Effect of cryomilling time on microstructure evolution and hardness of cryomilled AZ31 powders.

The synthesis of nanostructured AZ31 powder by cryomilling was studied in this paper. The microstructural evolution during cryomilling, including the changes of particle morphology and internal grain size, was characterized via optical microscopy, SEM, TEM and XRD. Observations during the cryomilling produced four main findings. Firstly, cryomilling can refine the grains of AZ31 particles down to 100 nm after around 1 h milling and the minimum average grain size of about 30 nm was reached when the cryomilling time was extended to 6 h or longer. Secondly, cold welding played a dominant role in the early stage of cryomilling, while fracture took place in the late stage and surpassed cold welding. The former led to a particle size increase while the latter decreased the particle size. The minimum average particle size after 6 h cryomilling was approximately 26 µm. Thirdly, a few particles were agglomerated with other particles and could not be processed by cryomilling due to cold welding. Finally, after cryomilling 6 h and longer times, the hardness reached 162 HV which was much higher than other values reported in AZ31 alloy studies.

Bilayer nanostructure coated AZ31 magnesium alloy implants: in vivo reconstruction of critical-sized rabbit femoral segmental bone defect.

Healing or reconstruction of critical-sized bone defects is still challenging in orthopaedic practice. In this study, we developed a new approach to control the degradation and improve the bone regeneration of the AZ31 magnesium substrate, fabricated as mesh cage implants. Subsequently, bilayer nanocomposite coating was carried out using polycaprolactone (PCL) and nano-hydroxyapatite (nHA) by dip-coating and electrospinning. Lastly, the healing capacity of the implants was studied in New Zealand White (NZW) rabbit critical-sized femur bone defects. X-ray analysis showed the coated implant group bridged and healed the critical defects 100% during four weeks of post-implantation. Micro-computed tomography (Micro-CT) study showed higher total bone volume (21.10%), trabecular thickness (0.73), and total porosity (85.71%) with bilayer coated implants than uncoated. Our results showed that nanocomposite coated implants controlled the in vivo degradation and improved bioactivity. Hence, the coated implants can be used as a promising bioresorbable implant for critical segmental bone defect repair applications.

A step towards intelligent EBSD microscopy: machine-learning prediction of twin activity in MgAZ31.

Although microscopy is often treated as a quasi-static exercise for obtaining a snapshot of events and structure, it is clear that a more dynamic approach, involving real-time decision making for guiding the investigation process, may provide deeper insights, more efficiently. On the other hand, many applications of machine learning involve the interpretation of local circumstances from experience gained over many observations; that is, machine learning potentially provides an ideal solution for more efficient microscopy. This paper explores the potential for informing the microscope's observation strategy while characterising critical events. In particular, the identification of regions likely to experience twin activity (twin interaction with grain boundary) in AZ31 magnesium is attempted, from only local information. EBSD-based observations in the neighbourhoods of twin activity are fed into a machine-learning environment to inform the future search for such events, and the accuracy of the resultant decisions is quantified relative to the number of prior observations. The potential for utilising different types of local information, and their resultant value in the prediction process, is also assessed. After applying an attribute selection filter, and various other machine-learning tools, a decision-tree model is able to classify likely neighbourhoods of twin activity with 85% accuracy. The resultant framework provides the first step towards an intelligent microscopy for efficient observation of stochastic events during in situ microscopy campaigns. LAY DESCRIPTION: One role of artificial intelligence is to predict future events after learning from many previous observations. In materials science, various phenomena (such as crack nucleation) are difficult to predict because they have been insufficiently observed. Furthermore, observation is difficult, precisely because their location cannot be predicted, leading to a chicken and egg conundrum. This paper applies machine learning to the search for twin nucleation sites in a magnesium alloy, in an attempt to guide the observation of twin nucleation events in a microscope based on previous observations. As more data is obtained, the accuracy of the location prediction will increase. In the current case, the machine-learning tool achieved 85% accuracy for predicting the location of twin interactions with grain boundaries after several thousand observations. The resultant framework provides the first step towards an intelligent microscopy for efficient observation of stochastic events during in situ microscopy campaigns.

Microstructure and corrosion behavior of laser surface-treated AZ31B Mg bio-implant material.

Although magnesium and magnesium alloys are considered biocompatible and biodegradable, they suffer from poor corrosion performance in the human body environment. In light of this, surface modification via rapid surface melting of AZ31B Mg alloy using a continuous-wave Nd:YAG laser was conducted. Laser processing was performed with laser energy ranging from 1.06 to 3.18 J/mm2. The corrosion behavior in simulated body fluid of laser surface-treated and untreated AZ31B Mg alloy samples was evaluated using electrochemical technique. The effect of laser surface treatment on phase and microstructure evolution was evaluated using X-ray diffraction and scanning electron microscopy. Microstructure examination revealed grain refinement as well as formation and uniform distribution of Mg17Al12 phase along the grain boundary for laser surface-treated samples. Evolution of such unique microstructure during laser surface treatment indicated enhancement in the corrosion resistance of laser surface-treated samples compared to untreated alloy.

Enhanced mechanical properties and increased corrosion resistance of a biodegradable magnesium alloy by plasma electrolytic oxidation (PEO).

We report the enhanced mechanical properties of AZ31 magnesium alloys by plasma electrolytic oxidation (PEO) coating in NaOH, Na2SiO3, KF and NaH2PO4·2H2O containing electrolytes. Mechanical properties including wear resistance, surface hardness and elastic modulus were increased for PEO-coated AZ31 Mg alloys (PEO-AZ31). DC polarization in Hank's solution indicating that the corrosion resistance significantly increased for PEO-coating in KF-contained electrolyte. Based on these results, the PEO coating method shows promising potential for use in biodegradable implant applications where tunable corrosion and mechanical properties are needed.

Deformation Behavior of AZ31 Magnesium Alloy with Pre-Twins under Biaxial Tension.

In the present study, the mechanical response and deformation behavior of a Mg AZ31 plate with different types of pre-twins was systematically investigated under biaxial tension along the normal direction (ND) and transverse direction (TD) with different stress ratios. The results show that significant hardening was observed under biaxial tension. The yield values in the direction of larger stress values were higher than those under uniaxial loading conditions, and the solute atom segregation at twin boundaries generates more obvious strengthening effect. Noting that, for TRH (with cross compression along the rolling direction (RD) and TD and annealing at 180 °C for about 0.5 h) sample, the strength effect of the RD yield stress σRD:σND = 2:1 was higher than that of the ND yield stress under stress ratio σRD:σND = 1:2. There is a complex competition between twinning and detwinning under biaxal tension along the ND and TD of the pre-twinned samples with the variation in the stress ratio along the TD and RD. The variation in the twin volume fractions for all samples under biaxial firstly decreases and then increases with a higher stress ratio along the ND. As for the TDH sample (precompression along the TD and annealing), the changes of the twin volume fraction were lower than that of the TR sample (cross compression along the TD and RD). However, the amplitude of variation in twin volume fraction of the TRH sample is higher than that of the TR sample. This is because the relative activity of detwinning decreases and that of twinning increases, as the ND stress mainly leads to the growth of pre-twins and the TD stress often promotes detwinning of primary twins. With a higher stress ratio along the ND, the activity of twinning deformation increases and that of detwinning decreases.

Experimental investigation on characterization of friction stir processed AZ31-based composite.

Present study has been conducted to characterize the Mg alloy namely AZ31-based composite joined by Friction stir processing (FSP) technique. This study deals with the effect of single and double passes in FSP of AZ31 Mg alloy. The single pass run in FSP is followed at tool rotation speed (N) of 1000 to 1400 rpm. Also, the double pass run in FSP was followed at these speeds without using reinforcements. The feedstock particles namely SiC, Al2O3, Cr, and Si powders were used in fabrication process. The hardness, impact strength, and tensile strength characteristics were assessed in the stir region zone, and the results indicated significant improvement in these properties. The highest values of mechanical strength were seen in the FSPed area with N = 1000 rpm at a constant transverse speed (r) of 40 mm/min. Also, the tensile strength of the two passes FSPed plates is much higher than that of the single section without any reinforcement, as revealed in previous study also. The Scanning electron microscopy (SEM) analysis is done at two different magnifications for the Silicon carbide, Alumina, Chromium, and Silicon powder reinforced composites fabricated at speed of 1000 rpm. The microstructure shows that reinforced particles were uniform dispersed into FSPed region and agglomerated with Mg matrix. Si powder produces finer microstructure as compare to SiC, Al2O3, Cr. FSP decreases the grain size of processed material. Optical Microscopy results revealed that the reinforcement particle produced a homogenous microstructure and, a refined grain and equally dispersed in matrix material without split to the particle.

Microstructure and Corrosion of Mg-Based Composites Produced from Custom-Made Powders of AZ31 and Ti6Al4V via Pulse Plasma Sintering.

Magnesium (Mg) and its alloys offer promise for aerospace, railway, and 3D technology applications, yet their inherent limitations, including inadequate strength, pose challenges. Magnesium matrix composites, particularly with metallic reinforcements like titanium (Ti) and its alloys, present a viable solution. Therefore, this study investigates the impact of Ti6Al4V reinforcement on AZ31 magnesium alloy composites produced using pulse plasma sintering (PPS). Results show enhanced microhardness of the materials due to improved densification and microstructural refinement. However, Ti6Al4V addition decreased corrosion resistance, leading to strong microgalvanic corrosion and substrate dissolution. Understanding these effects is crucial for designing Mg-based materials for industries like petrochemicals, where degradation-resistant materials are vital for high-pressure environments. This research provides valuable insights into developing Mg-Ti6Al4V composites with tailored properties for diverse industrial applications, highlighting the importance of considering corrosion behavior in material design. Further investigation is warranted to establish predictive correlations between Ti6Al4V content and corrosion rate for optimizing composite performance.

Improvement of mechanical performance on zirconium dioxide nanoparticle synthesized magnesium alloy nano composite.

With excellent mechanical properties and distinct solidification, the AZ31B series magnesium alloy has great potential for targeting engineering applications and synthesized via die casting process found a drawback on oxidation results porosity and reduced mechanical properties. Here, the magnesium alloy AZ31B series nanocomposite was synthesized with varied weight percentages of zirconium dioxide nanoparticles through a liquid metallurgy route with an applied stir speed of 200 rpm under an argon nature. With the help of a scanning electron microscope, the distribution of particles in the composite surface was found to be homogenous and void-free surface, which output results in less percentage of porosity (<1 %), and the composite contained 6 wt% ZrO2 offers superior yield strength (212 ± 3 MPa), tensile strength (278 ± 2 MPa), and impact strength of 16.4 ± 0.4 J/mm2. In addition, 8 wt% ZrO2 blended composite showed the maximum microhardness value (78.3 ± 1 HV). The best-enhanced result of NC3 (AZ31B/6 wt% ZrO2) is suggested for lightweight to high-strength structural applications.

Investigation of Synthesis, Characterization, and Finishing Applications of Spherical Al2O3 Magnetic Abrasives via Plasma Molten Metal Powder and Powder Jetting.

Magnetic abrasive finishing (MAF) is an efficient finishing process method using magnetic abrasive particles (MAPs) as finishing tools. In this study, two iron-based alumina magnetic abrasives with different particle size ranges were synthesized by the plasma molten metal powder and powder jetting method. Characterization of the magnetic abrasives in terms of microscopic morphology, phase composition, magnetic permeability, particle size distribution, and abrasive ability shows that the magnetic abrasives are spherical in shape, that the hard abrasives are combined in the surface layer of the iron matrix and remain sharp, and that the hard abrasives combined in the surface layer of the magnetic abrasives with smaller particle sizes are sparser than those of the magnetic abrasives with larger particle sizes. The magnetic abrasives are composed of α-Fe and Al2O3; the magnetic permeability of the magnetic abrasives having smaller particle sizes is slightly higher than that of the magnetic abrasives having larger particle sizes; the two magnetic abrasives are distributed in a range of different particle sizes; the magnetic abrasives have different magnetic permeabilities, which are higher than those of the larger ones; both magnetic abrasives are distributed in the range of smaller particle sizes; and AZ31B alloy can obtain smaller surface roughness of the workpiece after the grinding process of the magnetic abrasives with a small particle size.

Effect of Welding Parameters on Al/Mg Dissimilar Friction Stir Lap Welding with and without Ultrasonic Vibration.

The amount of heat input during welding impacts the weld's thermal and mechanical behavior and the joint's properties. The current study involved conducting AA 6061 and AZ31B Mg dissimilar welding, using friction stir lap welding (FSLW) and ultrasonic vibration-enhanced FSLW (UVeFSLW). The comparison and analysis of the welding load, the weld's macro-microstructure, intermetallic compounds (IMCs), and joint properties were conducted by adjusting the process parameters. The study also examined the effect of ultrasonic vibration (UV) variations on welding heat input. The study demonstrated that it is possible to reduce the welding load by employing UV. Moreover, this impact becomes more pronounced as the welding heat input decreases. Additionally, the material flow in the weld, the width of the weld nugget zone, and the continuous IMC layer are significantly influenced by ultrasonic vibration, irrespective of the heat input during welding. However, the impact on large areas of irregular IMCs or eutectic structures is relatively small. Furthermore, achieving better joint properties becomes more feasible when a higher welding speed is employed for the Al alloy placed on top. Specifically, the impact of UV becomes more evident at higher welding speeds (≥220 mm/min).

Phase Field Simulation of the Effect of Second Phase Particles with Different Orientations on the Microstructure of Magnesium Alloys.

In this study, the phase field method has been used to study the effect of second phase particles with different shapes and different orientations on the grain growth of AZ31 magnesium alloy, after annealing at 350 °C for 100 min. The results show that the shape of the second phase particles would have an effect on the grain growth; the refinement effect of elliptical particles and rod-shaped particles was similar, and better than the spherical particles; the spatial arrangement direction of the second phase particles had no significant effect on the grain growth. On the other hand, when the microstructure of AZ31 magnesium alloy contained second phase particles with different shapes, the effect of mixing different shapes of second phase particles on the grain refinement was enhanced gradually with the decrease im the volume fraction of spherical particles.

Effect of Plasma Argon Pretreatment on the Surface Properties of AZ31 Magnesium Alloy.

Climate change has evidenced the need to reduce carbon dioxide emissions into the atmosphere, and so for transport applications, lighter weight alloys have been studied, such as magnesium alloys. However, they are susceptible to corrosion; therefore, surface treatments have been extensively studied. In this work, the influence of argon plasma pretreatment on the surface properties of an AZ31 magnesium alloy focus on the enhancement of the reactivity of the surface, which was examined by surface analysis techniques, electrochemical techniques, and gravimetric measurements. The samples were polished and exposed to argon plasma for two minutes in order to activate the surface. Contact angle measurements revealed higher surface energy after applying the pretreatment, and atomic force microscopy showed a roughness increase, while X-Ray photoelectron spectroscopy showed a chemical change on the surface, where after pretreatment the oxygen species increased. Electrochemical measurements showed that surface pretreatment does not affect the corrosion mechanism of the alloy, while electrochemical impedance spectroscopy reveals an increase in the original thickness of the surface film. This increase is likely associated with the high reactivity that the plasma pretreatment confers to the surface of the AZ31 alloy, affecting the extent of oxide formation and, consequently, the increase in its protection capacity. The weight loss measurements support the effect of the plasma pretreatment on the oxide thickness since the corrosion rate of the pretreated AZ31 specimens was lower than that of those that did not receive the surface pretreatment.

Effect of Recrystallization Behavior of AZ31 Magnesium Alloy on Damping Capacity.

For a wide industrial application of magnesium alloys, a method for imparting high damping properties while maintaining mechanical properties is required. Controlling the crystallographic texture seems to be useful, because dislocations are known to have a significant influence on the damping characteristics of magnesium alloys. In addition, textures are affected by the microstructure and texture variation when the deformation or annealing is applied. However, there were less reports about their effect on damping capacity. Therefore, the effect of twinning and annealing, which can affect the recrystallization, were investigated in this study. An AZ31 alloy was hot rolled at 673 K with a reduction ratio of 10% and 50%, and then annealed at 673 K and 723 K for 0.5, 1, 2, and 3 h, respectively. SEM-EBSD was used to examine the microstructure and texture. In addition, each specimen's hardness and internal friction were contemporarily measured. As a result, hot rolling produced tensile twins and their fraction increased with internal friction when the reduction ratio increased. Due to annealing, a discontinuous type of static recrystallization occurred within the twinning grains, and was highly activated along with the increasing annealing temperature and the fraction of twinning. In the samples annealed at 723 K, the internal friction continuously increased over the annealing time, whereas in the samples annealed at 673 K, the decrease in dislocation density was delayed while the internal friction showed a relatively low value.

Microstructure and Salt Fog Corrosion of Wrought Mg-Al-Zn and Mg-RE Alloys.

Wrought magnesium alloys have received attention due to their potential application as lightweight materials. However, their use is limited by their poor corrosion resistance. Rare earth additions have the potential to enhance corrosion resistance. The present work included a microstructural investigation and corrosion testing of the alloy WE-43, containing Nd and Y, which was compared against the more conventional compositions of AZ31 and AZ61 alloys. All three alloys exhibited a recrystallized equiaxed structure after hot rolling with the presence of second phases-precipitates. The WE-43 alloy exhibited a better corrosion resistance than AZ31 and AZ61 under salt fog testing, indicated by the lower depth of attack and lower weight loss. The second phases in the microstructure of AZ31 and AZ61 alloys determined their corrosion resistance. The second phases in the AZ31 and AZ61 alloys (based on Al-Mg and Al-Mn phases) were nobler than the Mg matrix and catholically acted, thus sacrificing the Mg matrix. The superior corrosion resistance of WE43 was due to the incorporation of Y in the oxide/hydroxide film. In addition, the second phases in the WE43 consisted of Nd and Y and were less noble than the Mg-matrix. Thus, they acted as anodic sites protecting the Mg-matrix. The above results show the beneficial effect of rare earth additions to wrought Mg alloys towards increased corrosion resistance.

Texture and High Yield Strength of Rapidly Solidified AZ31 Magnesium Alloy Extruded at 250 °C.

In this study, commercial AZ31B magnesium alloy was used to compare the differences between the microstructure, texture, and mechanical properties of conventional solidification (as homogenized AZ31) and rapid solidification (as RS AZ31). The results demonstrate that a rapidly solidified microstructure leads to better performance after hot extrusion with a medium extrusion rate (6 m/min) and extrusion temperature (250 °C). The average grain size of as-homogenized AZ31 extruded rod is 100 µm after annealing and 4.6 µm after extrusion, respectively, but that of the as-RS AZ31 extruded rod is only about 5 µm and 1.1 µm, correspondingly. The as-RS AZ31 extruded rod attains a high average yield strength of 289.6 MPa, which is superior to the as-homogenized AZ31 extruded rod, and is improved by 81.3% in comparison. The as-RS AZ31 extruded rod shows a more random crystallographic orientation and has an unconventional weak texture component in <112¯1>/<202¯1> direction, which has not been reported yet, while the as-homogenized AZ31 extruded rod has an expected texture with prismatic <101¯0>/<1¯21¯0>//ED.

Enhancing bone formation using absorbable AZ31B magnesium alloy membranes during distraction osteogenesis: A new material study.

Purpose: To investigate whether the use of absorble AZ31B magnesium alloys over distraction gaps improves the quality and quantity of regenerated bone better than the use of Collagen membranes. Methods: Fifteen mixed-breed dogs were randomly divided into the experimental (n = 10) and control (n = 5) groups. In the experimental group, two devices were implanted along the mandible; one side with absorble AZ31B and the other side with Collagen. The control animals did not undergo osteotomy or distraction. After a consolidation time of two months, 30 specimens were harvested, and newly created bone was identified using CBCT and micro-CT. Results: The Collagen membranes were absorbed completely, and the AZ31B membranes became irregular and rough. Mandible length was successfully extended approximately 1 cm. More bone formation was found after using AZ31B than Collagen, and there was a significant difference in width reduction between experimental sites treated with AZ31B (0.11 ± 0.04 cm) and Collagen (0.42 ± 0.06 cm) (p < 0.05). Trabecular thickness was also significantly higher in AZ31B (0.338 ± 0.08 cm) and control (0.417 ± 0.05 cm) than Collagen (0.178 ± 0.04 cm) (p < 0.05). Conclusion: An AZ31B membrane barrier is biocompatible and absorbable which can maintain the distraction gap and provide support to the attached osteoprogenitors by providing space for them to proliferate.

The Influence of Heat and Cryogenic Treatment on Microstructure Evolution and Mechanical Properties of Laser-Welded AZ31B.

The pores and coarse lamellar Mg17Al12 that inevitably occur in the weld zone are the major challenge for laser-welded magnesium (Mg) alloys including AZ31B. In order to improve microstructure uniformity and eliminate welding defects, a new process assisted with combination of heat and cryogenic treatment was applied in this study. The results showed that after solution treatment, the number and size of precipitates decreased and the uniformity of the microstructure improved. After cryogenic treatment, the lamellar Mg17Al12 was cracked into particles, and the grain size was refined. After solution + cryogenic treatment, Al8Mn5 substituted the lamellar Mg17Al12. Through studying the changes in microhardness, precipitates, and microstructure under different treatments, it was found that the conversation of Mg17Al12 from lamellar state into particle-like state as well as the appearance of dispersed Al8Mn5 particles played a second-phase strengthening role in improving the mechanical properties of Mg alloy laser-welded joint, and the tensile strength (258.60 MPa) and elongation (10.90%) of the sample were 4.4% and 32.6% higher than those of the as-welded joint.

Warm Deformation Behavior and Flow Stress Modeling of AZ31B Magnesium Alloy under Tensile Deformation.

Constitutive equations were recognized for AZ31B magnesium alloy at higher temperatures and strain rates from conventional empirical models like the original Johnson-Cook (JC), modified JC, and modified Zerilli-Armstrong (ZA) models for capturing the material warm deformation behavior. Uniaxial warm tensile tests were performed at temperatures (50 to 250 °C) and strain rates (0.005 to 0.0167 s-1) to probe AZ31 magnesium alloy flow stress values. Depending on the calculated flow stress, constitutive equations were recognized, and these established models were assessed by the coefficient of determination (R2), relative mean square error (RMSE), and average absolute relative error (AARE) metrics. The results demonstrated that the flow stress calculated by the modified JC and ZA models revealed good agreement against the test data. Thus, the outcomes confirmed that the recognized modified JC and modified ZA models could effectively forecast AZ31 magnesium alloy flow behavior by capturing the material deformation behavior accurately.

Hybrid Artificial Neural Network-Based Models to Investigate Deformation Behavior of AZ31B Magnesium Alloy at Warm Tensile Deformation.

The uniaxial warm tensile experiments were carried out in deformation temperatures (50-250 °C) and strain rates (0.005 to 0.0167 s-1) to investigate the material workability and to predict flow stress of AZ31B magnesium alloy. The back-propagation artificial neural network (BP-ANN) model, a hybrid models with a genetic algorithm (GABP-ANN), and a constrained nonlinear function (CFBP-ANN) were investigated. In order to train the exploited machine learning models, the process parameters such as strain, strain rate, and temperature were accounted as inputs and flow stress was considered as output; moreover, the experimental flow stress values were also normalized to constructively run the neural networks and to achieve better generalization and stabilization in the trained network. Additionally, the proposed model's closeness and validness were quantified by coefficient of determination (R2), relative mean square error (RMSE), and average absolute relative error (AARE) metrics. The computed statistical outcomes disclose that the flow stress predicted by both GABP-ANN and CFBP-ANN models exhibited better closeness with the experimental data. Moreover, compared with the GABP-ANN model outcomes, the CFBP-ANN model has a relatively higher predictability. Thus, the outcomes confirm that the proposed CFBP-ANN model can result in the accurate description of AZ31 magnesium alloy deformation behavior, showing potential for the purpose of practicing finite element analysis.