCp Metal-Matrix Composites

The solidification behavior of two composites based on Al-Si alloy has been investigated as a function of cooling rate. Thermal analysis techniques have been used to establish the relationship between solidification history and the microstructure developed. The results of thermal analysis show that the characteristic parameters are influenced by the cooling rate. A marked difference in these parameters is observed between the reinforced and the unreinforced materials at all cooling rates studied. The cooling rates used in the present study range from 0.3 to 20 K/s. Increasing the cooling rate is shown to affect the undercooling parameters both in the liquidus and eutectic solidification region. The eutectic growth temperature of the composites is observed to be higher than that of the base alloy at all cooling rates. The depression in eutectic temperature ΔT is found to decrease by 27 K for the unreinforced alloy (A356) and by 17 K for the com- posites (A356 + 10, 20 vol pct SiC) at a higher cooling rate of ≃16 K/s. The presence of SiC reinforcement is observed to suppress the Mg₂Si precipitate formation and decrease the amount of heat liberated during both primary and eutectic phase formation. Dendrite arm spacing (DAS) is correlated to the cooling rate by a relationship of the form DAS =A(T) ^-n, wheren is found to be of the order of 0.33.