Microstructure evolution during homogenization of Al–Mn–Fe–Si alloys: Modeling and experimental results

Microstructure evolution during the homogenization heat treatment of Al–Mn–Fe–Si, or AA3xxx, alloys has been investigated using a combination of modeling and experimental studies. The model is fully coupled to CALculation PHAse Diagram (CALPHAD) software and has explicitly taken into account the two different length scales for diffusion encountered in modeling the homogenization process. The model is able to predict the evolution of all the important microstructural features during homogenization, including the inhomogeneous spatial distribution of dispersoids and alloying elements in solution, the dispersoid number density and the size distribution, and the type and fraction of intergranular constituent particles. Experiments were conducted using four direct chill (DC) cast AA3xxx alloys subjected to various homogenization treatments. The resulting microstructures were then characterized using a range of characterization techniques, including optical and electron microscopy, electron micro probe analysis, field emission gun scanning electron microscopy, and electrical resistivity measurements. The model predictions have been compared with the experimental measurements to validate the model. Further, it has been demonstrated that the validated model is able to predict the effects of alloying elements (e.g. Si and Mn) on microstructure evolution. It is concluded that the model provides a time and cost effective tool in optimizing and designing industrial AA3xxx alloy chemistries and homogenization heat treatments.     

Microstructure evolution during homogenization of Al-Mg-Si-Mn-Fe alloys: Modelling and experimental results

Microstructure evolution during the homogenization heat treatment of an Al-Mg-Si-Fe-Mn (AA6xxx) alloy was investigated using a combination of modelling and experimental studies. The model is based on the CALPHAD-coupled homogenization heat treatment model originally developed for AA3xxx alloys (i.e., Al-Mn-Fe-Si). In this work, the model was adapted to the more complex AA6xxx system (Al-Mg-Si-Mn-Fe) to predict the evolution of critical microstructural features such as the spatial distribution of solute, the type and fraction of constituent particles and dispersoid number density and size distribution. Experiments were also conducted using three direct chill (DC) cast AA6xxx alloys with different Mn levels subjected to various homogenization treatments. The resulting microstructures were characterized using a range of techniques including scanning electron microscopy, electron microprobe analysis (EPMA), XRD, and electrical resistivity measurements. The model predictions were compared with the experimental measurements, and reasonable agreement was found.     

Phase-field modelling of as-cast microstructure evolution in nickel-based superalloys

A modelling approach is presented for the prediction of microstructure evolution during directional solidification of nickel-based superalloys. A phase-field model is coupled to CALPHAD thermodynamic and kinetic (diffusion) databases, so that a multicomponent alloy representative of those used in industrial practice can be handled. Dendritic growth and the formation of interdendritic phases in an isothermal (2-D) cross-section are simulated for a range of solidification parameters. The sensitivity of the model to changes in the solidification input parameters is investigated. It is demonstrated that the predicted patterns of microsegregation obtained from the simulations compare well to the experimental ones; moreover, an experimentally observed change in the solidification sequence is correctly predicted. The extension of the model to 3-D simulations is demonstrated. Simulations of the homogenization of the as-cast structure during heat treatment are presented.     

Modeling of precipitate-free zone formed upon homogenization in a multi-component alloy

A comprehensive model is presented for the simulation of microstructure evolution during industrial solidification and homogenization processing of aluminum alloys. The model combines on the one hand microsegregation due to long-range diffusion during solidification and subsequent heat treatment with, on the other hand, precipitation in the primary Al phase. The thermodynamic data are directly obtained from a CALPHAD (CALculation of PHAse Diagrams) approach to thermodynamic equilibrium in multicomponent systems. The model is applied to the prediction of structure and segregation evolutions in a 3003 aluminum alloy for typical industrial solidification and homogenization sequences. It is shown that: (i) accounting for the nucleation undercooling of the eutectic/peritectic structures solidifying from the melt is essential to retrieval of the measured volume fractions of intergranular precipitates; (ii) calculations of intragranular precipitation are generally not applicable if long-range diffusion is neglected; (iii) the precipitate-free zone can be quantitatively predicted only based on the coupling between intergranular and intragranular precipitation calculations.     

Statistical model for intergranular corrosion growth kinetics

A statistical model has been developed to predict the anisotropy of intergranular corrosion (IGC) kinetics and effect of microstructure on IGC kinetics in high strength AA2024-T3 alloys. The methodology is to estimate the statistical distribution of minimum IGC path length that will be found through the thickness of a given thickness ST sample using the principle of order statistics. A brick-wall model is adopted for wrought Al alloy microstructure and different distributions of grain dimension are assumed for the purpose of the estimation of total IGC path length. Numerical stimulation using a gamma distribution model stimulated the anisotropy of localized corrosion in AA2024-T3 alloys, which quite agrees with the growth rate anisotropy experimentally determined by the foil penetration technique. Some limitations regarding the statistical model are discussed. The statistical model provides a new approach to predicting and quantifying localized corrosion kinetics on basis of the alloy microstructure.     

均匀化处理对AA3003铝合金铸轧板再结晶组织的影响

采用光学显微镜、硬度仪、扫描电镜、双臂电桥等手段,研究了均匀化处理对AA3003铝合金铸轧板组织、析出相和再结晶温度的影响。结果表明,高温均匀化退火对AA3003铝合金的再结晶具有显著地促进作用。铸轧板经580℃均匀化退火5h,冷轧后合金的再结晶温度明显降低,并且再结晶后得到尺寸梯度很小的等轴晶组织。     

Effect of Zr, Mn and Sc additions on the grain size of Mg–Gd alloy

The effect of Zr, Mn and Mn + Sc additions on the grain size of Mg–10Gd alloy has been investigated and the grain refinement mechanisms are also suggested. The results reveal that the addition of Zr results in a significant grain refinement of as-cast Mg–10Gd alloy by generating nucleants. However, it cannot restrict grain growth during homogenization treatment at 520 °C, and completely loss the grain refining effect for extruded alloy sample. Mn has a negligible effect on grain size of as-cast Mg–10Gd alloy, but α-Mn particles precipitate during homogenization treatment, which helps to refine the grains of extruded alloy sample due to α-Mn particles restricting recrystallization grain growth during extrusion. Successful grain refinement can be obtained by the addition of Mn + Sc. It is effective to refine microstructure of as-cast Mg–10Gd alloy, inhibit grain growth during homogenization treatment and also have a significant grain refining effect on extruded Mg–10Gd alloy sample, which are ascribed to the precipitation of a large number of Mn₂Sc particles.     

脉冲电磁场下铝合金半连续铸造技术研究进展

利用脉冲电磁场引起的力效应、热效应及磁势能可显著改善铝合金半连续铸造组织性能,同时,脉冲电磁铸造技术在绿色生产、智能控制等方面紧密契合“低碳冶金”的国家战略要求。综述了脉冲电磁场在铸造晶粒细化、微观结构演变及析出物细化3方面的研究成果,分析了脉冲电磁场特性与材料相变的耦合机制,提出了脉冲电磁场控制凝固、析出相变组织的初步构想,以满足高性能铝合金的质量要求。着重介绍了基于理论指导开发的熔体表面脉冲电磁场技术及其在7XXX(φ203)、6XXX(φ380)、Al-Si(φ120)等多规格半连续铸造的工业实践,脉冲电磁场有望在今后铸造、热处理等多个冶金环节发挥更大作用。     

Role of Ca in hot compression behavior and microstructural stability of AlMg5 alloy during homogenization

Effects of a minor Ca addition on microstructural stability and dynamic restoration behavior of AlMg5 during hot deformation were investigated. They were studied using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), electron backscatter diffraction (EBSD) analyses and transmission electron microscopy (TEM). JMatPro package was used for simulation of the solidification path of the alloys. The results show that the addition of Ca does not affect the microstructure and hot compression behavior of the as-cast samples. However, it prevents the drastic grain growth during homogenization. It is found that coarse grains of Ca-free alloy promote the dynamic recovery and slow down the dynamic recrystallization during hot compression. Also, the particle stimulated nucleation is suggested as the main nucleation mechanism of new recrystallized grains for hot compressed Ca-free alloy. On the other hand, the microstructure of the hot compressed Ca-added alloy is greatly affected by the presence of Al₄Ca intermetallics. The formation of Al₄Ca phase is predicted by JMatPro and revealed by DSC, SEM and TEM studies. Finally, it is found that the presence of Al₄Ca precipitates on the grain boundaries of Ca-added alloy prevents the growth of α(Al) by Zener pinning effect and results in the stability of microstructure during homogenization.     

AA 7055铝合金时效析出强化模型

利用小角度X射线散射技术获得的系列定量信息,综合运用时效析出动力学理论和析出相切过、绕过强化机制,研究了AA 7055铝合金在120和160℃时效过程中的屈服强度演变模型。结果表明,在时效早期盘状析出相的盘面半径和半厚度均与t^1/2(t为时效时间)成线性关系;在时效后期,析出相尺寸则与t^1/3成线性关系。时效过程中析出相体积分数与t的变化关系遵循JMA (Johnson-Mehl-Avrami)型表达式。综合考虑了GPI区和η’相2类析出相对合金强度的贡献,并且分别考察了这2类析出相的模量强化机制和共格应变强化机制,最终建立了AA 7055铝合金在120和160℃时效过程中的屈服强度变化模型,确定了该合金时效过程中析出相与屈服强度之间的定量关系。     

7050铝合金铸锭均匀化过程中相的转变

介绍了7050铝合金半连续铸造铸锭的相组成,以及在均匀化过程中相的转变。说明了7050铝合金铸锭经470℃48h均匀化后仍有大量残留相存在的原因。     

Computation of the homogenization regime for aluminum alloy AA2219 on the basis of diffusion theory

An analytical evaluation of homogenization of aluminum alloy AA2219 with different grain sizes is performed. The homogenization parameters are computed with the use of diffusion laws and under the assumption that a low-melting eutectic can form in alloys of the Al-Cu system. With allowance for the difference in the grain sizes a two-stage homogenization regime is shown to be optimum for alloy AA2219.     

形变热处理对Cu-Ti-Fe-Sn合金组织与性能的影响

利用真空熔炼法制备了Cu-3Ti-0.2Fe-1Sn合金,通过均匀化退火、固溶+冷轧(变形量分别为40%、60%、80%)+450 ℃时效处理,研究了形变热处理对Cu-3Ti-0.2Fe-1Sn合金显微组织、导电率及硬度的影响。结果表明:真空熔炼制得的 Cu-3Ti-0.2Fe-1Sn合金铸态组织中含有大量的枝状晶组织,经固溶处理后组织中出现了晶粒长大;铸态合金的硬度和导电率分别为178.1 HV和10.85%IACS,固溶处理后硬度和导电率都相应降低,分别为102.7 HV和4.58%IACS。经过冷变形和时效处理后Cu-3Ti-0.2Fe-1Sn合金硬度明显提高,变形量为60%时,时效480 min时硬度达到峰值,合金硬度为310.2 HV,此时合金的导电率为18.59%IACS。     

均匀化处理Al-Mg-Mn合金的组织及热变形行为

研究了半连续水冷铸造方法制备的Al-Mg-Mn合金均匀化处理过程中显微组织的演变过程,同时采用 Gleeble-1500热模拟试验机对均匀化退火态合金的高温塑性变形行为进行了研究,分析了合金流变应力与变形温度和变形量之间的关系,并对合金变形过程中显微组织变化进行了探讨。结果表明,均匀化处理后原铸态合金中粗大的非平衡析出相逐渐溶解,变细、断裂,趋于球化,呈珠链状,数量减少。在热模拟变形过程中,475 ℃×15 h 均匀化退火态Al-Mg-Mn合金流变应力随着变形温度升高而降低;随着变形量增加,流变应力的峰值增大。随着变形温度升高,合金热变形组织首先发生缓慢的回复,位错密度降低,进而形成亚晶、出现再结晶晶粒组织特征。     

AA3104铝合金均匀化过程中的（Fe,Mn）Al6相向α-Al12（Fe,Mn）3Si相转变研究

采用SEM背散射电子（BSE）技术以及能谱（EDS）等手段定量研究了加热温度和保温时间对AA3104铝合金中（Fe,Mn）Al₆相向α-Al₁₂（Fe,Mn）₃Si相转变作用规律,通过连续截面方法对600℃保温条件下不同阶段的共晶相(即（Fe,Mn）Al₆相及α-Al₁₂（Fe,Mn）₃Si相)形貌进行三维重构,从三维角度揭示了转化各阶段共晶相的三维形态.对转变过程中标志性的铝点进行了定量表征,结果表明在转化的不同阶段,对应的铝点形貌特征也不尽相同,在均匀化进行到一定阶段后,大量铝点通过扩散而消失,导致α相体积明显减小.分析了转化后α相的微观形貌特征,认为转化后存在的脆弱"双相"界面以及α相内部"疏松多孔"的状态,将有助于其在轧制过程中的破碎.     

Overheating temperature of 7B04 high strength aluminum alloy

The microstructure and overheating characteristics of the direct chill semicontinuous casting ingot of 7B04 high strength aluminum alloy, and those after industrial homogenization treatment and multi-stage homogenization treatments, were studied by differential scanning calorimetry(DSC), optical microscopy(OM) and scanning electron microscopy with energy dispersive X-ray spectroscopy(SEM-EDX). The results show that the microstructure of direct chill semicontinuous casting ingot of the 7B04 alloy contains a large number of constituents in the form of dendritic networks that consist of nonequilibrium eutectic and Fe-containing phases. The nonequilibrium eutectic contains Al, Zn, Mg and Cu, and the Fe-containing phases include two kinds of phases, one containing Al, Fe, Mn and Cu, and the other having Al, Fe, Mn, Cr, Si and Cu. The melting point of the nonequilibrium eutectic is 478 ℃ for the casting ingot of the 7B04 alloy which is usually considered as its overheating temperature. During industrial homogenization treatment processing at 470 ℃, the nonequilibrium eutectic dissolves into the matrix of this alloy partly, and the remainder transforms into Al2CuMg phase that cannot be dissolved into the matrix at that temperature completely. The melting point of the Al2CuMg phase which can dissolve into the matrix completely by slow heating is about 490 ℃. The overheating temperature of this high strength aluminum alloy can rise to 500-520 ℃. By means of special multi-stage homogenization, the temperature of the homogenization treatment of the ingot of the 7B04 high strength aluminum alloy can reach 500 ℃ without overheating.     

3003-H16铝合金卷材生产过程中的组织演变

利用热分析仪、光学显微镜、扫描电镜和能谱仪等方法研究了3003-H16铝合金卷材生产过程中的组织演变。结果表明,晶粒尺寸、二次枝晶间距和金属间化合物尺寸从铸锭心部至铸锭表层逐渐减小。当均匀化温度为590 ℃时,α-Al晶体内析出细小颗粒状的Al₆Mn;随均匀化温度的提高,颗粒状析出相不断溶解并促进针棒状析出相长大;当均匀化温度为640 ℃时,针棒状析出相开始溶解,至650 ℃时完全溶解。金属间化合物Al₆(Fe,Mn)和Al₆Mn随均匀化温度的升高而变得圆滑球化,部分Al₆(Fe,Mn)在均匀化过程中转变为Al(Fe,Mn)Si。3003铝合金热轧卷材的晶粒组织在厚度方向上存在不均匀性,冷轧和中间退火后有所改善。3003铝合金卷材中的化合物沿轧制方向成行排列,具有明显的方向性,其中大尺寸化合物的比例随加工率的增大逐渐降低。均匀化可以改善3003铝合金的成分和组织均匀性,改善合金的塑性。变形加工在提高3003铝合金强度的同时降低了合金的塑性。中间退火过程中纤维状的变形组织转变为再结晶组织,消除了硬化现象,合金的塑性得到改善。     

热轧Al-Zn共析合金的显微组织演变

Al-Zn共析合金是一种典型的超塑性金属材料,其细小晶粒组织一般通过热处理获得。近来,热力学控制过程已经运用于微观组织细化。据此,将20mm厚的铸锭分别按以下3种方案进行均匀化,并热轧至2mm厚以获得细化微观组织。这3种方案分别为：1）均匀化后空冷和热轧;2）均匀化后水淬和热轧;3）均匀化后立即热轧。微观组织观察表明：采用方案1和3均匀化后形成片层组织,并且在热轧进行的时候破碎成细小的晶粒组织。采用方案2处理时,细小的晶粒组织直接通过热轧过程获得,中间没有形成层片组织。结果表明,采用方案3处理后获得的材料晶粒最小,其尺寸为1．6μm;室温下拉伸测试结果表明,采用方案3处理的材料的伸长率最大。     

Mg-6Zn-3Sn合金的均匀化热处理及其对显微组织和力学性能的影响（英文）

利用DSC、OM、XRD、SEM、TEM、维氏硬度计和万能试验机，研究Mg-6Zn-3Sn合金均匀化过程中的显微组织和力学性能演变，分析合金过烧的原因和扩散动力学，确定合金的均匀化制度。结果表明，单级均匀化处理后，Mg₂Zn₃相分解，同时伴随着Mg₂Sn相的析出。当均匀化温度上升到350℃时，Mg₂Zn₃相导致合金的过烧。合金合适的均匀化制度为(335℃，24 h)+(400℃，6 h)。在双级均匀化过程中，合金的硬度持续下降，力学性能呈现先升后降的趋势，这与Zn和Sn原子的固溶和Mg₂Sn相的析出有关。     

高合金化Al-9Zn-2Mg-2Cu-0.3Ce合金均匀化过程中的组织演变

采用光学显微镜(OM)、扫描电镜(SEM)、电子探针显微分析(EPMA)、X射线衍射(XRD)以及差示扫描量热仪(DSC),研究了一种高合金化Al-9Zn-2.0Mg-2Cu-0.3Ce(质量分数,%)合金的铸态微观组织,以及其均匀化过程中微观组织的演变,获得了较优的单级均匀化工艺。结果表明:铸态时,合金晶粒内部枝晶网络发达,Zn、Mg、Cu元素偏聚严重,合金中主要的非平衡凝固相为T(AlZnMgCu) 相和θ(Al₂Cu)相。经过470 ℃×48 h均匀化热处理后,合金中的枝晶网络基本消除,凝固相T逐渐回溶至基体中,主要的残留相为耐高温相Al₂CuMg、Al₈Cu₄Ce和Al₇Cu₂Fe。扩散动力学分析表明,470 ℃退火48 h的单级均匀化工艺足以使合金中的非平衡相回溶至基体中。