X-Ray Videomicroscopy Studies of Eutectic Al-Si Solidification in Al-Si-Cu

Al-Si eutectic growth has been studied in-situ for the first time using X-ray video microscopy during directional solidification (DS) in unmodified and Sr-modified Al-Si-Cu alloys. In the unmodified alloys, Si is found to grow predominantly with needle-like tip morphologies, leading a highly irregular progressing eutectic interface with subsequent nucleation and growth of Al from the Si surfaces. In the Sr-modified alloys, the eutectic reaction is strongly suppressed, occurring with low nucleation frequency at undercoolings in the range 10 K to 18 K. In order to transport Cu rejected at the eutectic front back into the melt, the modified eutectic colonies attain meso-scale interface perturbations that eventually evolve into equiaxed composite-structure cells. The eutectic front also attains short-range microscale interface perturbations consistent with the characteristics of a fibrous Si growth. Evidence was found in support of Si nucleation occurring on potent particles suspended in the melt. Yet, both with Sr-modified and unmodified alloys, Si precipitation alone was not sufficient to facilitate the eutectic reaction, which apparently required additional undercooling for Al to form at the Si-particle interfaces.     

外吸除用硅片背面加工技术的研究

用SEM、TEM和光学显微镜研究了硅片背面的机械损伤（包括软损伤）和多晶硅的晶格结构,以及热处理过程中晶格结构和缺陷的演化,探索了吸杂的机理。实验结果表明,用本技术能减少S坑密度,提高硅片生产寿命,对金、铜等金属杂质有吸杂的效果。     

Experimental Investigation and optimization of Process Parameters for Shear Strength of Compound Cast Bimetallic Joints

Joining of A356 alloy and magnesium was carried out by vacuum assisted sand mold compound casting process. Microstructure at the joint interface was studied by using optical microscope, scanning electron microscope, energy dispersive X-ray spectroscopy and X-ray diffractometer. Characterization indicated that a relatively uniform joint interface was obtained. The joint interface was composed of three distinct layers containing Mg₂Al₃ on aluminum side, Mg₁₇Al₁₂?+?δ eutectic structure on magnesium side and Mg₁₇Al₁₂ as middle layer. As a result of interaction between silicon, present in A356 with magnesium, Mg₂Si compound was formed. Push out test was conducted on electronics universal testing machine to measure the shear strength across the joint interface. The important process parameters (grit size of sand paper, insert temperature, pouring temperature and vacuum pressure) were optimized to maximize the shear strength. Optimization was carried out by using response surface methodology, desirability analysis and genetic algorithm (GA) techniques. It was observed that the shear strength increased by 14.21, 8.60 and 4.80% with genetic algorithm, desirability analysis and regression model respectively. GA reported the optimal value of shear strength.     

铸造氧化铝／锌合金复合材料界面的SEM观察

利用挤压铸造制备氧化铝／锌合金复合材料,在扫描电镜（SEM）上观察复合材料的界面。在复合材料中纤维与基体间存在致密界面层,合金元素通过适当的化学反应可改善纤维与基体间的结合,在凝固过程中,纤维／基体界面上的硅在共晶体的生长过程中起到领先作用,导致复合材料的共晶转变是由铝硅共晶转变和锌铝共晶转变两者组成。     

Melting of secondary-phase particles in Al-Mg-Si alloys

The melting of secondary-phase particles—or, more precisely, the melting of such particles together with the surrounding matrix—in two ternary Al-Mg-Si alloys has been studied. In the quasi-binary Al-Mg₂Si alloy, one melting reaction is found. In the alloy with an Si content in excess of that necessary to form Mg₂Si, three different melting reactions are observed. At upquenching temperatures above the eutectic temperature, the reaction rates are very high, and it is assumed that they are controlled by diffusion of the alloying elements in the liquid. Melting is also observed after prolonged annealing at temperatures below the eutectic temperature in these alloys, which is explained by the different diffusion rates of Mg and Si. The rate of the melting reaction is in this case assumed to be controlled by diffusion of the alloying elements in the solid α-Al phase. It is shown that calculation of the particle/matrix interface composition, which determines when melting is possible, cannot be made solely on the basis of the phase diagram, but must also include the rate of diffusion of Mg and Si. The melting temperatures observed differ somewhat from the accepted eutectic temperatures for these alloys. On prolonged annealing, the liquid droplets formed dissolve into the surrounding matrix and their chemical composition is found to change during dissolution. The resulting eutectic structure after quenching of a droplet is explained by the phase diagram and the different diffusion rates of Mg and Si as well as by the nucleation conditions of the constituents involved.     

Melting of secondary-phase particles in Al-Mg-Si alloys

The melting of secondary-phase particles—or, more precisely, the melting of such particles together with the surrounding matrix—in two ternary Al-Mg-Si alloys has been studied. In the quasi-binary Al-Mg₂Si alloy, one melting reaction is found. In the alloy with an Si content in excess of that necessary to form Mg₂Si, three different melting reactions are observed. At upquenching temperatures above the eutectic temperature, the reaction rates are very high, and it is assumed that they are controlled by diffusion of the alloying elements in the liquid. Melting is also observed after prolonged annealing at temperatures below the eutectic temperature in these alloys, which is explained by the different diffusion rates of Mg and Si. The rate of the melting reaction is in this case assumed to be controlled by diffusion of the alloying elements in the solid α-Al phase. It is shown that calculation of the particle/matrix interface composition, which determines when melting is possible, cannot be made solely on the basis of the phase diagram, but must also include the rate of diffusion of Mg and Si. The melting temperatures observed differ somewhat from the accepted eutectic temperatures for these alloys. On prolonged annealing, the liquid droplets formed dissolve into the surrounding matrix and their chemical composition is found to change during dissolution. The resulting eutectic structure after quenching of a droplet is explained by the phase diagram and the different diffusion rates of Mg and Si as well as by the nucleation conditions of the constituents involved.     

Characterization of In-Based Eutectic Alloys Used in Josephson Packaging

InBiSn and InSn eutectic alloy solders used for Josephson packaging were characterized for the basic understanding of their behavior. Both physical structures and mechanical properties of these solders were studied under various conditions which partly simulate the processing and environmental exposure of these materials. Their interaction with the interface material (Pd/Au) was also probed in an attempt to understand the failure mechanism and to assess the package reliability.     

The behavior of silicon in the solidification of Zn-55Al-1.6Si coating on steel

Silicon is an essential element in the Zn-55Al-1.6Si coating. It is added to promote the formation of an adherent coating and prevent the excessive growth of an intermetallic alloy layer at the steel/coating interface. The addition of silicon also results in the formation of a silicon phase distributed in the interdendritic region of the overlay, having a flowery pattern on the surface, and appearing needlelike when observed inside the overlay. The behavior of silicon during the solidification process of the Zn-55Al-1.6Si coating is examined in the current study. It is found that the coating solidification proceeds in three stages. At stage I, primary α-Al dendrites develop at about 566 °C to 520 °C, forming the framework of the coating structure. This is followed by stage II at about 520 °C to 381 °C, where the binary Al-Si eutectic reaction takes place, with the majority of the silicon phase forming at about 520 °C to 480 °C. At stage III the remaining molten phase undergoes a ternary Al-Zn-Si eutectic reaction forming the interdendritic zinc-rich network. The ternary Al-Zn-Si eutectic reaction is essentially equivalent to the binary Al-Zn eutectic reaction because of the very low level of silicon at the Al-Zn-Si eutectic point.     

The coupled zone of rapidly solidified AlSi alloys in laser treatment

Laser-melted tracks were produced on AlSi samples containing between 15.5 and 26 wt% Si with the resultant solidification rates being measured by taking a longitudinal section through the centre of the laser trace. The Al-rich boundary of the coupled zone, i.e.the growth rate-concentration limit at which the transition from fibrous AlSi eutectic to α-Al dendrites plus interdendritic eutectic takes place, has been experimentally determined for concentrations of Si varying from 15.5 to 20 wt%. Supposing that the growing structure, for a given growth rate, is the one having the higher growth temperature, good agreement is found with the more recent microstructural growth models when kinetic effects are taken into account. For concentrations of Si higher than 20 wt%, primary Si crystals imbedded in equiaxed eutectic grains are observed which replace columnar eutectic and dendritic growth.     

Study of the formation and intergrowth of granular eutectic in austenitic steel matrix composite by directional solidification technology

The formation and intergrowth of granular eutectic in austenitic steel matrix composite has been studied by directional solidification technology. The results indicate that the modifying element Si enhances the dendritic segregation of C and Mn. The surface active elements, such as Y and Ca, concentrate highly ahead of the solid-liquid (S-L) interface of the composite due to the nonequilibrium solidification. As a result, the S-L interface of the composite is unstable during solidification. The spatiotemporal condition of the formation and the growth of the granular eutectic is the formation of granular eutectic between austenitic dendrite arms at the end of solidification and its growth restricted by the austenitic dendrites. By the simulating eutectic growth of the granular eutectic by Fe−C−Mn alloy, the Si, Ca, and Y adsorb and enrich on the growing surface of the eutectic during crystallization, which makes the crystallization model of the eutectic turn from facet/nonfacet to nonfacet/nonfacet. The intergrowth of the eutectic can be explained by (1) the influence of the modifying elements on the crystallization of the eutectic, (2) the coarse solidification growth interface of the eutectic and the same growth rate for austenite and cementite ((Fe, Mn)₃C), and (3) the austenite and cementite ((Fe, Mn)₃C) have not lateral branch during eutectic growth.     

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.     

The Influence of a TiN Film on the Electronic Contribution to the Thermal Conductivity of a TiC Film in a TiN-TiC Layer System

TiC and TiN films were deposited by reactive magnetron sputtering on Si substrates. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) characterization of the microstructure and interface structure have been carried out and the stoichiometric composition of TiC is determined. Thermal conductivity and interface thermal conductance between different layers in the films are evaluated by the transient thermo reflectance (TTR) and three-omega (3-ω) methods. The results showed that the thermal conductivity of the TiC films increased with temperature. The thermal conductivity of TiC in the absence of TiN is dominated by phonon contribution. The electronic contribution to the thermal conductivity of TiC in the presence of TiN is found to be more significant. The interface thermal conductance of the TiC/TiN interface is much larger than that of interfaces at Au/TiC, TiC/Si, or TiN/Si. The interface thermal conductance between TiC and TiN is reduced by the layer formed as a result of interdiffusion.

     

Fatigue crack growth mechanisms at the microstructure scale in Al-Si-Mg cast alloys: Mechanisms in regions II and III

The fatigue crack growth behavior in Regions II and III of crack growth was investigated for hypoeutectic and eutectic Al-Si-Mg cast alloys. To isolate and establish the mechanistic contributions of characteristic microstructural features (dendritic α-Al matrix, eutectic phases, Mg-Si strengthening precipitates), alloys with various Si content/morphology, grain size level, and matrix strength were studied; the effect of secondary dendrite arm spacing (SDAS) was also assessed. In Regions II and III of crack growth, the observed changes in the fracture surface appearance were associated with changes in crack growth mechanisms at the microstructural scale (from a linear advance predominantly through primary α-Al to a tortuous advance exclusively through Al-Si eutectic Regions). The extent of the plastic zone ahead of the crack tip was successfully used to explain the changes in growth mechanisms. The fatigue crack growth tests were conducted on compact tension specimens under constant stress ratio,R=0.1, in ambient conditions.     

Growth of interdendritic eutectic in directionally solidified Al-Si alloys

Interdendritic eutectic microstructures in Al-Si (6 to 12.6 wt pct Si) alloys have been investigated as a function of growth velocity and temperature gradient. The interface morphology, as well as the behavior of the eutectic spacing and undercooling, suggest that the resultant microstructure is governed by two different growth processes. That is, at low growth rates, steady-state columnar eutectic growth is found and obeys the relationship, λ²V = constant, where λ is the eutectic spacing andV is the growth rate. At higher growth rates, the nucleation of equiaxed eutectic grains occurs in the interdendritic liquid. The experimental findings are interpreted in the light of recently developed models for the columnar to equiaxed transition and for irregular eutectic growth.     

Investigation on the modification behavior of A356 alloy inoculated with a Sr-Y composite modifier

In the present paper, differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and X-ray diffraction (XRD) were used to examine the effects of a Sr-Y composite modifier on the microstructure of A356 alloy. After adding Y to A356, YAl 3 compounds formed, and the size of the α (Al) crystal nucleus increased. The degree of supercooling caused by Sr-Y composite modifier was higher than Sr modification by 2.7 °C, leading to an increased nucleation rate. This increase in supercooling temperature was favorable to the refinement of eutectic structure of the alloy and its eutectic reaction was delayed to the maximum extent. The Si phase in the as-cast Sr-Y composite-modified A356 alloy was either granular or flaky. No large flakes of eutectic Si were found, and the modification effects were completely comparable with those obtained using a lone Sr modifier. After T6 heat treatment, most of the eutectic Si showed a grain-like shape with smaller grains. No eutectic Si with long-strip shapes, significant enhancements in the particle roundness and evenness of the Si crystals, and increased globosity were observed. Both the roundness and evenness of the grained Si crystals were enhanced, and the amount of globular eutectic Si available increased, these findings showed that excellent modification effects were achieved.     

Understanding texture domains and relations between pre-eutectic and eutectic phase during Al-Si alloy solidification

Phase morphology and crystallographic texture are important components of a solidification microstructure. Probability of nucleation of a nucleus is a strong function of local chemical & thermal conditions and its atomic orientation. Similarly, the growth kinetics for various crystal planes is dependent on its crystal orientation apart from local environmental conditions. The combined effects of nucleation & growth kinetics along with solidification conditions dictate the resulting microstructure of an alloy. In this study, various phases of a near eutectic Al-Si alloy are examined by serial sectioning and 3D reconstruction. A peculiar microstructure is observed in which primary silicon is present in the immediate proximity of primary aluminum. Observations through electron back scatter diffraction show that the microtexture of primary and eutectic Si is similar (with in a twin relation) and thus it is concluded that the formation of eutectic starts with eutectic Si forming on the primary Si.     

Growth of interdendritic eutectic in directionally solidified Al-Si alloys

Interdendritic eutectic microstructures in Al-Si (6 to 12.6 wt pct Si) alloys have been investigated as a function of growth velocity and temperature gradient. The interface morphology, as well as the behavior of the eutectic spacing and undercooling, suggest that the resultant microstructure is governed by two different growth processes. That is, at low growth rates, steady-state columnar eutectic growth is found and obeys the relationship, λ²V = constant, where λ is the eutectic spacing andV is the growth rate. At higher growth rates, the nucleation of equiaxed eutectic grains occurs in the interdendritic liquid. The experimental findings are interpreted in the light of recently developed models for the columnar to equiaxed transition and for irregular eutectic growth.     

Refinement of Eutectic Si Phase in Al-5Si Alloys with Yb Additions

A series of Al-5 wt pct Si alloys with Yb additions (up to 6100 ppm) have been investigated using thermal analysis and multiscale microstructure characterization techniques. The addition of Yb was found to cause no modification effect to a fibrous morphology involving Si twinning; however, a refined plate-like eutectic structure was observed. The Al₂Si₂Yb phase was observed with Yb addition level of more than 1000 ppm. Within the eutectic Al and Si phases, the Al₂Si₂Yb phase was also found as a precipitation from the remained liquid. No Yb was detected in the α-Al matrix or plate-like Si particle, even with Yb addition up to 6100 ppm. The absence of Yb inside the eutectic Si particle may partly explain why no significant Si twinning was observed along {111}_Si planes in the eutectic Si particle. In addition, the formation of the thermodynamic stable YbP phases is also proposed to deteriorate the potency of AlP phase in Al alloys. This investigation highlights to distinguish the modification associated with the ever present P in Al alloys. We define modification as a transition from faceted to fibrous morphology, while a reduction of the Si size is termed refinement.     

Lamellar eutectic stable growth — I. Modeling

Lamellar eutectic stable growth has been studied to set up a mathematical model on the growth. The model eliminates the restriction of isothermal(planar) growing interface, and is based on the coupling relation of thermal transfer, solute-diffusion effect, Gibbs-Thompson effect, and growth kinetics as well. A simple coupling equation for AlSi eutectic stable growth has been considered.     

Microstructure of laser treated Al alloys

In this study the microstructures of laser treated ultra pure Al and two AlSi alloys (Al0.4 Si and Al0.75 Si) were investigated. In ultra pure Al a large number of dislocation loops were found especially at higher laser scan velocities. During annealing only at laser scan velocities above 2 cm/s a large quantity of dislocation loops became visible. Both results indicate that at high laser velocities vacancies are frozen in, but at laser velocities around 1 cm/s there is still enough time at high temperature to reduce the vacancy concentration towards lower super-saturation. In AlSi alloys the dislocation density rises with higher laser scan velocities probably caused by the smaller distances between the eutectic cell walls. In these alloys entangled dislocation structures were found in contrast to ultra pure Al. For solidification structures consisting of an eutectic material with a high hardness as for an eutectic structure in AlSi alloys it was found that the hardness can be described by a pile up mechanism, which depends on the difficulty to exert stresses on neighbouring cells due to thick and hard walls. The hardness has been described by a 1/d² dependence, i.e. it is mainly determined by the small size d, of the solidification structure.