In situ observation of nucleation,fragmentation and microstructure evolution in Sn–Bi and Al–Cu alloys

Abstract

This paper presents recent progress of in situ observation for the microstructure evolution during solidification. Nucleation and fragmentation of dendrite arms are important issues for controlling microstructure during solidification. However, there are few studies on in situ observation of nucleation and fragmentation in metallic alloys. Time resolved X-ray imaging technique has been developed to observe solidification of metallic alloy systems in situ. Fragmentation of dendrite arms often occurred at the root after growth velocity was reduced for the Sn–13 at.-%Bi alloys and the Al–15 mass%Cu alloys. In the Al–15 mass%Cu alloys, both of nucleation and fragmentation contribute to formation of grain structure. The result suggested that fragmentation should be considered for controlling grain structure.     

Microstructure evolution of Cu-Pb monotectic alloys during directional solidification

1 Introduction Monotectic alloy is an important class of alloy whose binary phase diagram has a miscibility gap, in which the original single liquid will decompose into two distinct immiscible liquids within a few seconds. In the normal gravity field, a …     

In situ observation of solidification phenomena in Al–Cu and Fe–Si–Al alloys

Abstract

Synchrotron radiation enables the observation of solidification in metallic alloys. In situ observations of solidification for Al–Cu alloys (5, 10 and 15 wt-%Cu) are reported. Nucleation and fragmentation of dendrite arms were often observed in the 15 and 10%Cu alloys when unidirectional solidification was performed from the planar interface. In contrast, nucleation and fragmentation were rarely observed in the 5%Cu alloys. The nucleation ahead of the solidifying front and the fragmentation in the mushy region strongly depended on alloy composition. This paper also presents in situ observation of solidification of Fe–10Si–0·5Al (at-%) alloys. The dendritic growth of δ-Fe was clearly observed using this technique. The development of X-ray imaging techniques enables the solidification of various conventional cast alloys such as Al, Ni and Fe alloys to be observed and will be increasingly used to investigate solidification phenomena.     

磁场作用下Al-Pb偏晶合金的凝固过程

在恒定磁场作用下对Al-Pb合金进行定向凝固实验, 考察了合金成分、凝固速度、恒定磁场对凝固组织的影响. 模拟研究了恒定磁场作用下Al-Pb合金定向凝固组织的形成过程, 分析了磁场的影响机理和合金成分、凝固速度、磁场强度对弥散型凝固组织获得的影响. 模拟和实验均表明恒定磁场促进弥散型偏晶合金凝固组织的形成.     

Fragmentation in an Al–7 wt-%Si alloy studied in real time by X-ray synchrotron techniques

Abstract

One mechanism for the formation of equiaxed grains is the detachment of dendrite fragments which is believed to be at the origin of the central equiaxed core region in casting processes. Unfortunately, the dynamics of the fragmentation phenomena cannot be revealed by classical methods. Investigation of a unrefined Al–7 wt-%Si alloy using in situ and real time synchrotron X-radiography and X-ray topography at the European Synchrotron Radiation Facility, has allowed verification of the existence of dendrite fragmentation and of cascade fragmentation during directional solidification, and to study the evolution of the growth and sedimentation of the equiaxed grains formed from these fragments. An examination of the crystallographic misorientation of dendrites as fragmentation is ongoing. These results contribute to the understanding of the characteristics of the columnar to equiaxed transition and to knowledge of the origin of new equiaxed grains in unrefined alloys.     

Influence of a high magnetic field on columnar dendrite growth during directional solidification

The influence of a high magnetic field on the growth of MnBi, α-Al and Al₃Ni dendrites in directionally solidified Bi–Mn, Al–Cu and Al–Ni alloys have been investigated. Results indicate that the magnetic field changes the dendrite growth significantly. Indeed, the magnetic field aligns the primary dendrite arm and the effect is different for different dendrites. For the MnBi dendrite, an axial high magnetic field enhanced the growth of the primary dendrite arm along the solidification direction; however, for the α-Al and Al₃Ni dendrites, the magnetic field caused the primary dendrite arm to deviate from the solidification direction. At a lower growth speed, a high magnetic field is capable of causing the occurrence of the columnar-to-equiaxed transition (CET). Moreover, it has also been observed that a high magnetic field affects the growth of the high-order (i.e., secondary and tertiary) dendrite arms of the α-Al dendrite at a higher growth speed; as a consequence, the field enhances the branching of the dendrite and the formation of the (1 1 1)-twin planes. The above results may be attributed to the alignment of the primary dendrite arm under a high magnetic field and the effect of a high magnetic field on crystalline anisotropy during directional solidification.     

Investment casting of NiAl single-crystal alloys

Significant progress has been made in the understanding of solidification conditions, microstructure evolution, and defect formation during investment casting of NiAl single crystals. The high liquidus temperatures of NiAl alloys result in a larger dendrite arm spacing than is found in superalloy René N5. Because of their higher thermal conductivities, NiAl alloys have higher cooling rates and lower temperature gradients during solidification than René N5. These differences give NiAl alloys a lower tendency to form freckles and a higher tendency to form equiaxed grains. However, with the aid of process modeling, single crystals of various shapes of NiAl alloys have been produced.     

Revealing the Diversity of Dendritic Morphology Evolution During Solidification of Magnesium Alloys using Synchrotron X-ray Imaging: A Review

In this paper, the diversity of complicated dendrite microstructure and its evolution behavior during solidification in different magnesium alloys under various processing conditions were illustrated using synchrotron X-ray imaging technique. A variety of dendritic morphologies and branching structures were revealed, i.e., sixfold plate-like symmetric structure in Mg-Al-based structure, 12-branch structure in Mg-Zn-based alloys and 18-branch structure in Mg-Sn- and Mg-Ca-based alloys as well as seaweed like hyper-branched structure in Mg-38wt%Zn alloy. In addition, a dendrite morphology and orientation transition with increasing addition of Zn content were also observed in Mg-Zn alloy, with dendrite growth pattern transform from anisotropy (low Zn addition) with sixfold symmetric snow-flake structure to relative isotropy (intermediate Zn addition) where seaweed morphology presented and then back to anisotropy (high Zn addition) when only 12 branches with preferred < $11\overline{2}1$ > orientations were observed. The phase-field model representing the typical dendritic morphologies and branching structures under various conditions was also depicted and discussed. Further, the two-dimensional (2D) real-time dendrite growth dynamics in different Mg-based alloys captured using synchrotron X-ray radiography for unveiling the originate of the α-Mg dendrite was reviewed. Following this, the four-dimensional (3D + time) synchrotron X-ray tomographic in situ observation of dendritic morphology evolution indicating the formation mechanism of the diverse dendritic morphology during Mg-Sn- and Mg-Zn-based alloys was also summarized. Finally, the future study on exploring the complicated dendritic morphologies and their origination during solidification of Mg-based alloys is prospected.     

Ag-Ni电接触材料快速/亚快速凝固过程研究

采用快速/亚快速凝固方法制备了富Ni相粒子弥散分布于Ag基体的Ag-Ni合金。建立了Ag-Ni合金凝固过程中组织演变的动力学模型,模拟计算了Ag-Ni合金凝固组织形成过程,分析讨论了合金成分对Ag-Ni合金凝固组织形成过程的影响。结果表明,合金的Ni含量越高,凝固组织中富Ni相粒子平均尺寸越大;Ag-Ni合金熔体冷却凝固时,富Ni相液滴/粒子的尺寸主要受形核和长大控制,Ostwald粗化作用很弱。     

Microstructures and evolution mechanism of highly undercooled Ni-Pb hypermonotectic alloy

The microstructures and evolution mechanism of the undercooled Ni-20%Pb(molar fraction) alloy were investigated systematically by high undercooling solidification technique. The experiment results indicate that the morphology of α-Ni phase and the distribution of Pb element in undercooled Ni-20% Pb alloys change with the in-crease of undercooling. The main evolution mechanisms of α-Ni are dendrite remelting and recrystallization. Pb phase in the microstructure of Ni-20% Pb hypermonotectic alloy originates from L2 phase separated from the parent melt during the cooling process through immiscible gap and L2 phase formed at the temperature of monotectic trans-formation. The solubility of Ph element in α-Ni phase under high undercooling condition is up to 5.83% which is ob-viously higher than that under equilibrium solidification condition. The real reason that causes the solubility difference is distinct solute trapping.     

Solidification paths of multicomponent monotectic aluminum alloys

Solidification paths of three ternary monotectic alloy systems, Al–Bi–Zn, Al–Sn–Cu and Al–Bi–Cu, are studied using thermodynamic calculations, both for the pertinent phase diagrams and also for specific details concerning the solidification of selected alloy compositions. The coupled composition variation in two different liquids is quantitatively given. Various ternary monotectic four-phase reactions are encountered during solidification, as opposed to the simple binary monotectic, L′ → L′′ + solid. These intricacies are reflected in the solidification microstructures, as demonstrated for these three aluminum alloy systems, selected in view of their distinctive features. This examination of solidification paths and microstructure formation may be relevant for advanced solidification processing of multicomponent monotectic alloys.     

High temperature phase equilibria near Ti–50 at% Al composition in Ti–Al system studied by directional solidification

High temperature phase diagram near the stoichiometric composition of TiAl has been established by the directional solidification and quenching technique. The quenched dendrite morphologies showed that the first solidified phase was the β phase in Ti–44, 46, 48 at% Al alloys and the α phase in Ti–50, 52 at% Al alloys. From the EDS analysis of the quenched dendrite tips and measurement of the temperature gradient directly recorded during directional solidification in Ti–(44–52 at%)Al alloys, the solid-liquid phase equilibria could be determined. The phase transformation temperatures were also confirmed by DTA. The phase equilibria established in this study agreed with the phase diagram that Okamoto proposed, while the β+γ two phase region, which Murray suggested, was not found near the TiAl composition. The lamellar orientation in TiAl alloys has been reported to be controlled in the growth direction in the presence of the primary β phase from a liquid. A composition in which the liquid phase was fully transformed to the β phase was selected, Ti–44 at% Al alloy, and directional solidification was performed at the growth rate of 45 mm/h. It was found that the lamellar orientation was aligned at nearly 0° and 45° to the growth direction. It is thought that the success in controlling the lamellar orientation is due to β solidification of the Ti–44 at% Al alloy at the beginning of liquid/solid transformation.     

Observation of dendritic growth and fragmentation in Ga–In alloys by X-ray radioscopy

Abstract

Capabilities of the X-ray attenuation contrast radioscopy were utilised to provide a real time diagnostic technique for observations of dendritic growth and fragmentation during solidification of a Ga–30In (wt-%) alloy. The solidification process was visualised by means of a microfocus X-ray tube providing shadow radiographs at spatial resolutions of about 10 μm. Experiments have been carried out to solidify the Ga–In alloy unidirectionally either starting from the bottom or the top of the specimen. The first case is significantly affected by solutal convection, which governs a redistribution of solute concentration. A detachment of dendrite side arms, which is unambiguously caused by melt flow, was not observed. Dendritic fragmentation occurs during the solidification in the reverse top down direction. Variations of the applied cooling rate excited a transition from a columnar to an equiaxed dendritic growth (CET).     

偏晶合金Ni—31.44％Pb过冷组织粒化机制

利用溶融玻璃净化、循环过热相结合的方法对Ni-31.44%Pb(质量分数）偏晶合金宽过冷区间组织演化规律进行研究。结果表明：随过冷度的增大,凝固组织发生三次转变。其中当△T＞242K时,合金组织发生第三次转变,由细密枝晶骤燃粒化为过冷粒状晶。通过组织观察和过冷熔体枝晶生长过程的理论计算发现,快速凝固过程中液相变速率骤然增加,引起枝晶全面碎断,然后在枝晶块表面能和就变能的驱动下,晶界移动,发生碎晶合并－再结晶是形成过冷粒状晶的原因。     

Effect of melt flow on dendritic growth in AlSi7-based alloys during directional solidification

Abstract

High-strength automotive components are often made of AlSi7-based alloys. A very challenging problem with aluminium casting is the influence of melt flow during solidification, because it affects the microstructure formation and therefore the material properties. The scope of this paper is to investigate the effect of forced melt flow on the evolution of the dendritic microstructure in a binary AlSi7 alloy during directional solidification. Global modelling using the software CrysMAS provides typical flow patterns and velocities. These values are used as boundary condition for the flow in the phase field code MICRESS, which allows the numerical simulation of dendritic array solidification in 2D with applied flow. From solidification experiments in a gradient furnace with applied rotating magnetic field the dendrite shapes are determined. It is found consistently that intense melt flow leads to asymmetric dendrite shapes and the growth behaviour of the dendrite arms is directly correlated with the flow direction.     

Influence of dendrite arrangement on coarsening during solidification of high-solute Al alloys

Abstract

Coarsening of dendrite arms during continuous solidification is usually characterised by measuring the secondary dendrite arm spacing (SDAS). Images obtained in-situ from X-ray microscopy studies during solidification were used to study SDAS development. Local coarsening and growth kinetics were studied during the solidification of high-solute content aluminium alloys (i.e. Al–30 Cu and Al–20 Cu (wt-%)). Downward and upward solidification conditions were imposed on the sample alloys in order to study the effect of those on coarsening and growth kinetics. The dendritic arrangement, direction of growth and growth fluctuations influence solute-rich liquid distribution which in turn affects solute gradients changing undercooling and thus coarsening and growth kinetics.     

高温度梯度下Al-In偏晶合金定向凝固组织的演化规律

应用高温度梯度的方法，研究了在定向凝固条件下温度梯度与凝固速率的比值G／R对Al-17．5％In(质量分数)合金凝固组织的影响．结果表明，偏晶合金的定向凝固与共晶合金定向凝固的生长规律类似．在高温度梯度下，仅在很低的生长速度时才能形成二相有序排列的共生．在偏晶合金定向凝固进入稳态生长以后，在各自的相凝固前沿富集了另一相的溶质，由于两相的层间距不大，长大过程中的横向扩散占主导地位．随着生长速度的增大或温度梯度的降低，Al-17．5％In合金定向凝固组织从纤维结构到周期性或规则排列的串状结构再到弥散分布结构转变．这种转变与固一’液界面形状的转变有密切关系．     

In Situ Investigation of Dendrite Deformation During Upward Solidification of Al-7wt.%Si

The in situ investigation of dendrite deformation during solidification processing is an ongoing challenge because of the technical difficulties in carrying out experimental observations and direct measurements in metallic systems that are opaque to visible light and have a high melting temperature. Over the last 20 years, x-ray imaging has been established as a method of choice to overcome this experimental barrier by taking advantage of the increased capabilities of third-generation synchrotron x-ray sources, providing information on growth process and semisolid deformation that is not available otherwise. In this article, we present results showing that the unique combination of synchrotron x-ray radiography and synchrotron white beam x-ray topography can help to reveal the deformations that dendritic microstructures undergo during the upward directional solidification of Al-7wt.%Si alloys. Particular focus will be placed on the bending phenomena of dendrites because of gravity, which may precede fragmentation in the case of well-developed secondary arms.     

MICROSTRUCTURAL FEATURE OF Al-In MONOTECTIC ALLOY PROCESSED UNDER MICROGRAVITY

The microstructural feature of Al-In monotectic alloy processed under microgravity has beeninvestigated It was found that in the sample cooled in space,there are a lot of In particles inA! dendrite,but no particle has been observed in the sample cooled on the ground.Moreover,the In particles distribute with regularity and the A1 dendrite has an obvious boundary layermarked by a string of particles.Thus,the distinction between them may reflect the character-istics of the solid/liquid interface during solidification under different gravity conditions.     

Al-17.5In偏晶合金定向凝固规则第二相纤维的失稳判据

对Al-17.5In偏晶合金进行了定向凝固,考察了不同凝固速度对Al-17.5In偏晶合金凝固组织的影响.结果表明,在低速定向凝固时,通过偏晶反应析出的第二相纤维规则地排列在Al基体中.随着凝固速度的增大,第二相纤维逐渐演变成珍珠串状.分析了这种组织转变过程并推导出新的Al-17.5In偏晶合金规则第二相纤维失稳的判据.