Effects of friction stir processing and nano-hydroxyapatite on the microstructure,hardness,degradation rate and in-vitro bioactivity of WE43 alloy for biomedical applications

Nowadays,magnesium alloys are emerging in biomedical implants for their similar properties to natural bones.However,the rapid degradation of magnesium alloys in biological media hinders successful implantation.Refinement of microstructure,as well as reinforcement particles can significantly improve the degradation rate.In this work,multi-pass friction stir processing(FSP)was proposed to synthesize WE43/nano-hydroxyapatite(n HA)surface composite,the microstructure,reinforced particle distribution,micro-hardness,corrosion behavior and in-vitro bioactivity were studied.The subsequent FSP passes of WE43 alloy and WE43/n HA composite refined the grain size which was reduced by 94.29%and 95.92%(2.63 and 1.88μm,respectively)compared to base metal after three passes.This resulted in increasing the microhardness by 120%(90.86 HV0.1)and 135%(105.59 HV0.1)for the WE43 and WE43-n HA,respectively.It is found that increasing FSP passes improved the uniform distribution of n HA particles within the composite matrix which led to improved corrosion resistance and less degradation rate.The corrosion rate of the FSPed WE43/n HA composite after three passes was reduced by 38.2%(4.13 mm/year)and the degradation rate was reduced by 69.7%(2.87 mm/y).This is attributed to secondary phase(Mg24Y5and Mg41Nd5)particle fragmentation and redistribution,as well as a homogeneous distribution of n HA.Additionally,the growing Ca-P and Mg(OH)2layer formed on the surface represented a protective layer that reduced the degradation rate.The wettability test revealed a relatively hydrophilic surface with water contact angle of 49.1±2.2°compared to 71.2±2.1°for base metal.Also,biomineralization test showed that apatite layer grew after immersion 7d in simulated body fluid with atomic ratio of Ca/P 1.60 approaching the stoichiometric ratio(1.67)indicating superior bioactivity of FSPed WE43/n HA composite after three passes.These results raise that the grain refinement by FSP and introduction of n HA particles significantly improved the degradation rate and in-vitro bioactivity of WE43 alloy for biomedical applications.

A new insight into LPSO phase transformation and mechanical properties uniformity of large-scale Mg-Gd-Y-Zn-Zr alloy prepared by multi-pass friction stir processing

A large-scale fine-grained Mg-Gd-Y-Zn-Zr alloy plate with high strength and ductility was successfully prepared by multi-pass friction stir processing(MFSP)technology in this work.The structure of grains and long period stacking ordered(LPSO)phase were characterized,and the mechanical properties uniformity was investigated.Moreover,a quantitative relationship between the microstructure and tensile yield strength was established.The results showed that the grains in the processed zone(PZ)and interfacial zone(IZ)were refined from 50μm to 3μm and 4μm,respectively,and numerous original LPSO phases were broken.In IZ,some block-shaped 18R LPSO phases were transformed into needle-like 14H LPSO phases due to stacking faults and the short-range diffusion of solute atoms.The severe shear deformation in the form of kinetic energy caused profuse stacking fault to be generated and move rapidly,greatly increasing the transformation rate of LPSO phase.After MFSP,the ultimate tensile strength,yield strength and elongation to failure of the large-scale plate were 367 MPa,305 MPa and 18.0% respectively.Grain refinement and LPSO phase strengthening were the major strengthening mechanisms for the MFSP sample.In particularly,the strength of IZ was comparable to that of PZ because the strength contribution of the 14H LPSO phase offsets the lack of grain refinement strengthening in IZ.This result opposes the widely accepted notion that IZ is a weak region in MFSP-prepared large-scale fine-grained plate.

Prediction of corrosion rate for friction stir processed WE43 alloy by combining PSO-based virtual sample generation and machine learning

The corrosion rate is a crucial factor that impacts the longevity of materials in different applications.After undergoing friction stir processing(FSP),the refined grain structure leads to a notable decrease in corrosion rate.However,a better understanding of the correlation between the FSP process parameters and the corrosion rate is still lacking.The current study used machine learning to establish the relationship between the corrosion rate and FSP process parameters(rotational speed,traverse speed,and shoulder diameter)for WE43 alloy.The Taguchi L27 design of experiments was used for the experimental analysis.In addition,synthetic data was generated using particle swarm optimization for virtual sample generation(VSG).The application of VSG has led to an increase in the prediction accuracy of machine learning models.A sensitivity analysis was performed using Shapley Additive Explanations to determine the key factors affecting the corrosion rate.The shoulder diameter had a significant impact in comparison to the traverse speed.A graphical user interface(GUI)has been created to predict the corrosion rate using the identified factors.This study focuses on the WE43 alloy,but its findings can also be used to predict the corrosion rate of other magnesium alloys.

Microstructural evolution and its influence on mechanical and corrosion behaviors in a high-Al/Zn containing duplex Mg-Li alloy after friction stir processing

Ultralight Mg-Li alloys offer promising applications across various fields.Mg-Li alloys enriched with Al and Zn hold theoretical potential for achieving excellent mechanical strength and corrosion resistance.However,the structural and performance characteristics of such Mg-Li alloys,particularly after thermo-mechanical processing,remain inadequately explored and understood.This study investigated the mi-crostructural evolution of a Mg-9Li-5Al-4Zn alloy after friction stir processing and its consequent effects on the mechanical and corrosion performance.The grain size of the alloy was effectively refined and sta-bilized during friction stir processing at various heat inputs.The yield strength of the alloy increased by 86.4%after friction stir processing under the highest heat input condition,which was attributed to fine grain strengthening,solid solution strengthening and dispersion strengthening.Concurrently,the alloy ex-perienced a slight decrease in elongation after the friction stir processing.The alloy subjected to friction stir processing with the highest heat input exhibited a minimal corrosion current density of 6.10×10^(−6) A/cm^(2),which was only 25%of the base metal.The enhanced anti-corrosion properties can be attributed to the dispersion and distribution of precipitated particles induced by friction stir processing,which hin-dered the micro-galvanic corrosion and promoted the generation of a compact surface film,leading to minimal and uniform corrosion.This investigation can be significant for understanding the metallurgical mechanisms and performance evolution of Mg-Li alloys during thermomechanical processes.

Predicting grain size-dependent superplastic properties in friction stir processed ZK30 magnesium alloy with machine learning methods

The aim of this work is to predict,for the first time,the high temperature flow stress dependency with the grain size and the underlaid deformation mechanism using two machine learning models,random forest(RF)and artificial neural network(ANN).With that purpose,a ZK30 magnesium alloy was friction stir processed(FSP)using three different severe conditions to obtain fine grain microstructures(with average grain sizes between 2 and 3μm)prone to extensive superplastic response.The three friction stir processed samples clearly deformed by grain boundary sliding(GBS)deformation mechanism at high temperatures.The maximum elongations to failure,well over 400% at high strain rate of 10^(-2)s^(-1),were reached at 400℃ in the material with coarsest grain size of 2.8μm,and at 300℃ for the finest grain size of 2μm.Nevertheless,the superplastic response decreased at 350℃ and 400℃ due to thermal instabilities and grain coarsening,which makes it difficult to assess the operative deformation mechanism at such temperatures.This work highlights that the machine learning models considered,especially the ANN model with higher accuracy in predicting flow stress values,allow determining adequately the superplastic creep behavior including other possible grain size scenarios.

Microstructural evolution and hot tensile behavior of Mg−3Zn−0.5Zr alloy subjected to multi-pass friction stir processing

The microstructures and hot tensile behaviors of ZK30 alloys subjected to single-and multi-pass friction stir processing(FSP)were systematically investigated.Following single-pass FSP(S-FSP),coarse grains underwent refinement to 1−2μm,with a distinct basal texture emerging in the stir zone(SZ).Additionally,second-phase particles were fragmented,dispersed,and partially dissolved.Multi-pass FSP(M-FSP)further enhanced the homogeneity of the microstructure,reduced texture intensity differences,and decreased the fraction of second-phase particles by 50%.Both S-FSP and M-FSP SZs demonstrated superplasticity at strain rates below 1×10^(−3)s^(−1)and at temperatures of 250−350℃.The S-FSP SZ exhibited an elongation of 390%at 250℃and 1×10^(−4)s^(−1),while the M-FSP SZ achieved an elongation of 406%at 350℃and 1×10^(−3)s^(−1).The superplastic deformation of SZ was co-dominated by grain boundary sliding(GBS)and the solute-drag mechanism in S-FSP and mainly by GBS in M-FSP.

Research progress in friction stir processing of magnesium alloys and their metal matrix surface composites: Evolution in the 21^(st )century

Rising concerns about climate change drive the demand for lightweight components.Magnesium(Mg)alloys are highly valued for their low weight,making them increasingly important in various industries.Researchers focusing on enhancing the characteristics of Mg alloys and developing their Metal Matrix Composites(MMCs)have gained significant attention worldwide over the past decade,driven by the global shift towards lightweight materials.Friction Stir Processing(FSP)has emerged as a promising technique to enhance the properties of Mg alloys and produce Mg-MMCs.Initially,FSP adapted to refine grain size from the micro to the nano level and accelerated the development of MMCs due to its solid-state nature and the synergistic effects of microstructure refinement and reinforcement,improving strength,hardness,ductility,wear resistance,corrosion resistance,and fatigue strength.However,producing defect-free and sound FSPed Mg and Mg-MMCs requires addressing several variables and their interdependencies,which opens up a broad range of practical applications.Despite existing reviews on individual FSP of Mg,its alloys,and MMCs,an attempt has been made to analyze the latest research on these three aspects collectively to enhance the understanding,application,and effectiveness of FSP for Mg and its derivatives.This review article discusses the literature,classifies the importance of Mg alloys,provides a historical background,and explores developments and potential applications of FSPed Mg alloys.It focuses on novel fabrication methods,reinforcement strategies,machine and tool design parameters,material characterization,and integration with other methods for enhanced properties.The influence of process parameters and the emergence of defects are examined,along with specific applications in mono and hybrid composites and their microstructure evolution.The study identifies promising reinforcement materials and highlights research gaps in FSP for Mg alloys and MMCs production.It concludes with significant recommendations for further exploration,reflecting ongoing advancements in this field.

Tailoring the microstructure of Mg-Al-Sn-RE alloy via friction stir processing and the impact on its electrochemical discharge behaviour as the anode for Mg-air battery

Constructing the magnesium alloy with fine grains,low density of dislocations,and weak crystal orientation is of crucial importance to enhance its comprehensive performance as the anode for Mg-air battery.However,this unique microstructure can hardly be achieved with conventional plastic deformation such as rolling or extrusion.Herein,we tailor the microstructure of Mg-Al-Sn-RE alloy by using the friction stir processing,which obviously refines the grains without increasing dislocation density or strengthening crystal orientation.The Mg-air battery with the processed Mg-Al-Sn-RE alloy as the anode exhibits higher discharge voltages and capacities than that employing the untreated anode.Furthermore,the impact of friction stir processing on the electrochemical discharge behaviour of Mg-Al-Sn-RE anode and the corresponding mechanism are also analysed according to microstructure characterization and electrochemical response.

Superplasticity of AZ31 magnesium alloy prepared by friction stir processing

Microstructure and tensile behaviors of AZ31 magnesium alloy prepared by friction stir processing（FSP） were investigated.The results show that microstructure of the AZ31 hot-rolled plate with an average grain size of 92.0 μm is refined to 11.4 μm after FSP.The FSP AZ31 alloy exhibits excellent plasticity at elevated temperature,with an elongation to failure of 1050% at 723 K and a strain rate of 5×10-4 s-1.The elongation of the FSP material is 268% at 723 K and 1×10-2 s-1,indicating that high strain rate superplasticity could be achieved.On the other hand,the hot-rolled base material,which has a coarse grain structure,possesses no superplasticity under the experimental conditions.

Preparation of ultra-fine grain Ni-Al-WC coating with interlocking bonding on austenitic stainless steel by laser clad and friction stir processing

The ultra-fine structured Ni?Al?WC layer with interlocking bonding was fabricated on austenitic stainless steel by combination of laser clad and friction stir processing (FSP). Laser was initially applied to Ni?Al elemental powder preplaced on the austenitic stainless steel substrate to produce a coating for further processing. The as-received coating was subjected to FSP treatment, processed by a rotary tool rod made of WC?Co alloy, to obtain sample for inspection. Microstructure, phase constitutions, hardness and wear property were investigated by methods of scanning electronic microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDX) microanalysis, and X-ray diffraction (XRD), hardness test alongside with dry sliding wear test. The results show that the severe deformation effect exerted on the specimen resulted in an ultra-fine grain layer of about 100μmin thickness and grain size of 1?2μm. Synergy between introduction of WC particles to the deformation layer and deformation strengthening contributes greatly to the increase in hardness and friction resistance. An interlocking bonding between the coating and matrix which significantly improves bonding strength was formed due to the severe deformation effect.

Evolution of microstructure and hardness of aluminum after friction stir processing

The effects of friction stir processing （FSP） on the microstructure, microtexture and hardness of rolled pure aluminum were investigated. The microstructure and microtexture were characterized using electron backscattered diffraction （EBSD） technique on the transversal section. The stir zone （SZ） contains fine, equiaxed and fully recrystallized grains. The texture component of the base material mainly consists of R, S and brass R textures. Miner copper texture component is also determined. In the center of the stir zone, the dominant texture is （111） parallel to about 70° from ND pointing toward RD. The textures of this location rotating clockwise about 30° and anticlockwise about 60° around the ND result in the textures of the areas, which are 3 mm apart from this location on the retreating side and advancing side, respectively.

Influence of bimodal grain size distribution on the corrosion behavior of friction stir processed biodegradable AZ31 magnesium alloy

In the present study,AZ31 magnesium alloy sheets were processed by friction stir processing(FSP)to investigate the effect of the grain refinement and grain size distribution on the corrosion behavior.Grain refinement from a starting size of 16.4±6.8µm to 3.2±1.2µm was attained after FSP.Remarkably,bimodal grain size distribution was observed in the nugget zone with a combination of coarse(11.62±8.4µm)and fine grains(3.2±1.2µm).Due to the grain refinement,a slight improvement in the hardness was found in the nugget zone of FSPed AZ31.The bimodal grain size distribution in the stir zone showed pronounced influence on the corrosion rate of FSPed AZ31 as observed from the immersion and electrochemical tests.From the X-ray diffraction analysis,more amount of Mg(OH)_(2) was observed on FSPed AZ31 compared with the unprocessed AZ31.Polarization measurements demonstrated the higher corrosion current density for FSPed AZ31(8.92×10^(−5)A/cm^(2))compared with the unprocessed condition(2.90×10^(−5)A/cm^(2))that can be attributed to the texture effect and large variations in the grain size which led to non-uniform galvanic intensities.

A comparative study on microstructural evolution and surface properties of graphene/CNT reinforced Al6061-SiC hybrid surface composite fabricated via friction stir processing

A comparative study on the surface properties of Al-SiC-multi walled carbon nanotubes (CNT) and Al-SiC-graphene nanoplatelets (GNP) hybrid composites fabricated via friction stir processing (FSP) was documented. Microstructural characterization reveals a more homogeneous dispersion of GNPs in the Al matrix as compared to CNTs. Dislocation blockade by SiC and GNP particles along with the defect-free interface between the matrix and reinforcements is also observed. Nanoindentation study reveals a remarkable ~207% and ~27% increment in surface nano-hardness of Al-SiC-GNP and Al-SiC-CNT hybrid composite compared to as-received Al6061 alloy, respectively. On the other hand, the microhardness values of Al-SiC-GNP and Al-SiC-CNT are increased by ~36% and ~17% relative to as-received Al6061 alloy, respectively. Tribological assessment reveals ~56% decrease in the specific wear rate of Al-SiC-GNP hybrid composite, whereas it is increased by ~122% in Al-SiC-CNT composite. The higher strength of Al-SiC-GNP composite is attributed to the mechanical exfoliation of GNPs to few layered graphene (FLG) in the presence of SiC. Also, various mechanisms such as thermal mismatch, grain refinement, and Orowan looping contribute significantly towards the strengthening of composites. Moreover, the formation of tribolayer by the squeezed-out GNP on the surface is responsible for the improved tribological performance of the composites. Raman spectroscopy and various other characterization methods corroborate the results.

Synthesize of AZ31/TiC magnesium matrix composites using friction stir processing

Friction stir processing(FSP)is a novel solid state technique to synthesize metal matrix composites.In the present work,an attempt has been made to synthesize AZ31/TiC magnesium matrix composites using FSP and to analyze the microstructure using scanning electron microscopy.A groove was prepared on 6 mm thick AZ31 magnesium alloy plates and compacted with TiC particles.The width of the groove was varied to result in four different volume fraction of TiC particles(0,6,12 and 18 vol.%).A single pass FSP was carried out using a tool rotational speed of 1200 rpm,traverse speed of 40 mm/min and an axial force of 10 kN.Scanning electron microscopy was employed to study the microstructure of the synthesized composites.The results indicated that TiC particles were distributed uniformly in the magnesium matrix without the formation of clusters.There was no interfacial reaction between the magnesium matrix and the TiC particle.TiC particles were properly bonded to the magnesium matrix.

Assessment of Ti-6Al-4V particles as a reinforcement for AZ31 magnesium alloy-based composites to boost ductility incorporated through friction stir processing

Poor ductility is the primary concern of magnesium matrix composites(MMCs)inflicted by non-deformable ceramic particle reinforcements.Metal particles which melt at elevated temperature can be used as reinforcement to improve the deformation characteristics.Ti-6Al-4V particles reinforced AZ31 MMCs were produced through friction stir processing(FSP)which was carried out in a traditional vertical milling machine.The microstructural features as well as the response to external tensile load were explored.A homogenous distribution of Ti-6Al-4V was achieved at every part of the stir zone.There was no chemical decomposition of Ti-6Al-4V.Further,Ti-6Al-4V did not react with Al and Zn present in AZ31 alloy to form new compounds.A continuous strong interface was obtained around Ti-6Al-4V particle with the matrix.Ti-6Al-4V particles underwent breakage during processing due to severe plastic strain.There was a remarkable refinement of grains in the composite caused by dynamic recrystallization in addition to the pinning of smaller size broken particles.Dense dislocations were observed in the matrix because of plastic deformation and the associated strain misfit.Ti-6Al-4V particles improved the tensile behavior and assisted to obtain appreciable deformation before fracture.Brittle mode of failure was avoided.

Microstructures and mechanical properties of friction stir processed Mge2.0Nde0.3Zne1.0Zr magnesium alloy

The effect of Friction stir process(FSP)parameters on the microstructure and mechanical properties of an extruded Mge2.0Nde0.3Zne1.0Zr(wt.%)alloy was investigated in this paper.The alloy was friction stir processed with different passes:single-pass,three-pass and five-pass,under a tool rotation rate of 800μm and a traverse speed of 200 mm min^(-1).FSP results in remarkable grain refinement of the extruded alloy(average grain size w3.8 mm as 3 passes)and almost complete dissolution of the Mg_(12)Nd phase in the matrix.With the increase of pass,the average grain size in the stir zone(SZ)is decreased firstly and then increases.The Vikers hardness of SZs in all FSPed samples is higher than that of the parent material(PM).Tensile tests at room-temperature show that the tensile strengths of the stir zones along the FSP advancing direction are slightly lower than those of PM.However,the elongations are remarkably improved from 13.0%for PM to 24.5%for SZ FSPed with three-passes.These improved tensile properties are attributed to the microstructure refinement,dynamic recrystallization and dissolution of the Mg_(12)Nd phase.

Magnesium based surface metal matrix composites by friction stir processing

Surface metal matrix composites(MMCs)are a group of modern engineered materials where the surface of the material is modified by dispersing secondary phase in the form of particles or fibers and the core of the material experience no change in chemical composition and structure.The potential applications of the surface MMCs can be found in automotive,aerospace,biomedical and power industries.Recently,friction stir processing(FSP)technique has been gaining wide popularity in producing surface composites in solid state itself.Magnesium and its alloys being difficult to process metals also have been successfully processed by FSP to fabricate surface MMCs.The aim of the present paper is to provide a comprehensive summary of state-of-the-art in fabricating magnesium based composites by FSP.Influence of the secondary phase particles and grain refinement resulted from FSP on the properties of these composites is also discussed.

Improvement in grain refinement efficiency of Mg-Zr master alloy for magnesium alloy by friction stir processing

Previous studies have proved that the zirconium(Zr)alloying and grain refining performance of a Mg-Zr master alloy on Mg alloy is closely related to the distribution of Zr particle size,and a Mg-Zr master alloy with more Zr particles in size range of 1-5μm exhibits a better refining efficiency.In this paper,friction stir processing(FSP)was used to modify the Zr particles size distribution of a commercially available Mg-30 wt.%Zr master alloy,and the subsequent grain refinement ability was studied by trials on a typical Mg-3Nd-0.2Zn-0.6Zr(wt.%,NZ30K)alloy.It is found that plenty of large Zr particles in the as-received Mg-30%Zr master alloy are broken by FSP.Grain refinement tests reveal that the refining efficiency of Mg-30%Zr alloy is significantly improved by FSP,which is attributed to the better distribution of Zr particles.The refinement effect by adding 0.6%FSP-ed Mg-30%Zr is approximately equivalent to that by adding 1.0%as-received Mg-30%Zr.Due to the easy and convenient operation of FSP,this study provides a new method to develop a more efficient Mg-Zr refiner.

Development and characterization studies on magnesium alloy(RZ 5)surface metal matrix composites through friction stir processing

Surface metal matrix composite is produced on the as cast Magnesium Rare Earth alloy-RZ 5 by single pass friction stir processing using various micro/nano sized reinforcement particles namely Boron Carbide(B_(4)C),Multi Walled Carbon Nano Tubes(MWCNTs),and a mixture of ZrO_(2)+Al_(2)O_(3)particles.Fine grained metal matrix composites having the grain size ranging 0.8μm to 1.87μm are achieved.Grain boundary pinning by the reinforcement particles has resulted in the transformation of coarse grained(∼81μm)base material into fine grained(<1μm)metal matrix composite.Finer grain structure and the presence of reinforcements at the stir zone have resulted in increased and improved mechanical properties of the developed composites.Microhardness ranging between 125 HV and 403 HV is achieved.Uni-axial Tensile Testing of the developed composites exhibited improvement in tensile strength.Metal matrix composites developed using various reinforcements exhibited an increase in strength ranges between 250 MPa and 320 MPa.

Influence of friction stir processing conditions on corrosion behavior of AZ31B magnesium alloy

The present study aims to investigate the effect of friction stir processing(FSP)conditions on the corrosion characteristic of AZ31B magnesium alloy.Specimens made of AZ31B alloy were friction stir processed under various processing conditions,and their microstructure and corrosion behavior were studied.The corrosion behavior was studied by potentiodynamic polarization,electrochemical impedance spectroscopy(EIS),and immersion test in 3.5%sodium chloride(NaCl)solution.The results showed a substantial improvement in the corrosion resistance of the friction stir processed AZ31B alloy.The improvement is likely a result of more stable corrosion products and microstructure refinement formed after friction sir processing.