Application of novel constrained friction processing method to produce fine grained biomedical Mg-Zn-Ca alloy

In order to obtain Mg alloys with fine microstructures and high mechanical performances,a novel friction-based processing method,name as“constrained friction processing(CFP)”,was investigated.Via CFP,defect-free Mg-Zn-Ca rods with greatly refined grains and high mechanical properties were produced.Compared to the previous as-cast microstructure,the grain size was reduced from more than 1 mm to around 4μm within 3 s by a single process cycle.The compressive yield strength was increased by 350%while the ultimate compressive strength by 53%.According to the established material flow behaviors by“tracer material”,the plastic material was transported by shear deformation.From the base material to the rod,the material experienced three stages,i.e.deformation by the tool,upward flow with additional tilt,followed by upward transportation.The microstructural evolution was revealed by“stop-action”technique.The microstructural development at regions adjacent to the rod is mainly controlled by twinning,dynamic recrystallization(DRX)as well as particle stimulated nucleation,while that within the rod is related to DRX combined with grain growth.

Effect of thermo-mechanical conditions during constrained friction processing on the particle refinement of AM50 Mg-alloy phases

Constrained Friction Processing(CFP)is a novel solid-state processing technique suitable for lightweight materials,such Mg-and Al-alloys.The technique enables grain size refinement to fine or even ultrafine scale.In this study,the effect of CFP on the microstructural refinement of AM50 rods is investigated in terms of particle size and morphology of the eutectic and secondary phases originally present in the base material,in particular the eutecticβ-Mg_(17)Al_(12)and Al-Mn phases.For that purpose,as-cast and solution heat-treated base material and processed samples were analyzed.The Al_(8)Mn_(5) intermetallic phase was identified as the main secondary phase present in all samples before and after the processing.A notorious refinement of these particles was observed,starting from particles with an average equivalent length of a few micrometers to around 560 nm after the processing.The refinement of the secondary phase refinement is attributed to a mechanism analogous to the attrition comminution,where the combination of temperature increase and shearing of the material enables the continuous breaking of the brittle intermetallic particles into smaller pieces.As for the eutectic phase,the results indicate the presence of the partially divorcedβ-Mg_(17)Al_(12)particles exclusively in the as-cast base material,indicating that no further phase transformations regarding the eutectic phase,such as dynamic precipitation,occurred after the CFP.In the case of the processed as-cast material analyzed after the CFP,the thermal energy generated during the processing led to temperature values above the solvus limit of the eutectic phase,which associated with the mechanical breakage of the particles,enabled the complete dissolution of this phase.Therefore,CFP was successfully demonstrated to promote an extensive microstructure refinement in multiple aspects,in terms of grain sizes of theα-Mg phase and presence and morphology of the Al-Mn and eutecticβ-Mg_(17)Al_(12).

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.

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.

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.

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.

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.

Surface metal-matrix composites based on AZ91 magnesium alloy via friction stir processing:A review

This monograph presents an overview of friction stir processing(FSP)of surface metal-matrix composites(MMCs)using the AZ91 magnesium alloy.The reported results in relation to various reinforcing particles,including silicon carbide(SiC),alumina(Al_(2)O_(3)),quartz(SiO_(2)),boron carbide(B_(4)C),titanium carbide(TiC),carbon fiber,hydroxyapatite(HA),in-situ formed phases,and hybrid reinforcements are summarized.AZ91 composite fabricating methods based on FSP are explained,including groove filling(grooving),drilled hole filling,sandwich method,stir casting followed by FSP,and formation of in-situ particles.The effects of introducing second-phase particles and FSP process parameters(e.g.,tool rotation rate,traverse speed,and the number of passes)on the microstructural modification,grain refinement,homogeneity in the distribution of particles,inhibition of grain growth,mechanical properties,strength–ductility trade-off,wear/tribological behavior,and corrosion resistance are discussed.Finally,useful suggestions for future work are proposed,including focusing on the superplasticity and superplastic forming,metal additive manufacturing processes based on friction stir engineering(such as additive friction stir deposition),direct FSP,stationary shoulder FSP,correlation of the dynamic recrystallization(DRX)grain size with the Zener–Hollomon parameter similar to hot deformation studies,process parameters(such as the particle volume fraction and external cooling),and common reinforcing phases such as zirconia(ZrO_(2))and carbon nanotubes(CNTs).

Simultaneous enhancement of mechanical properties and corrosion resistance of as-cast Mg-5Zn via microstructural modification by friction stir processing

Magnesium alloys are ideal lightweight materials;however,their applications are extremely limited due to their low strength,poor ductility,and weak corrosion resistance.In the present study,a friction stir processing(FSP)treatment was employed to optimize the mechanical properties and corrosion resistance of an as-cast Mg-5Zn alloy.The average grain size of the Mg-5Zn alloy was refined from 133.8μm to1.3μm as a result of FSP.Along different directions,FSP exhibited the enhancement effects on different mechanical properties.Furthermore,according to the potentiodynamic polarization results,the corrosion current density at the free-corrosion potential of the FSPed sample,was 4.1×10^(-6)A/cm^(2)in 3.5 wt.%Na Cl aqueous solution,which was significantly lower than that of the as-cast sample.Electrochemical impedance spectroscopy revealed that the polarization impedance,Rp,of the FSPed sample was 1534Ω/cm^(2)in 3.5 wt.%NaCl aqueous solution,which was 71.4%greater than that of the as-cast sample.The corrosion morphology of the FSPed sample in 3.5 wt.%NaCl aqueous solution exhibited largely uniform corrosion,rather than severe localized corrosion characteristics,which further reduced the corrosion depth on the basis of reducing the corrosion current density.The results presented herein indicate that FSP is a viable technique for simultaneously improving the mechanical properties and corrosion resistance of the as-cast Mg-5Zn alloy.

Influence of tool rotational speed on mechanical and corrosion behaviour of friction stir processed AZ31/Al_(2)O_(3)nanocomposite

Nano-sized reinforcements improved the mechanical characteristics efficiently by promoting more implicit particle hardening mechanisms compared to micron-sized reinforcements.Nano-sized particles lessen the critical particle solidification velocity for swamp and thus offers better dispersal.In the present investigation,the friction stir processing(FSP)is utilized to produce AZ31/Al_(2)O_(3)nanocomposites at various tool rotation speeds(i.e.,900,1200,and 1500 rpm)with an optimized 1.5%volume alumina(Al_(2)O_(3))reinforcement ratio.The mechanical and corrosion behavior of AZ31/Al_(2)O_(3)-developed nanocomposites was investigated and compared with that of the AZ31 base alloy.The AZ31 alloy experienced a comprehensive dynamic recrystallization during FSP,causing substantial grain refinement.Grain-size strengthening is the primary factor contributed to the enhancement in the strength of the fabricated nanocomposite.Tensile strength and yield strength values were lower than those for the base metal matrix,although an upward trend in both values has been observed with an increase in tool rotation speed.An 19.72%increase in hardness along with superior corrosion resistance was achieved compared to the base alloy at a tool rotational speed of 1500 rpm.The corrosion currents(Jcorr)of all samples dropped with increase in the rotational speed,in contrast to the corrosion potentials(Ecorr),which increased.The values of Jcorr of AZ31/Al_(2)O_(3)were 42.3%,56.8%,and 65.5%lower than those of AZ31 alloy at the chosen rotating speeds of 900,1200,and 1500 rpm,respectively.The corrosion behavior of friction stir processed nanocomposites have been addressed in this manuscript which has not been given sufficient attention in the existing literature.Further,this work offers an effective choice for the quality assurance of the FSP process of AZ31/Al_(2)O_(3)nanocomposites.The obtained results are relevant to the development of lightweight automobile and aerospace structures and components.

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.

Microstructure and texture evolution in titanium subjected to friction roll surface processing and subsequent annealing

Commercial purity and high purity titanium sheets were initially strained by a new technique, named as friction roll surface processing （FRSP）. Severe strain was imposed into the surface layer and strain gradient was formed through the thickness of the sheet. The microstructure and texture in as-strained state were investigated by optical microscopy and X-ray diffraction technique On the surface of the sheets, ultra-fine grains were found to have a sharp texture with a preferred orientation strongly related to the FRSP direction. The evolution of microstructure and crystallographic texture of FRSPed samples during recrystallization were also studied by electron back-scattered diffraction （EBSD） technique after being annealed at selected temperatures and time. The results indicated that the preferred orientations resulting from FRSP and annealing in the surface layer were formed during rolling and its recrystallization textures were reduced by FRSP. In addition, the texture evolved stably without change in main components during the annealing.

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.

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.

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.

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.

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.

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.