In-situ observations and acoustic measurements upon fragmentation of free-floating intermetallics under ultrasonic cavitation in water

Grain refinement in alloys is a well-known effect of ultrasonic melt processing. Fragmentation of primary crystals by cavitation-induced action in liquid metals is considered as one of the main driving mechanisms for producing finer and equiaxed grain structures. However, in-situ observations of the fragmentation process are generally complex and difficult to follow in opaque liquid metals, especially for the free-floating crystals. In the present study, we develop a transparent test rig to observe in real time the fragmentation potential of free-floating primary Al₃Zr particles under ultrasonic excitation in water (an established analogue medium to liquid aluminium for cavitation studies). An effective treatment domain was identified and fragmentation time determined using acoustic pressure field mapping. For the first time, real-time high-speed imaging captured the dynamic interaction of shock waves from the collapsing bubbles with floating intermetallic particles that led to their fragmentation. The breakage sequence as well as the cavitation erosion pattern were studied by means of post-treatment microscopic characterisation of the fragments. Fragment size distribution and crack patterns on the fractured surface were then analysed and quantified. Application of ultrasound is shown to rapidly (<10 s) reduce intermetallic size (from 5 mm down to 10 μm), thereby increasing the number of potential nucleation sites for the grain refinement of aluminium alloys during melt treatment.     

Effect of ultrasonic melt processing and Al-Ti-B on the microstructural refinement of recycled Al alloys

Refining the α-Al grain size and controlling the morphology of intermetallic phases during solidification of Al alloys using ultrasonic melt processing (USMP) and Al-Ti-B have been extensively used in academic and industry. While, their synergy effect on the formation of these phases has not yet clearly demonstrated. In this paper, the influence of USMP and Al-Ti-B on the solidified microstructure of multicomponent Al-4.5Cu-0.5Mn-0.5Mg-0.2Si-xFe alloys (x = 0.7, and 1.2 wt%) has been comparatively studied. The results show that the USMP + Al-Ti-B method produce a more profound refinement effect than the individual methods. In addition, the area of single Fe-rich phases in both alloys with USMP + Al-Ti-B are also refined compared with conventional methods. A mechanism is proposed for the refinement, which are the deagglomerated TiB₂ parties induced by USMP providing more effective nucleation sites for α-Al, and the refined interdendritic regions limited the growth of Fe-rich phases in the following eutectic reaction. Finally, the application of combined USMP + Al-Ti-B methods is feasible in microstructural refinement, resulting in the improving the casting soundness and mechanical properties of alloys.     

On the governing fragmentation mechanism of primary intermetallics by induced cavitation

One of the main applications of ultrasonic melt treatment is the grain refinement of aluminium alloys. Among several suggested mechanisms, the fragmentation of primary intermetallics by acoustic cavitation is regarded as very efficient. However, the physical process causing this fragmentation has received little attention and is not yet well understood. In this study, we evaluate the mechanical properties of primary Al₃Zr intermetallics by nano-indentation experiments and correlate those with in-situ high-speed imaging (of up to 1 Mfps) of their fragmentation process by laser-induced cavitation (single bubble) and by acoustic cavitation (cloud of bubbles) in water. Intermetallic crystals were chemically extracted from an Al-3 wt% Zr alloy matrix. Mechanical properties such as hardness, elastic modulus and fracture toughness of the extracted intermetallics were determined using a geometrically fixed Berkovich nano-diamond and cube corner indenter, under ambient temperature conditions. The studied crystals were then exposed to the two cavitation conditions mentioned. Results demonstrated for the first time that the governing fragmentation mechanism of the studied intermetallics was due to the emitted shock waves from the collapsing bubbles. The fragmentation caused by a single bubble collapse was found to be almost instantaneous. On the other hand, sono-fragmentation studies revealed that the intermetallic crystal initially underwent low cycle fatigue loading, followed by catastrophic brittle failure due to propagating shock waves. The observed fragmentation mechanism was supported by fracture mechanics and pressure measurements using a calibrated fibre optic hydrophone. Results showed that the acoustic pressures produced from shock wave emissions in the case of a single bubble collapse, and responsible for instantaneous fragmentation of the intermetallics, were in the range of 20–40 MPa. Whereas, the shock pressure generated from the acoustic cavitation cloud collapses surged up to 1.6 MPa inducing fatigue stresses within the crystal leading to eventual fragmentation.     

Grain fragmentation in ultrasonic-assisted TIG weld of pure aluminum

Under the action of acoustic waves during an ultrasonic-assisted tungsten inert gas (TIG) welding process, a grain of a TIG weld of aluminum alloy is refined by nucleation and grain fragmentation. Herein, effects of ultrasound on grain fragmentation in the TIG weld of aluminum alloy are investigated via systematic welding experiments of pure aluminum. First, experiments involving continuous and fixed-position welding are performed, which demonstrate that ultrasound can break the grain of the TIG weld of pure aluminum. The microstructural characteristics of an ultrasonic-assisted TIG weld fabricated by fixed-position welding are analyzed. The microstructure is found to transform from plane crystal, columnar crystal, and uniform equiaxed crystal into plane crystal, deformed columnar crystal, and nonuniform equiaxed crystal after application of ultrasound. Second, factors influencing ultrasonic grain fragmentation are investigated. The ultrasonic amplitude and welding current are found to have a considerable effect on grain fragmentation. The degree of fragmentation first increases and then decreases with an increase in ultrasonic amplitude, and it increases with an increase in welding current. Measurement results of the vibration of the weld pool show that the degree of grain fragmentation is related to the intensity of acoustic nonlinearity in the weld pool. The greater the intensity of acoustic nonlinearity, the greater is the degree of grain fragmentation. Finally, the mechanism of ultrasonic grain fragmentation in the TIG weld of pure aluminum is discussed. A finite element simulation is used to simulate the acoustic pressure and flow in the weld pool. The acoustic pressure in the weld pool exceeds the cavitation threshold, and cavitation bubbles are generated. The flow velocity in the weld pool does not change noticeably after application of ultrasound. It is concluded that the high-pressure conditions induced during the occurrence of cavitation, lead to grain fragmentation in a pure aluminum TIG weld during an ultrasonic-assisted TIG welding process.     

Ultrasound cavitation induced nucleation in metal solidification: An analytical model and validation by real-time experiments

Microstructural refinement of metallic alloys via ultrasonic melt processing (USMP) is an environmentally friendly and promising method. However, so far there has been no report in open literature on how to predict the solidified microstructures and grain size based on the ultrasound processing parameters.In this paper, an analytical model is developed to calculate the cavitation enhanced undercooling and the USMP refined solidification microstructure and grain size for Al-Cu alloys. Ultrafast synchrotron X-ray imaging and tomography techniques were used to collect the real-time experimental data for validating the model and the calculated results. The comparison between modeling and experiments reveal that there exists an effective ultrasound input power intensity for maximizing the grain refinement effects for the Al-Cu alloys, which is in the range of 20-45 MW/m². In addition, a monotonous increase in temperature during USMP has negative effect on producing new nuclei, deteriorating the benefit of microstructure refinement due to the application of ultrasound.     

A model of grain refinement and strengthening of Al alloys due to cold severe plastic deformation

This paper presents a model which quantitatively predicts grain refinement and strength/hardness of Al alloys after very high levels of cold deformation through processes including cold rolling, equal channel angular pressing (ECAP), multiple forging (MF), accumulative roll bonding (ARB) and embossing. The model deals with materials in which plastic deformation is exclusively due to dislocation movement within grains, which is in good approximation the case for many metallic alloys at low temperature, for instance aluminium alloys. In the early stages of deformation, the generated dislocations are stored in grains and contribute to overall strength. With increase in strain, excess dislocations form and/or move to new cell walls/grain boundaries and grains are refined. We examine this model using both our own data as well as the data in the literature. It is shown that grain size and strength/hardness are predicted to a good accuracy.     

Titanium as an endogenous grain-refining nucleus

Several studies have confirmed the applicability of the inverse growth restriction theory for predicting grain size in titanium alloy systems. However, until now, no work has identified nuclei particles that could be used to refine the β-grain size of titanium alloys during solidification. This work investigated whether titanium powder can be used to nucleate β-grains during solidification. A novel technique was used to introduce titanium powder to a series of titanium alloys, which results in significant grain refinement with an order of magnitude increase in grain density. Electron back-scattered diffraction (EBSD) was used to prove that titanium substrates can epitaxially nucleate titanium during solidification, and although a number of other potential mechanisms were investigated, it was concluded that the titanium particles heterogeneously nucleate β-grains.     

Grain refinement caused by intensified cavitation within narrow channel and its improvement to ultrasonically soldered Al joint property

In this work, grain refinement of the aluminum soldered joint was obtained by applying cavitation within narrow channels and the possible grain refinement mechanism was proposed. Aluminum sheets with different channel widths were ultrasonically soldered by pure Sn in air. An ultrasonic system with a TC4 sonotrode, was operated at a frequency of 20 kHz and power of 1000 W during soldering. The effect of channel width on grain size, element distribution and strength of the soldered joint was studied. Results showed that the grain size decreased from 2.62 to 1.04 µm and the element ratio of Al in solder increased from 0.93 to 4.86% when the channel width decreased from 0.8 to 0.2 mm. Instant solidification of Sn grains was readily observed in the joint before cooling due to the large undercooling induced by the intensified cavitation inside the narrow channels. The random cavitation induced nucleation of Sn was believed to be mainly responsible for the grain refinement of the soldered joint. The shear strength of the joint increased from 29.5 to 48.8 MPa and the hardness increased from 16.5 to 25.2 HV due to the grain refinement of Sn and the presence of Al transferred from the substrates.     

Comparison of frequency domain and time domain methods for the numerical simulation of contactless ultrasonic cavitation

The use of a top-mounted electromagnetic induction coil has been demonstrated as a contactless alternative to traditional ultrasonic treatment (UST) techniques that use an immersed mechanical sonotrode for the treatment of metals in the liquid state. This method offers similar benefits to existing UST approaches, including degassing, grain refinement, and dispersion of nanoparticles, while also preventing contact contamination due to erosion of the sonotrode. Contactless treatment potentially extends UST to high temperature or reactive melts. Generally, the method relies on acoustic resonance to reach pressure levels suitable for inertial cavitation and as a result the active cavitation volume tends to lie deep in the melt rather than in the small volume surrounding the immersed sonotrode probe. Consequently, (i) with suitable tuning of the coil supply frequency for resonance, the treatment volume can be made arbitrarily large, (ii) the problem of shielding and pressure wave attenuation suffered by the immersed sonotrode is avoided. However, relying on acoustic resonance presents problems: (i) the emergence of bubbles alters the speed of sound, resonance is momentarily lost, and cavitation becomes intermittent, (ii) as sound waves travel through and reflect on all the materials surrounding the melt, the sound characteristics of the crucible and supporting structures need to be carefully considered. The physics of cavitation coupled with this intermittent behaviour poses a challenge to sonotrode modelling orthodoxy, a problem we are trying to address in this publication. Two alternative approaches will be discussed, one of which is in the time domain and one in the frequency domain, which couple the solution of a bubble dynamics solver with that of an acoustics solver, to give an accurate prediction of the acoustic pressure generated by the induction coil. The time domain solver uses a novel algorithm to improve simulation time, by detecting an imminent bubble collapse and prescribing its subsequent behaviour, rather than directly solving a region that would normally require extremely small time steps. This way, it is shown to predict intermittent cavitation. The frequency domain solver for the first time couples the nonlinear Helmholtz model used for studying cavitation, with a background source term for the contribution of Lorentz forces. It predicts comparable RMS pressures to the time domain solver, but not the intermittent behaviour due to the underlying harmonic assumption. As further validation, the frequency domain method is also used to compare the generated acoustic pressure with that of traditional UST using a mechanical sonotrode.     

急冷条件下NiAl-Mo三元共晶合金的组织形成机制

采用单辊急冷技术实现了NiAl-Mo三元两相共晶合金的快速凝固, 同时与常规条件下的凝固组织进行了对比研究. 实验发现, 单辊急冷的合金条带与常规条件的凝固样品均由B2结构的NiAl金属间化合物和bcc结构的Mo固溶体两相组成, 两相均具有(110)晶面优先生长的趋势, 并呈现出(110)NiAl//(110)Mo取向关系. 常规条件下得到的微观结构主要由规则的两相共晶组织组成, 形成了类似菊花状的共晶胞. 而单辊急冷条件下形成的组织结构主要是由近辊面的柱状晶区和近自由面的等轴晶区组成的凝固组织. 理论计算发现, 合金熔体的单辊辊速由10 m/s增大至50 m/s后, 其冷却速率从1.01×10⁷ K/s逐渐增大到2.46×10⁷ K/s, 冷却速率明显高于常规铸造过程, 因而形成了差别很大的凝固组织. 随着辊速(冷却速率)的增加, 合金条带的厚度从54.4 μm减小至22 μm, 近辊面柱状晶区的厚度所占比例也逐渐增大, 晶粒发生了明显细化. 关键词： 快速凝固 三元共晶 共晶转变 冷却速率     

快速凝固Co-Cu包晶合金的电学性能

研究了Co-Cu包晶合金快速凝固过程中的相选择和组织形成特征, 探索了冷却速率、组织结构和晶体位向与合金电阻率之间的相关规律.实验发现, 快速凝固可使Co在(Cu)中的固溶度扩展至20%.Cu含量大于80%时, L+αCo→(Cu)包晶转变被抑制, (Cu)可从过冷熔体中直接形核析出.Cu含量在40%—70%范围时, Co-Cu合金的液相分离受到抑制, 凝固组织沿条带厚度方向分为两个晶区.细晶区中αCo和(Cu)相竞争形核并生长, αCo枝晶形态细密，细小的（Cu）等轴晶均匀分布于αCo的基体之中.粗晶区αCo相为领先相, 富Cu相分布于αCo枝晶的晶界处.随着冷速的增大, 合金组织显著细化, 晶界增多,对自由电子的散射作用增强, 合金电阻率显著增大.当晶界散射系数r＝0996—0999时, 可采用M-S模型综合分析快速凝固Co-Cu合金的电阻率. 关键词： 电阻率 快速凝固 相结构 晶体生长     

液态三元Fe-Cr-Ni合金中快速枝晶生长与溶质分布规律

采用落管方法实现了液态三元Fe-Cr-Ni合金的深过冷与快速凝固,合金液滴的冷却速率和过冷度均随液滴直径的减小而迅速增大.两种成分合金近平衡凝固组织均为粗大板条状α相.在快速凝固过程中,不同直径Fe_(81.4)Cr_(13.9)Ni_(4.7)合金液滴凝固组织均为板条状α相,其固态相变特征很明显,随着过冷度增大,初生δ相由具有发达主干的粗大枝晶转变为等轴晶.Fe_(81.4)Cr_(4.7)Ni_(13.9)合金液滴凝固组织由α相晶粒组成,随着过冷度增大,初生γ相由具有发达主干的粗大枝晶转变为等轴晶,其枝晶主干长度和二次分枝间距均显著下降,晶粒内溶质的相对偏析度也明显减小,溶质Ni的相对偏析度始终大于溶质Cr.理论计算表明,与γ相相比,δ相枝晶生长速度更大.在实验获得的过冷度范围内,两种Fe-Cr-Ni合金枝晶生长过程均由热扩散控制.     

Interactions between a cavitation bubble and solidification front under the effects of ultrasound: Experiments and lattice Boltzmann modeling

The phenomena of melting and dendritic fragmentation are captured by using an in-situ device during the ultrasound-assisted solidification of a succinonitrile-acetone (SCN-ACE) alloy. The experimental results show that the dendrite arms detach from primary trunk due to the melting of the solid phase, which is caused by a moving ultrasound cavitation bubble. To quantify the interactions between the ultrasound cavitation bubble and the solidification front, a coupled lattice Boltzmann (LB) model is developed for describing the fields of temperature, flow, and solid fraction, and their interactions. The multi-relaxation-time (MRT) scheme is applied in the LB model to calculate the liquid-gas flow field, while the Bhatnagar–Gross–Krook (BGK) equation is executed to simulate the evolution of temperature. The kinetics of solidification and melting are calculated according to the lever rule based on the SCN-ACE phase diagram. After the validation of the LB model by an analytical model, the morphologies of the cavitation bubble and solidification front are simulated. It is revealed that the solidification interface melts due to the increase of the temperature nearby the cavitation bubble in ultrasonic field. The simulated morphologies of the cavitation bubble and solidification front are compared well with the experimental micrograph. Quantitative investigations are carried out for analyzing the melting rate of the solidification front under different conditions. The simulated data obtained from LB modeling and theoretical predictions reasonably accord with the experimental results, demonstrating that the larger the ultrasonic intensity, the faster the melting rate. The present study not only reveals the evolution of the solidification front shape caused by the cavitation bubbles, which is invisible in the ultrasound-assisted solidification process of practical alloys, but also reproduces the complex interactions among the temperature field, acoustic streaming, and multi-phase flows.     

The cavitation erosion of ultrasonic sonotrode during large-scale metallic casting: Experiment and simulation

Ultrasonic sonotrodes play an essential role in transmitting power ultrasound into the large-scale metallic casting. However, cavitation erosion considerably impairs the in-service performance of ultrasonic sonotrodes, leading to marginal microstructural refinement. In this work, the cavitation erosion behaviour of ultrasonic sonotrodes in large-scale castings was explored using the industry-level experiments of Al alloy cylindrical ingots (i.e. 630 mm in diameter and 6000 mm in length). When introducing power ultrasound, severe cavitation erosion was found to reproducibly occur at some specific positions on ultrasonic sonotrodes. However, there is no cavitation erosion present on the ultrasonic sonotrodes that were not driven by electric generator. Vibratory examination showed cavitation erosion depended on the vibration state of ultrasonic sonotrodes. Moreover, a finite element (FE) model was developed to simulate the evolution and distribution of acoustic pressure in 3-D solidification volume. FE simulation results confirmed that significant dynamic interaction between sonotrodes and melts only happened at some specific positions corresponding to severe cavitation erosion. This work will allow for developing more advanced ultrasonic sonotrodes with better cavitation erosion-resistance, in particular for large-scale castings, from the perspectives of ultrasonic physics and mechanical design.     

A high-temperature acoustic field measurement and analysis system for determining cavitation intensity in ultrasonically solidified metallic alloys

A high-temperature acoustic field measurement and analysis system (HTAFS) was self-designed and developed to achieve real-time acoustic field analysis and quantitative cavitation characterization within high-temperature liquids. The acoustic signal was acquired by a high-temperature resistant waveguide and calibrated by separate compensation of line and continuous spectra to eliminate frequency offsets. Moreover, a new method was proposed to derive from the continuous-spectrum sound intensity and line-spectrum sound intensity in the frequency band above 1.5 times the fundamental frequency to characterize the intensity of transient cavitation and stable cavitation. The acoustic field characteristics within solidifying liquid Al-7 %Si alloy were successfully determined by this system. With the increase of ultrasound amplitude, the acoustic pressure in the alloy melt increased to be stable, the transient cavitation intensity first rose and then declined, and the stable cavitation intensity remained unchanged. Combined with the structural evolution of the primary α(Al) phase, the transient cavitation intensity was determined to be the dominant factor for the ultrasound-induced grain refinement effect.     

Microstructure evolution and grain refinement of ultrasonic-assisted soldering joint by using Ni foam reinforced Sn composite solder

In this investigation, ultrasonic-assisted soldering at 260 °C in air produced high strength and high melting point Cu connections in 60 s using Ni foam reinforced Sn composite solder. Systematically examined were the microstructure, grain morphology, and shear strength of connections made with various porosities of Ni foam composite solders. Results shown that Ni foams as strengthening phases could reinforce Sn solder effectively. The addition of Ni foam accelerated the metallurgical reaction due to great amount of liquid/solid interfaces, and refined the intermetallic compounds (IMCs) grains by ultrasonic cavitation. The joints had different IMCs by using Ni foam with different porosity. Layered (Cu,Ni)₆Sn₅ and (Ni,Cu)₃Sn₄ phases both existed in Cu/Ni60-Sn/Cu joint while only (Cu,Ni)₆Sn₅ IMCs grew in Cu/Ni98-Sn/Cu joint. As ultrasonic time increasing, Ni skeletons were dissolved and the IMCs were peeled off from substrates and broken into small particles. And then, the IMCs gradually dissociated into refined particles and distributed homogeneously in the whole soldering seam under cavitation effects. Herein, the Cu/Ni60-Sn/Cu joint ultrasonically soldered for 60 s exhibited the highest shear strength of 86.9 MPa, as well as a high melting point about 800 ℃ for the solder seam composed of Ni skeletons and Ni-Cu-Sn IMCs. The characterization indicated that the shearing failure mainly occurred in the interlayer of the soldering seam. The homogeneous distributed granular IMCs and Ni skeletons hindered the crack propagation and improved the strength of Cu alloy joints.     

Al-Ti-B细化工业纯铝凝固组织演变过程数值模拟

采用耦合群体动力学方法与元胞自动机方法建立了细化处理条件下铝合金凝固微观组织演变的数值模型.该模型考虑了a-Al的非均匀形核过程、晶粒的初始球形长大以及之后的枝晶生长过程.利用建立的模型模拟了Al-5Ti-1B中间合金细化工业纯铝凝固组织演变过程.结果表明:形核初始阶段,熔体中存在充足数量的有效形核粒子, a-Al形核率随着熔体过冷度的增大逐渐增高;形核开始不久后, a-Al的异质形核过程由熔体中有效形核粒子数量控制,直到再辉发生,形核停止.模拟分析了中间合金添加量以及熔体冷却速度对工业纯铝凝固组织演变过程的影响,模拟结果与实验结果相符,验证了模型的准确性.     

Role of external impacts in nanostructured titanium alloys

Specifics of the effects of electroplastic deformation, ion implantation (II), and ultrasonic treatment (UST) on the structure and characteristics of coarse-grained (CG) and ultrafine-grained (UFG) VT1-0, VT6 and TiNi titanium alloys are investigated. The introduction of pulse current during cold rolling promotes increased deformability and causes stress jumps during tension that result from phase transformations or the electroplastic effect (EPE). It is shown that EPE is a structurally sensitive property dependent on the size of grains. Methods of surface II and UST change the phase composition and lead to additional structural refinement in layers with a thickness of 0.1–10 microns.     

Characterization of acoustic cavitation in water and molten aluminum alloy

High-intensive ultrasonic vibrations have been recognized as an attractive tool for refining the grain structure of metals in casting technology. However, the practical application of ultrasonics in this area remains rather limited. One of the reasons is a lack of data needed to optimize the ultrasonic treatment conditions, particularly those concerning characteristics of cavitation zone in molten aluminum.The main aim of the present study was to investigate the intensity and spectral characteristics of cavitation noise generated during radiation of ultrasonic waves into water and molten aluminum alloys, and to establish a measure for evaluating the cavitation intensity. The measurements were performed by using a high temperature cavitometer capable of measuring the level of cavitation noise within five frequency bands from 0.01 to 10 MHz. The effect of cavitation treatment was verified by applying high-intense ultrasonic vibrations to a DC caster to refine the primary silicon grains of a model Al–17Si alloy. It was found that the level of high frequency noise components is the most adequate parameter for evaluating the cavitation intensity. Based on this finding, it was concluded that implosions of cavitation bubbles play a decisive role in refinement of the alloy structure.