In this work,the microstructural evolution and mechanical properties of a pre-deformed WE43 magnesium alloy when aged at 250 and 300℃ were further investigated.It is found that the abundant deformation twins introduc...In this work,the microstructural evolution and mechanical properties of a pre-deformed WE43 magnesium alloy when aged at 250 and 300℃ were further investigated.It is found that the abundant deformation twins introduced by pre-deformation were maintained within the alloy during the aging treatment.Second particles formed at the twin boundaries and coarsened with aging time,especially at 300℃.When peak-aged at 250℃,the fine metastable β'''and β' precipitates formed in the un-deformed alloy have been transformed into relatively large β1 and β precipitates by the pre-deformation.While peak-aged at 300℃,the pre-deformation obviously refined the β precipitates.Mechanical properties indicate that pre-deformation can increase the yield strength by 19MPa and 54MPa for the peak-aged alloy at 250℃ and 300℃,respectively,and will not obviously deteriorate the tensile elongations.展开更多
In this study, cyclic expansion extrusion（CEE）, as a relatively new severe plastic deformation（SPD） process, is applied to a rare earth（RE） containing Mg alloy WE43. The effects of the processing temperature and...In this study, cyclic expansion extrusion（CEE）, as a relatively new severe plastic deformation（SPD） process, is applied to a rare earth（RE） containing Mg alloy WE43. The effects of the processing temperature and the number of passes are also investigated. The results showed that dynamic recrystallization（DRX） occurred after CEE processing at 400°C, and a bimodal structure with ultrafine DRXed grains surrounded the unrecrystallized grains. However, the DRX at 330°C was retarded because of the existence of RE elements. The tensile tests showed that a simultaneous increase in the strength and the ductility of WE43 is obtained after CEE processing at 400°C via two passes. Furthermore, the highest ultimate tensile strength of 440 MPa was achieved after the second pass of CEE at 330°C, and the highest ductility of 21% was attained after the second pass of CEE at 400°C. The microhardness measurements showed that the hardness increased from HV 80 to HV 114 and HV 98 after two passes of CEE processing at 330 and 400°C, respectively. In conclusion, increasing the processing passes could increase the mechanical properties and the volume fraction of the recrystallized grains. Moreover, increasing the temperature reduced the strength and the microhardness even if the elongation increased.展开更多
High temperature tensile-creep behavior of Mg-4Y-2.3Nd-IGd-O.6Zr （wt%, WE43（T6）） alloy at 523- 573 K was investigated. The creep stress exponent is equal to 4.6, suggesting the underlying dislocation creep mechani...High temperature tensile-creep behavior of Mg-4Y-2.3Nd-IGd-O.6Zr （wt%, WE43（T6）） alloy at 523- 573 K was investigated. The creep stress exponent is equal to 4.6, suggesting the underlying dislocation creep mechanism. The activation energy is （199 _＋ 23） kJ/mol, which is higher than that for self- diffusion in Mg and is believed to be associated with precipitates coarsening or cross slip. The creep mechanism is further suggested to be dislocation climb at 523 K, while a cross slip at 573 K is possible. The metastable 13＇ and ~]1 phases in the WE43（T6） alloy were relatively thermal stable at 523 K and could be effective to hinder the dislocation climb, which contributed to its excellent creep resistance. However, at 573 K it readily transforms into equilibrium/3e phase and coarsens within two hours, thereby causing a decrease of creep resistance. In addition, precipitate free zones approximately normal to applied stress direction （directional PFZs） developed during the creep deformation, especially at 573 K. Those zones became preferential sites to nucleate, extend and connect microcracks and cavities, which lead to the intergranular creep fracture. Improving the thermal stability of precipitates or introducing thermally stable fine plate-shaped precipitates on the basal planes of Mg matrix could enhance the high temperature creep resistance.展开更多
Laser powder bed fusion(L-PBF)of Mg alloys has provided tremendous opportunities for customized production of aeronautical and medical parts.Layer thickness(LT)is of great significance to the L-PBF process but has not...Laser powder bed fusion(L-PBF)of Mg alloys has provided tremendous opportunities for customized production of aeronautical and medical parts.Layer thickness(LT)is of great significance to the L-PBF process but has not been studied for Mg alloys.In this study,WE43 Mg alloy bulk cubes,porous scaffolds,and thin walls with layer thicknesses of 10,20,30,and 40μm were fabricated.The required laser energy input increased with increasing layer thickness and was different for the bulk cubes and porous scaffolds.Porosity tended to occur at the connection joints in porous scaffolds for LT40 and could be eliminated by reducing the laser energy input.For thin wall parts,a large overhang angle or a small wall thickness resulted in porosity when a large layer thicknesses was used,and the porosity disappeared by reducing the layer thickness or laser energy input.A deeper keyhole penetration was found in all occasions with porosity,explaining the influence of layer thickness,geometrical structure,and laser energy input on the porosity.All the samples achieved a high fusion quality with a relative density of over 99.5%using the optimized laser energy input.The increased layer thickness resulted to more precipitation phases,finer grain sizes and decreased grain texture.With the similar high fusion quality,the tensile strength and elongation of bulk samples were significantly improved from 257 MPa and 1.41%with the 10μm layer to 287 MPa and 15.12%with the 40μm layer,in accordance with the microstructural change.The effect of layer thickness on the compressive properties of porous scaffolds was limited.However,the corrosion rate of bulk samples accelerated with increasing the layer thickness,mainly attributed to the increased number of precipitation phases.展开更多
Laser powder bed fusion(L-PBF)of magnesium(Mg)alloy porous scaffolds is expected to solve the dual challenges from customized structures and biodegradable functions required for repairing bone defects.However,one of t...Laser powder bed fusion(L-PBF)of magnesium(Mg)alloy porous scaffolds is expected to solve the dual challenges from customized structures and biodegradable functions required for repairing bone defects.However,one of the key technical difficulties lies in the poor L-PBF process performance of Mg,contributed by the high susceptibility to oxidation,vaporization,thermal expansion,and powder attachment etc.This work investigated the influence of L-PBF energy input and scanning strategy on the formation quality of porous scaffolds by using WE43 powder,and characterized the microstructure,mechanical properties,biocompatibility,biodegradation and osteogenic effect of the as-built WE43 porous scaffolds.With the customized energy input and scanning strategy,the relative density of struts reached over 99.5%,and the geometrical error between the designed and the fabricated porosity declined to below 10%.Massive secondary phases including intermetallic precipitates and oxides were observed.The compressive strength(4.37-23.49 MPa)and elastic modulus(154.40-873.02 MPa)were comparable to those of cancellous bone.Good biocompatibility was observed by in vitro cell viability and in vivo implantation.The biodegradation of as-built porous scaffolds promoted the osteogenic effect,but the structural integrity devastated after 12 h by the immersion tests in Hank’s solution and after 4 weeks by the implantation in rabbits’femur,indicating an excessively rapid degradation rate.展开更多
Magnesium(Mg)alloys are considered to be a new generation of revolutionary medical metals.Laser-beam powder bed fusion(PBF-LB)is suitable for fabricating metal implants withpersonalized and complicated structures.Howe...Magnesium(Mg)alloys are considered to be a new generation of revolutionary medical metals.Laser-beam powder bed fusion(PBF-LB)is suitable for fabricating metal implants withpersonalized and complicated structures.However,the as-built part usually exhibits undesirable microstructure and unsatisfactory performance.In this work,WE43 parts were firstly fabricated by PBF-LB and then subjected to heat treatment.Although a high densification rate of 99.91%was achieved using suitable processes,the as-built parts exhibited anisotropic and layeredmicrostructure with heterogeneously precipitated Nd-rich intermetallic.After heat treatment,fine and nano-scaled Mg24Y5particles were precipitated.Meanwhile,theα-Mg grainsunderwent recrystallization and turned coarsened slightly,which effectively weakened thetexture intensity and reduced the anisotropy.As a consequence,the yield strength and ultimate tensile strength were significantly improved to(250.2±3.5)MPa and(312±3.7)MPa,respectively,while the elongation was still maintained at a high level of 15.2%.Furthermore,the homogenized microstructure reduced the tendency of localized corrosion and favoredthe development of uniform passivation film.Thus,the degradation rate of WE43 parts was decreased by an order of magnitude.Besides,in-vitro cell experiments proved their favorable biocompatibility.展开更多
Laser powder bed fusion(L-PBF)has been employed to additively manufacture WE43 magnesium(Mg)alloy biodegradable implants,but WE43 L-PBF samples exhibit excessively rapid corrosion.In this work,dense WE43 L-PBF samples...Laser powder bed fusion(L-PBF)has been employed to additively manufacture WE43 magnesium(Mg)alloy biodegradable implants,but WE43 L-PBF samples exhibit excessively rapid corrosion.In this work,dense WE43 L-PBF samples were built with the relativity density reaching 99.9%.High temperature oxidation was performed on the L-PBF samples in circulating air via various heating temperatures and holding durations.The oxidation and diffusion at the elevated temperature generated a gradient structure composed of an oxide layer at the surface,a transition layer in the middle and the matrix.The oxide layer consisted of rare earth(RE)oxides,and became dense and thick with increasing the holding duration.The matrix was composed ofα-Mg,RE oxides and Mg_(24)RE_(5) precipitates.The precipitates almost disappeared in the transition layer.Enhanced passivation effect was observed in the samples treated by a suitable high temperature oxidation.The original L-PBF samples lost 40%weight after 3-day immersion in Hank’s solution,and broke into fragments after 7-day immersion.The casted and solution treated samples lost roughly half of the weight after 28-day immersion.The high temperature oxidation samples,which were heated at 525℃ for 8 h,kept the structural integrity,and lost only 6.88%weight after 28-day immersion.The substantially improved corrosion resistance was contributed to the gradient structure at the surface.On one hand,the outmost dense layer of RE oxides isolated the corrosive medium;on the other hand,the transition layer considerably inhibited the corrosion owing to the lack of precipitates.Overall,high temperature oxidation provides an efficient,economic and safe approach to inhibit the corrosion of WE43 L-PBF samples,and has promising prospects for future clinical applications.展开更多
The low-cycle fatigue behavior of solutionized(T4)and aged(T6)WE43 magnesium alloys was studied at room temperature.The total strain amplitudes(△ε_(t)/2)were 0.4%,0.5%,0.6%,0.7%and 1.0%.Detailed microstructure evolu...The low-cycle fatigue behavior of solutionized(T4)and aged(T6)WE43 magnesium alloys was studied at room temperature.The total strain amplitudes(△ε_(t)/2)were 0.4%,0.5%,0.6%,0.7%and 1.0%.Detailed microstructure evolution was characterized by scanning electron microscope(SEM),electron backscattered diffraction(EBSD)and transmission electron microscopy(TEM).The results showed that plastic strain amplitude decreased with the increasing cycle number in T4 alloy,which is due to the dense persistent slip bands(PSBs)and dynamic precipitates hinderingdislocation slip.In contrast,the plastic strain amplitude increases gradually in T6 alloy,which is attributed to the enhanced activation of pyramidal slip.The low-cycle fatigue life of T6 alloy with larger fatigue ductility coefficient is longer than that of T4 alloy.The Coffin-Manson model can accurately predict the fatigue life of T4 and T6 alloys compared to Jahed-Varvani(JV)energy model.For T4 alloy,the fatigue damage mechanism was dominated by basal slip.For T6 alloy,the enhanced pyramidal slip plays an important role to accommodate plastic deformation.展开更多
The effect of compression on the microstructures and flow behavior of WE43 magnesium alloy was investigated in this article. The relationship between flow stress and strain rate was discussed. According to the empiric...The effect of compression on the microstructures and flow behavior of WE43 magnesium alloy was investigated in this article. The relationship between flow stress and strain rate was discussed. According to the empirical formula ε = Aδ^n exp （-Q/R T）, the value of heat activation of WE43 magnesium alloys is 297,15 kJ/mol. A mechanism of deformation softening of WE43 alloy in testing hot deformation was identified to be dynamic recrystallization.展开更多
Permanent implants are going to be replaced by the implementation of biodegradable magnesium-based implants in fixation of internal bone fractures because of many concerns associated with conventional implants.However...Permanent implants are going to be replaced by the implementation of biodegradable magnesium-based implants in fixation of internal bone fractures because of many concerns associated with conventional implants.However,biodegradable magnesium-based biomaterials exhibit higher biodegradation rate and low mechanical properties which are the main challenges.This work aims to almost overcome both disadvantageous by grain refining of a WE43 magnesium alloy containing 93.04 wt% Mg,4.12 wt% Y,2.15 wt% Nd,0.43 wt% Zr,and 0.26 wt%La.In this study,the consequences of combined severe plastic deformation(SPD) on the mechanical properties,microstructure,and in vivo degradation behavior of WE43 magnesium alloy were investigated.To do so,WE43 magnesium alloy was chosen and processed through multipass equal channel angular pressing(ECAP) at 330℃ for up to four passes followed by an extrusion process.The results showed that higher strength and hardness with minimum ductility less was obtained in the sample processed via two-pass ECAP followed by extrusion.In vivo biodegradation experiments showed higher degradation rate for the unprocessed coarse-grained(CG) WE43 sample.The two-pass ECAP and extruded sample with ultrafine-grained(UFG) structure exhibited the lowest in vivo biodegradation rate besides appropriate mechanical properties.It may be concluded that the WE43 magnesium alloy processed via two-pass ECAP and extrusion could be a very promising candidate for biodegradable implants from both mechanical and biocorrosion viewpoints.展开更多
The direct industrial importance of the corrosion resistance in WE43 is best emphasized by its extensive use in the automotive, aerospace and electronic industries where weight reduction is a necessary requirement. In...The direct industrial importance of the corrosion resistance in WE43 is best emphasized by its extensive use in the automotive, aerospace and electronic industries where weight reduction is a necessary requirement. In this work, the corrosion especially the filiform corrosion in a 3.5 wt.% Na Cl solution and their dependence on the Zr distribution for WE43 were studied by weight loss tests, hydrogen evolution tests, electrochemical measurements and microscopic analyses. The Zr distribution significantly influenced the initiation and propagation of the filiform corrosion, and accordingly significantly influenced the corrosion rate. WE43 with a cluster Zr distribution displayed filiform corrosion throughout the entire surface with an irregular network distribution of filaments. WE43 with a uniform line Zr distribution exhibited only a few examples of linear filiform corrosion. WE43 with a dispersive Zr distribution exhibited no filiform corrosion. The stability of the corrosion film was responsible for the filiform corrosion. Anodic polarisation promoted the initiation and progression of the filiform corrosion,while cathodic polarisation had an inhibiting effect on the filiform corrosion. The serrated interface of the filiform corrosion increased the contact area between the substrate and the corrosive medium, and hence increased the corrosion rate.展开更多
The effects of pore size in additively manufactured biodegradable porous magnesium on the mechanical properties and biodegradation of the scaffolds as well as new bone formation have rarely been reported. In this work...The effects of pore size in additively manufactured biodegradable porous magnesium on the mechanical properties and biodegradation of the scaffolds as well as new bone formation have rarely been reported. In this work, we found that high temperature oxidation improves the corrosion resistance of magnesium scaffold. And the effects of pore size on the mechanical characteristics and biodegradation of scaffolds, as well as new bone formation, were investigated using magnesium scaffolds with three different pore sizes, namely, 500, 800, and 1400 μm (P500, P800, and P1400). We discovered that the mechanical characteristics of the P500 group were much better than those of the other two groups. In vitro and in vivo investigations showed that WE43 magnesium alloy scaffolds supported the survival of mesenchymal stem cells and did not cause any local toxicity. Due to their larger specific surface area, the scaffolds in the P500 group released more magnesium ions within reasonable range and improved the osteogenic differentiation of bone mesenchymal stem cells compared with the other two scaffolds. In a rabbit femoral condyle defect model, the P500 group demonstrated unique performance in promoting new bone formation, indicating its great potential for use in bone defect regeneration therapy.展开更多
Torsional properties are important performance parameters for bone screw applications,but they are seldom studied,especially for newly developed biodegradable Mg alloys.In this study,WE43 Mg alloy with different micro...Torsional properties are important performance parameters for bone screw applications,but they are seldom studied,especially for newly developed biodegradable Mg alloys.In this study,WE43 Mg alloy with different microstructures was achieved by equal channel angular pressing(ECAP)and heat treatment,and their torsional properties were studied.In addition,tensile properties were also tested as a comparison.The results indicated that grain refinement led to higher torsional strength and ductility,while the second phases improved the torsional strength but reduced the ductility.The texture was strengthened after ECAP,as a result the tensile strength increased,but the torsional strength did not increase and even decreased,especially for 2-pass ECAP sample with a typical basal fiber texture.The basal plane orientation deviation from the extrusion direction after 4-pass ECAP resulted in higher torsional strength and lower torsional ductility,but lower tensile strength and higher tensile ductility were obtained.This implied that a strong fiber texture would reduce the torsional strength but improve the torsional ductility,which was different from its effect on tensile properties.展开更多
It is well known that laser-based powder-bed fusion(L-PBF) additive manufacturing of magnesium(Mg) and its alloys is associated with high Mg loss due to vaporization(MgLoss) and high incidence of many types of defects...It is well known that laser-based powder-bed fusion(L-PBF) additive manufacturing of magnesium(Mg) and its alloys is associated with high Mg loss due to vaporization(MgLoss) and high incidence of many types of defects in the manufactured parts/samples. Despite this,MgLoss, densification, and defect characteristics have not been holistically considered in the determination of the optimal values of L-PBF processing parameters for Mg and its alloys. This study presents a combined modeling and experimental approach applied for a widely used Mg alloy(WE43) to address this shortcoming in the literature. First, an experimentally calibrated model is proposed to determine MgLoss as a function of the L-PBF processing parameters. The model couples the temperature profile using a double ellipsoidal heat source with a Langmuir vaporization model and is calibrated using the width of the single-track L-PBF process and the measured Mglossusing inductively coupled plasma mass spectrometry(ICP-MS). Second, the densification of the samples is determined using a modification of the Archimedes method that considers the amount of MgLossin the calculation of the relative density. Third, a comprehensive and quantitative study is conducted on the relationships between the characteristics of porosity defects and the L-PBF processing parameters. Finally, the optimized L-PBF processing parameters are determined by considering the MgLoss, densification, and the characteristics of defects. The present study yields 0.23 wt.% MgLosscompared to 2 wt.% MgLossthat was reported in the previous studies. Furthermore, more than 99.5% densification is achieved while only ~2% and ~0.5% of the total defects are characterized as keyhole and lack of fusion defects, respectively.展开更多
In order to improve the ductility of commercial WE43 alloy and reduce its cost,a Mg-3Y-2Gd-1Nd-0.4Zr alloy with a low amount of rare earths was developed and prepared by sand casting with a differential pressure casti...In order to improve the ductility of commercial WE43 alloy and reduce its cost,a Mg-3Y-2Gd-1Nd-0.4Zr alloy with a low amount of rare earths was developed and prepared by sand casting with a differential pressure casting system.Its microstructure,mechanical properties and fracture behaviors in the as-cast,solution-treated and as-aged states were evaluated.It is found that the aged alloy exhibited excellent comprehensive mechanical properties owing to the fine dense plate-shapedβ'precipitates formed on prismatic habits during aging at 200℃for 192 hrs after solution-treated at 500℃for 24 hrs.Its ultimate tensile strength,yield strength,and elongation at ambient temperature reach to 319±10 MPa,202±2 MPa and 8.7±0.3%as well as 230±4 MPa,155±1 MPa and 16.0±0.5%at 250℃.The fracture mode of as-aged alloy was transferred from cleavage at room temperature to quasi-cleavage and ductile fracture at the test temperature 300℃.The properties of large-scale components fabricated using the developed Mg-3Y-2Gd-1Nd-0.4Zr alloy are better than those of commercial WE43 alloy,suggesting that the new developed alloy is a good candidate to fabricate the large complex thin-walled components.展开更多
基金We thank the GDAS’Project of Science and Technology Development(Grants No.2018GDASCX0966,2019GDASYL-0203002,2018GDASCX-0117)Guangzhou Science and Technology Planning Project(Grant No.201904010309)for the financial support.
文摘In this work,the microstructural evolution and mechanical properties of a pre-deformed WE43 magnesium alloy when aged at 250 and 300℃ were further investigated.It is found that the abundant deformation twins introduced by pre-deformation were maintained within the alloy during the aging treatment.Second particles formed at the twin boundaries and coarsened with aging time,especially at 300℃.When peak-aged at 250℃,the fine metastable β'''and β' precipitates formed in the un-deformed alloy have been transformed into relatively large β1 and β precipitates by the pre-deformation.While peak-aged at 300℃,the pre-deformation obviously refined the β precipitates.Mechanical properties indicate that pre-deformation can increase the yield strength by 19MPa and 54MPa for the peak-aged alloy at 250℃ and 300℃,respectively,and will not obviously deteriorate the tensile elongations.
文摘In this study, cyclic expansion extrusion（CEE）, as a relatively new severe plastic deformation（SPD） process, is applied to a rare earth（RE） containing Mg alloy WE43. The effects of the processing temperature and the number of passes are also investigated. The results showed that dynamic recrystallization（DRX） occurred after CEE processing at 400°C, and a bimodal structure with ultrafine DRXed grains surrounded the unrecrystallized grains. However, the DRX at 330°C was retarded because of the existence of RE elements. The tensile tests showed that a simultaneous increase in the strength and the ductility of WE43 is obtained after CEE processing at 400°C via two passes. Furthermore, the highest ultimate tensile strength of 440 MPa was achieved after the second pass of CEE at 330°C, and the highest ductility of 21% was attained after the second pass of CEE at 400°C. The microhardness measurements showed that the hardness increased from HV 80 to HV 114 and HV 98 after two passes of CEE processing at 330 and 400°C, respectively. In conclusion, increasing the processing passes could increase the mechanical properties and the volume fraction of the recrystallized grains. Moreover, increasing the temperature reduced the strength and the microhardness even if the elongation increased.
基金funded by the National Basic Research Program of China(No.2013CB632202 and No.51531002)the National Natural Science Foundation of China(No.51301173)
文摘High temperature tensile-creep behavior of Mg-4Y-2.3Nd-IGd-O.6Zr （wt%, WE43（T6）） alloy at 523- 573 K was investigated. The creep stress exponent is equal to 4.6, suggesting the underlying dislocation creep mechanism. The activation energy is （199 _＋ 23） kJ/mol, which is higher than that for self- diffusion in Mg and is believed to be associated with precipitates coarsening or cross slip. The creep mechanism is further suggested to be dislocation climb at 523 K, while a cross slip at 573 K is possible. The metastable 13＇ and ~]1 phases in the WE43（T6） alloy were relatively thermal stable at 523 K and could be effective to hinder the dislocation climb, which contributed to its excellent creep resistance. However, at 573 K it readily transforms into equilibrium/3e phase and coarsens within two hours, thereby causing a decrease of creep resistance. In addition, precipitate free zones approximately normal to applied stress direction （directional PFZs） developed during the creep deformation, especially at 573 K. Those zones became preferential sites to nucleate, extend and connect microcracks and cavities, which lead to the intergranular creep fracture. Improving the thermal stability of precipitates or introducing thermally stable fine plate-shaped precipitates on the basal planes of Mg matrix could enhance the high temperature creep resistance.
基金funded by the National Key Research and Development Program of China(2018YFE0104200)National Natural Science Foundation of China(51875310,52175274,82172065)Tsinghua Precision Medicine Foundation.
文摘Laser powder bed fusion(L-PBF)of Mg alloys has provided tremendous opportunities for customized production of aeronautical and medical parts.Layer thickness(LT)is of great significance to the L-PBF process but has not been studied for Mg alloys.In this study,WE43 Mg alloy bulk cubes,porous scaffolds,and thin walls with layer thicknesses of 10,20,30,and 40μm were fabricated.The required laser energy input increased with increasing layer thickness and was different for the bulk cubes and porous scaffolds.Porosity tended to occur at the connection joints in porous scaffolds for LT40 and could be eliminated by reducing the laser energy input.For thin wall parts,a large overhang angle or a small wall thickness resulted in porosity when a large layer thicknesses was used,and the porosity disappeared by reducing the layer thickness or laser energy input.A deeper keyhole penetration was found in all occasions with porosity,explaining the influence of layer thickness,geometrical structure,and laser energy input on the porosity.All the samples achieved a high fusion quality with a relative density of over 99.5%using the optimized laser energy input.The increased layer thickness resulted to more precipitation phases,finer grain sizes and decreased grain texture.With the similar high fusion quality,the tensile strength and elongation of bulk samples were significantly improved from 257 MPa and 1.41%with the 10μm layer to 287 MPa and 15.12%with the 40μm layer,in accordance with the microstructural change.The effect of layer thickness on the compressive properties of porous scaffolds was limited.However,the corrosion rate of bulk samples accelerated with increasing the layer thickness,mainly attributed to the increased number of precipitation phases.
基金funded by the National Key Research and Development Program of China(2018YFE0104200)National Natural Science Foundation of China(51875310,52175274,82172065)and AO Foundation(AOTAP21-47).
文摘Laser powder bed fusion(L-PBF)of magnesium(Mg)alloy porous scaffolds is expected to solve the dual challenges from customized structures and biodegradable functions required for repairing bone defects.However,one of the key technical difficulties lies in the poor L-PBF process performance of Mg,contributed by the high susceptibility to oxidation,vaporization,thermal expansion,and powder attachment etc.This work investigated the influence of L-PBF energy input and scanning strategy on the formation quality of porous scaffolds by using WE43 powder,and characterized the microstructure,mechanical properties,biocompatibility,biodegradation and osteogenic effect of the as-built WE43 porous scaffolds.With the customized energy input and scanning strategy,the relative density of struts reached over 99.5%,and the geometrical error between the designed and the fabricated porosity declined to below 10%.Massive secondary phases including intermetallic precipitates and oxides were observed.The compressive strength(4.37-23.49 MPa)and elastic modulus(154.40-873.02 MPa)were comparable to those of cancellous bone.Good biocompatibility was observed by in vitro cell viability and in vivo implantation.The biodegradation of as-built porous scaffolds promoted the osteogenic effect,but the structural integrity devastated after 12 h by the immersion tests in Hank’s solution and after 4 weeks by the implantation in rabbits’femur,indicating an excessively rapid degradation rate.
基金supported by the following funds:National Natural Science Foundation of China(51935014,52165043)Jiangxi Provincial Cultivation Program for Academic and Technical Leaders of Major Subjects(20225BCJ23008)+1 种基金Jiangxi Provincial Natural Science Foundation(20224ACB204013,20224ACB214008)Scientific Research Project of Anhui Universities(KJ2021A1106)。
文摘Magnesium(Mg)alloys are considered to be a new generation of revolutionary medical metals.Laser-beam powder bed fusion(PBF-LB)is suitable for fabricating metal implants withpersonalized and complicated structures.However,the as-built part usually exhibits undesirable microstructure and unsatisfactory performance.In this work,WE43 parts were firstly fabricated by PBF-LB and then subjected to heat treatment.Although a high densification rate of 99.91%was achieved using suitable processes,the as-built parts exhibited anisotropic and layeredmicrostructure with heterogeneously precipitated Nd-rich intermetallic.After heat treatment,fine and nano-scaled Mg24Y5particles were precipitated.Meanwhile,theα-Mg grainsunderwent recrystallization and turned coarsened slightly,which effectively weakened thetexture intensity and reduced the anisotropy.As a consequence,the yield strength and ultimate tensile strength were significantly improved to(250.2±3.5)MPa and(312±3.7)MPa,respectively,while the elongation was still maintained at a high level of 15.2%.Furthermore,the homogenized microstructure reduced the tendency of localized corrosion and favoredthe development of uniform passivation film.Thus,the degradation rate of WE43 parts was decreased by an order of magnitude.Besides,in-vitro cell experiments proved their favorable biocompatibility.
基金funded by the National Key Research and Development Program of China (2018YFE0104200)National Natural Science Foundation of China (51875310, 52175274, 82172065)Tsinghua Precision Medicine Foundation
文摘Laser powder bed fusion(L-PBF)has been employed to additively manufacture WE43 magnesium(Mg)alloy biodegradable implants,but WE43 L-PBF samples exhibit excessively rapid corrosion.In this work,dense WE43 L-PBF samples were built with the relativity density reaching 99.9%.High temperature oxidation was performed on the L-PBF samples in circulating air via various heating temperatures and holding durations.The oxidation and diffusion at the elevated temperature generated a gradient structure composed of an oxide layer at the surface,a transition layer in the middle and the matrix.The oxide layer consisted of rare earth(RE)oxides,and became dense and thick with increasing the holding duration.The matrix was composed ofα-Mg,RE oxides and Mg_(24)RE_(5) precipitates.The precipitates almost disappeared in the transition layer.Enhanced passivation effect was observed in the samples treated by a suitable high temperature oxidation.The original L-PBF samples lost 40%weight after 3-day immersion in Hank’s solution,and broke into fragments after 7-day immersion.The casted and solution treated samples lost roughly half of the weight after 28-day immersion.The high temperature oxidation samples,which were heated at 525℃ for 8 h,kept the structural integrity,and lost only 6.88%weight after 28-day immersion.The substantially improved corrosion resistance was contributed to the gradient structure at the surface.On one hand,the outmost dense layer of RE oxides isolated the corrosive medium;on the other hand,the transition layer considerably inhibited the corrosion owing to the lack of precipitates.Overall,high temperature oxidation provides an efficient,economic and safe approach to inhibit the corrosion of WE43 L-PBF samples,and has promising prospects for future clinical applications.
基金financially supported by the Natural Science Foundation of Liaoning Province(No.2020-MS-004)the Natural Science Foundation of Liaoning(ZR2021ME241)+1 种基金the National Natural Science Foundation of China(Nos.51601193 and 51701218)the National Key Research and Development Program of China(No.2016YFB0301104)。
文摘The low-cycle fatigue behavior of solutionized(T4)and aged(T6)WE43 magnesium alloys was studied at room temperature.The total strain amplitudes(△ε_(t)/2)were 0.4%,0.5%,0.6%,0.7%and 1.0%.Detailed microstructure evolution was characterized by scanning electron microscope(SEM),electron backscattered diffraction(EBSD)and transmission electron microscopy(TEM).The results showed that plastic strain amplitude decreased with the increasing cycle number in T4 alloy,which is due to the dense persistent slip bands(PSBs)and dynamic precipitates hinderingdislocation slip.In contrast,the plastic strain amplitude increases gradually in T6 alloy,which is attributed to the enhanced activation of pyramidal slip.The low-cycle fatigue life of T6 alloy with larger fatigue ductility coefficient is longer than that of T4 alloy.The Coffin-Manson model can accurately predict the fatigue life of T4 and T6 alloys compared to Jahed-Varvani(JV)energy model.For T4 alloy,the fatigue damage mechanism was dominated by basal slip.For T6 alloy,the enhanced pyramidal slip plays an important role to accommodate plastic deformation.
基金the National Natu-ral Science Foundation of China (No. 30670562)the Post-graduate Science and Innovation Fund of Chongqing Uni-versity (No. 200706A1A0070227)
文摘The effect of compression on the microstructures and flow behavior of WE43 magnesium alloy was investigated in this article. The relationship between flow stress and strain rate was discussed. According to the empirical formula ε = Aδ^n exp （-Q/R T）, the value of heat activation of WE43 magnesium alloys is 297,15 kJ/mol. A mechanism of deformation softening of WE43 alloy in testing hot deformation was identified to be dynamic recrystallization.
基金financially supported by the Iran National Science Foundation(No.96000854)。
文摘Permanent implants are going to be replaced by the implementation of biodegradable magnesium-based implants in fixation of internal bone fractures because of many concerns associated with conventional implants.However,biodegradable magnesium-based biomaterials exhibit higher biodegradation rate and low mechanical properties which are the main challenges.This work aims to almost overcome both disadvantageous by grain refining of a WE43 magnesium alloy containing 93.04 wt% Mg,4.12 wt% Y,2.15 wt% Nd,0.43 wt% Zr,and 0.26 wt%La.In this study,the consequences of combined severe plastic deformation(SPD) on the mechanical properties,microstructure,and in vivo degradation behavior of WE43 magnesium alloy were investigated.To do so,WE43 magnesium alloy was chosen and processed through multipass equal channel angular pressing(ECAP) at 330℃ for up to four passes followed by an extrusion process.The results showed that higher strength and hardness with minimum ductility less was obtained in the sample processed via two-pass ECAP followed by extrusion.In vivo biodegradation experiments showed higher degradation rate for the unprocessed coarse-grained(CG) WE43 sample.The two-pass ECAP and extruded sample with ultrafine-grained(UFG) structure exhibited the lowest in vivo biodegradation rate besides appropriate mechanical properties.It may be concluded that the WE43 magnesium alloy processed via two-pass ECAP and extrusion could be a very promising candidate for biodegradable implants from both mechanical and biocorrosion viewpoints.
基金Financially supported by Chinese Natural Science Foundation (NSFC,China) (No.51874368)。
文摘The direct industrial importance of the corrosion resistance in WE43 is best emphasized by its extensive use in the automotive, aerospace and electronic industries where weight reduction is a necessary requirement. In this work, the corrosion especially the filiform corrosion in a 3.5 wt.% Na Cl solution and their dependence on the Zr distribution for WE43 were studied by weight loss tests, hydrogen evolution tests, electrochemical measurements and microscopic analyses. The Zr distribution significantly influenced the initiation and propagation of the filiform corrosion, and accordingly significantly influenced the corrosion rate. WE43 with a cluster Zr distribution displayed filiform corrosion throughout the entire surface with an irregular network distribution of filaments. WE43 with a uniform line Zr distribution exhibited only a few examples of linear filiform corrosion. WE43 with a dispersive Zr distribution exhibited no filiform corrosion. The stability of the corrosion film was responsible for the filiform corrosion. Anodic polarisation promoted the initiation and progression of the filiform corrosion,while cathodic polarisation had an inhibiting effect on the filiform corrosion. The serrated interface of the filiform corrosion increased the contact area between the substrate and the corrosive medium, and hence increased the corrosion rate.
文摘The effects of pore size in additively manufactured biodegradable porous magnesium on the mechanical properties and biodegradation of the scaffolds as well as new bone formation have rarely been reported. In this work, we found that high temperature oxidation improves the corrosion resistance of magnesium scaffold. And the effects of pore size on the mechanical characteristics and biodegradation of scaffolds, as well as new bone formation, were investigated using magnesium scaffolds with three different pore sizes, namely, 500, 800, and 1400 μm (P500, P800, and P1400). We discovered that the mechanical characteristics of the P500 group were much better than those of the other two groups. In vitro and in vivo investigations showed that WE43 magnesium alloy scaffolds supported the survival of mesenchymal stem cells and did not cause any local toxicity. Due to their larger specific surface area, the scaffolds in the P500 group released more magnesium ions within reasonable range and improved the osteogenic differentiation of bone mesenchymal stem cells compared with the other two scaffolds. In a rabbit femoral condyle defect model, the P500 group demonstrated unique performance in promoting new bone formation, indicating its great potential for use in bone defect regeneration therapy.
基金supported financially by the Key Program of China on Biomedical Materials Research and Tissue and Organ Replacement(Nos.2016YFC11018 and 2016YFC1100604)the Shenyang Key R&D and Technology Transfer Program(No.Z18-0-027)the National Natural Science Foundation of China(No.51801220)。
文摘Torsional properties are important performance parameters for bone screw applications,but they are seldom studied,especially for newly developed biodegradable Mg alloys.In this study,WE43 Mg alloy with different microstructures was achieved by equal channel angular pressing(ECAP)and heat treatment,and their torsional properties were studied.In addition,tensile properties were also tested as a comparison.The results indicated that grain refinement led to higher torsional strength and ductility,while the second phases improved the torsional strength but reduced the ductility.The texture was strengthened after ECAP,as a result the tensile strength increased,but the torsional strength did not increase and even decreased,especially for 2-pass ECAP sample with a typical basal fiber texture.The basal plane orientation deviation from the extrusion direction after 4-pass ECAP resulted in higher torsional strength and lower torsional ductility,but lower tensile strength and higher tensile ductility were obtained.This implied that a strong fiber texture would reduce the torsional strength but improve the torsional ductility,which was different from its effect on tensile properties.
文摘It is well known that laser-based powder-bed fusion(L-PBF) additive manufacturing of magnesium(Mg) and its alloys is associated with high Mg loss due to vaporization(MgLoss) and high incidence of many types of defects in the manufactured parts/samples. Despite this,MgLoss, densification, and defect characteristics have not been holistically considered in the determination of the optimal values of L-PBF processing parameters for Mg and its alloys. This study presents a combined modeling and experimental approach applied for a widely used Mg alloy(WE43) to address this shortcoming in the literature. First, an experimentally calibrated model is proposed to determine MgLoss as a function of the L-PBF processing parameters. The model couples the temperature profile using a double ellipsoidal heat source with a Langmuir vaporization model and is calibrated using the width of the single-track L-PBF process and the measured Mglossusing inductively coupled plasma mass spectrometry(ICP-MS). Second, the densification of the samples is determined using a modification of the Archimedes method that considers the amount of MgLossin the calculation of the relative density. Third, a comprehensive and quantitative study is conducted on the relationships between the characteristics of porosity defects and the L-PBF processing parameters. Finally, the optimized L-PBF processing parameters are determined by considering the MgLoss, densification, and the characteristics of defects. The present study yields 0.23 wt.% MgLosscompared to 2 wt.% MgLossthat was reported in the previous studies. Furthermore, more than 99.5% densification is achieved while only ~2% and ~0.5% of the total defects are characterized as keyhole and lack of fusion defects, respectively.
基金This work was funded by the National Natural Science Foundation of China(No.U2037601 and No.52074183)The authors appreciate Ge Chen,Wenbin Zou as well as Shiwei Wang for preparing the alloys,Wenyu Liu as well as Xuehao Zheng from ZKKF(Beijing)Science&Technology Co.,Ltd for the TEM measurement,Gert Wiese as well as Petra Fischer for SEM and hardness measurement and Yunting Li from the Instrument Analysis Center of Shanghai Jiao Tong University(China)for SEM measurement.Lixiang Yang also gratefully thanks the China Scholarship Council(201906230111)for awarding a fellowship to support his study stay at Helmholtz-Zentrum Geesthacht.
文摘In order to improve the ductility of commercial WE43 alloy and reduce its cost,a Mg-3Y-2Gd-1Nd-0.4Zr alloy with a low amount of rare earths was developed and prepared by sand casting with a differential pressure casting system.Its microstructure,mechanical properties and fracture behaviors in the as-cast,solution-treated and as-aged states were evaluated.It is found that the aged alloy exhibited excellent comprehensive mechanical properties owing to the fine dense plate-shapedβ'precipitates formed on prismatic habits during aging at 200℃for 192 hrs after solution-treated at 500℃for 24 hrs.Its ultimate tensile strength,yield strength,and elongation at ambient temperature reach to 319±10 MPa,202±2 MPa and 8.7±0.3%as well as 230±4 MPa,155±1 MPa and 16.0±0.5%at 250℃.The fracture mode of as-aged alloy was transferred from cleavage at room temperature to quasi-cleavage and ductile fracture at the test temperature 300℃.The properties of large-scale components fabricated using the developed Mg-3Y-2Gd-1Nd-0.4Zr alloy are better than those of commercial WE43 alloy,suggesting that the new developed alloy is a good candidate to fabricate the large complex thin-walled components.
