Influence of heat treatment on microstructure,mechanical and corrosion behavior of WE43 alloy fabricated by laser-beam powder bed fusion

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.

Influence of layer thickness on formation quality,microstructure,mechanical properties,and corrosion resistance of WE43 magnesium alloy fabricated by laser powder bed fusion

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.

Alloy design for laser powder bed fusion additive manufacturing:a critical review

Metal additive manufacturing(AM)has been extensively studied in recent decades.Despite the significant progress achieved in manufacturing complex shapes and structures,challenges such as severe cracking when using existing alloys for laser powder bed fusion(L-PBF)AM have persisted.These challenges arise because commercial alloys are primarily designed for conventional casting or forging processes,overlooking the fast cooling rates,steep temperature gradients and multiple thermal cycles of L-PBF.To address this,there is an urgent need to develop novel alloys specifically tailored for L-PBF technologies.This review provides a comprehensive summary of the strategies employed in alloy design for L-PBF.It aims to guide future research on designing novel alloys dedicated to L-PBF instead of adapting existing alloys.The review begins by discussing the features of the L-PBF processes,focusing on rapid solidification and intrinsic heat treatment.Next,the printability of the four main existing alloys(Fe-,Ni-,Al-and Ti-based alloys)is critically assessed,with a comparison of their conventional weldability.It was found that the weldability criteria are not always applicable in estimating printability.Furthermore,the review presents recent advances in alloy development and associated strategies,categorizing them into crack mitigation-oriented,microstructure manipulation-oriented and machine learning-assisted approaches.Lastly,an outlook and suggestions are given to highlight the issues that need to be addressed in future work.

Microstructure and thermal properties of dissimilar M300–CuCr1Zr alloys by multi-material laser-based powder bed fusion

Multi-material laser-based powder bed fusion (PBF-LB) allows manufacturing of parts with 3-dimensional gradient and additional functionality in a single step. This research focuses on the combination of thermally-conductive CuCr1Zr with hard M300 tool steel.Two interface configurations of M300 on CuCr1Zr and CuCr1Zr on M300 were investigated. Ultra-fine grains form at the interface due to the low mutual solubility of Cu and steel. The material mixing zone size is dependent on the configurations and tunable in the range of0.1–0.3 mm by introducing a separate set of parameters for the interface layers. Microcracks and pores mainly occur in the transition zone.Regardless of these defects, the thermal diffusivity of bimetallic parts with 50vol% of CuCr1Zr significantly increases by 70%–150%compared to pure M300. The thermal diffusivity of CuCr1Zr and the hardness of M300 steel can be enhanced simultaneously by applying the aging heat treatment.

Microstructure evolution and strengthening mechanism of high -performance powder metallurgy TA15 titanium alloy by hot rolling

Hot deformation of sintered billets by powder metallurgy(PM)is an effective preparation technique for titanium alloys,which is more significant for high-alloying alloys.In this study,Ti–6.5Al–2Zr–Mo–V(TA15)titanium alloy plates were prepared by cold press-ing sintering combined with high-temperature hot rolling.The microstructure and mechanical properties under different process paramet-ers were investigated.Optical microscope,electron backscatter diffraction,and others were applied to characterize the microstructure evolution and mechanical properties strengthening mechanism.The results showed that the chemical compositions were uniformly dif-fused without segregation during sintering,and the closing of the matrix craters was accelerated by increasing the sintering temperature.The block was hot rolled at 1200℃ with an 80%reduction under only two passes without annealing.The strength and elongation of the plate at 20–25℃ after solution and aging were 1247 MPa and 14.0%,respectively,which were increased by 24.5%and 40.0%,respect-ively,compared with the as-sintered alloy at 1300℃.The microstructure was significantly refined by continuous dynamic recrystalliza-tion,which was completed by the rotation and dislocation absorption of the substructure surrounded by low-angle grain boundaries.After hot rolling combined with heat treatment,the strength and plasticity of PM-TA15 were significantly improved,which resulted from the dense,uniform,and fine recrystallization structure and the synergistic effect of multiple slip systems.

Effect of solution treatment on the microstructure,phase transformation behavior and functional properties of NiTiNb ternary shape memory alloys fabricated via laser powder bed fusion in-situ alloying

Post-heat treatment is commonly employed to improve the microstructural homogeneity and enhance the mechanical performances of the additively manufactured metallic materials.In this work,a ternary(NiTi)91Nb9(at.%)shape memory alloy was produced by laser powder bed fusion(L-PBF)using pre-alloyed NiTi and elemental Nb powders.The effect of solution treatment on the microstructure,phase transformation behavior and mechanical/functional performances was investigated.The in-situ alloyed(NiTi)91Nb9 alloy exhibits a submicron cellular-dendritic structure surrounding the supersaturated B2-NiTi matrix.Upon high-temperature(1273 K)solution treatment,Nb-rich precipitates were precipitated from the supersaturated matrix.The fragmentation and spheroidization of the NiTi/Nb eutectics occurred during solution treatment,leading to a morphological transition from mesh-like into rod-like and sphere-like.Coarsening of theβ-Nb phases occurred with increasing holding time.The martensite transformation temperature increases after solution treatment,mainly attributed to:(i)reduced lattice distortion due to the Nb expulsion from the supersaturated B2-NiTi,and(ii)the Ti expulsion from theβ-Nb phases that lowers the ratio Ni/Ti in the B2-NiTi matrix,which resulted from the microstructure changes from non-equilibrium to equilibrium state.The thermal hysteresis of the solutionized alloys is around 145 K after 20%pre-deformation,which is comparable to the conventional NiTiNb alloys.A short-term solution treatment(i.e.at 1273 K for 30 min)enhances the ductility and strength of the as-printed specimen,with the increase of fracture stress from(613±19)MPa to(781±20)MPa and the increase of fracture strain from(7.6±0.1)%to(9.5±0.4)%.Both the as-printed and solutionized samples exhibit good tensile shape memory effects with recovery rates>90%.This work suggests that post-process heat treatment is essential to optimize the microstructure and improve the mechanical performances of the L-PBF in-situ alloyed parts.

Effect of process parameters on microstructure and mechanical properties of a nickel-aluminum-bronze alloy fabricated by laser powder bed fusion

This work investigated the effect of process parameters on densification,microstructure,and mechanical properties of a nickel-aluminum-bronze(NAB)alloy fabricated by laser powder bed fusion(LPBF)additive manufacturing.The LPBF-printed NAB alloy samples with relative densities of over 98.5%were obtained under the volumetric energy density range of 200−250 J/mm^(3).The microstructure of the NAB alloy printed in both horizontal and vertical planes primarily consisted ofβ'martensitic phase and bandedαphase.In particular,a coarser-columnar grain structure and stronger crystallographic texture were achieved in the vertical plane,where the maximum texture intensity was 30.56 times greater than that of random textures at the(100)plane.Increasing the volumetric energy density resulted in a decrease in the columnar grain size,while increasing the amount ofαphase.Notably,β_(1)'martensitic structures with nanotwins and nanoscaleκ-phase precipitates were identified in the microstructure of LPBF-printed NAB samples with a volumetric energy density of 250 J/mm^(3).Furthermore,under optimal process parameters with a laser power of 350 W and scanning speed of 800 mm/s,significant improvements were observed in the microhardness(HV 386)and ultimate tensile strength(671 MPa),which was attributed to an increase in refined acicular martensite.

Micro-aluminum powder with bi-or tri-component alloy coating as a promising catalyst:Boosting pyrolysis and combustion of ammonium perchlorate

A novel design of micro-aluminum(μAl)powder coated with bi-/tri-component alloy layer,such as:Ni-P and Ni-P-Cu(namely,Al@Ni-P,Al@Ni-P-Cu,respectively),as combustion catalysts,were introduced to release its huge energy inside Al-core and promote rapid pyrolysis of ammonium perchlorate(AP)at a lower temperature in aluminized propellants.The microstructure of Al@Ni-P-Cu demonstrates that a three-layer Ni-P-Cu shell,with the thickness of~100 nm,is uniformly supported byμAl carrier(fuel unit),which has an amorphous surface with a thickness of~2.3 nm(catalytic unit).The peak temperature of AP with the addition of Al@Ni-P-Cu(3.5%)could significantly drop to 316.2℃ at high-temperature thermal decomposition,reduced by 124.3℃,in comparison to that of pure AP with 440.5℃.It illustrated that the introduction of Al@Ni-P-Cu could weaken or even eliminate the obstacle of AP pyrolysis due to its reduction of activation energy with 118.28 kJ/mol.The laser ignition results showed that the ignition delay time of Al@Ni-P-Cu/AP mixture with 78 ms in air is shorter than that of Al@Ni-P/AP(118 ms),decreased by 33.90%.Those astonishing breakthroughs were attributed to the synergistic effects of adequate active sites on amorphous surface and oxidation exothermic reactions(7597.7 J/g)of Al@Ni-P-Cu,resulting in accelerated mass and/or heat transfer rate to catalyze AP pyrolysis and combustion.Moreover,it is believed to provide an alternative Al-based combustion catalyst for propellant designer,to promote the development the propellants toward a higher energy.

Laser powder bed fusion additive manufacturing of NiTi shape memory alloys: a review

NiTi alloys have drawn significant attentions in biomedical and aerospace fields due to their unique shape memory effect(SME),superelasticity(SE),damping characteristics,high corrosion resistance,and good biocompatibility.Because of the unsatisfying processabilities and manufacturing requirements of complex NiTi components,additive manufacturing technology,especially laser powder bed fusion(LPBF),is appropriate for fabricating NiTi products.This paper comprehensively summarizes recent research on the NiTi alloys fabricated by LPBF,including printability,microstructural characteristics,phase transformation behaviors,lattice structures,and applications.Process parameters and microstructural features mainly influence the printability of LPBF-processed NiTi alloys.The phase transformation behaviors between austenite and martensite phases,phase transformation temperatures,and an overview of the influencing factors are summarized in this paper.This paper provides a comprehensive review of the mechanical properties with unique strain-stress responses,which comprise tensile mechanical properties,thermomechanical properties(e.g.critical stress to induce martensitic transformation,thermo-recoverable strain,and SE strain),damping properties and hardness.Moreover,several common structures(e.g.a negative Poisson’s ratio structure and a diamond-like structure)are considered,and the corresponding studies are summarized.It illustrates the various fields of application,including biological scaffolds,shock absorbers,and driving devices.In the end,the paper concludes with the main achievements from the recent studies and puts forward the limitations and development tendencies in the future.

Investigation of the Laser Powder Bed Fusion Process of Ti-6.5Al-3.5Mo-1.5Zr-0.3Si Alloy

Laser powder bed fusion(LPBF)is an advanced manufacturing technology;however,inappropriate LPBF process parameters may cause printing defects in materials.In the present work,the LPBF process of Ti-6.5Al-3.5Mo-1.5Zr-0.3Si alloy was investigated by a two-step optimization approach.Subsequently,heat transfer and liquid flow behaviors during LPBF were simulated by a well-tested phenomenological model,and the defect formation mechanisms in the as-fabricated alloy were discussed.The optimized process parameters for LPBF were detected as laser power changed from 195 W to 210 W,with scanning speed of 1250 mm/s.The LPBF process was divided into a laser irradiation stage,a spreading flow stage,and a solidification stage.The morphologies and defects of deposited tracks were affected by liquid flow behavior caused by rapid cooling rates.The findings of this research can provide valuable support for printing defect-free metal components.

Powder mixed electrochemical discharge process for micro machining of C103 niobium alloy

This work demonstrates the viability of the powder-mixed micro-electrochemical discharge machining(PMECDM) process to fabricate micro-holes on C103 niobium-based alloy for high temperature applications.Three processes are involved simultaneously i.e.spark erosion,chemical etching,and abrasive grinding for removal of material while the classical electrochemical discharge machining process involves double actions i.e.spark erosion,and chemical etching.The powder-mixed electrolyte process resulted in rapid material removal along with a better surface finish as compared to the classical microelectrochemical discharge machining(MECDM).Further,the results are optimized through a multiobjective optimization approach and study of the surface topography of the hole wall surface obtained at optimized parameters.In the selected range of experimental parameters,PMECDM shows a higher material removal rate(MRR) and lower surface roughness(R_(a))(MRR:2.8 mg/min and R_(a) of 0.61 μm) as compared to the MECDM process(MRR:2.01 mg/min and corresponding Raof 1.11 μm).A detailed analysis of the results is presented in this paper.

Ballistic performance of titanium-based layered composites made using blended elemental powder metallurgy and hot isostatic pressing

Metal matrix composites tiles based on Ti-6Al-4V(Ti64)alloy,reinforced with 10,20,and 40(vol%)of either TiC or TiB particles were made using press-and-sinter blended elemental powder metallurgy(BEPM)and then bonded together into 3-layer laminated plates using hot isostatic pressing(HIP).The laminates were ballistically tested and demonstrated superior performance.The microstructure and properties of the laminates were analyzed to determine the effect of the BEPM and HIP processing on the ballistic properties of the layered plates.The effect of porosity in sintered composites on further diffusion bonding of the plates during HIP is analyzed to understand the bonding features at the interfaces between different adjacent layers in the laminate.Exceptional ballistic performance of fabricated structures was explained by a significant reduction in the residual porosity of the BEPM products by their additional processing using HIP,which provides an unprecedented increase in the hardness of the layered composites.It is argued that the combination of the used two technologies,BEPM and HIP is principally complimentary for the materials in question with the abilities to solve the essential problems of each used individually.

Oxygen variation in titanium powder and metal injection molding

The control of oxygen is paramount in achieving high-performance titanium(Ti)parts by powder metallurgy such as metal in-jection molding(MIM).In this study,we purposely selected the Ti and Ti-6Al-4V powders as the reference materials since these two are the most representative Ti materials in the industry.Herein,hydride-dehydride(HDH)Ti powders were pre-oxidized to examine the ef-fect of oxygen variation on the characteristics of oxide layer on the particle surface and its resultant color feature.The results indicate that the thickness and Ti oxide level(Ti^(0)→Ti^(4+))of the oxide layer on the HDH Ti powders increased as the oxygen content increased,lead-ing to the transition of color appearance from grey,brown to blue.This work aids in the powder feedstock selection at the initial stage in powder metallurgy.In addition,the development of oxygen content was comprehensively studied during the MIM process using the gas-atomized(GA)Ti-6Al-4V powders.Particularly,the oxygen variation in the form of oxide layer,the change of oxygen content in the powders,and the relevant parts were investigated during the processes of kneading,injection,debinding,and sintering.The oxygen vari-ation was mainly concentrated in the sintering stage,and the content increased with the increase of sintering temperature.The variation of oxygen content during the MIM process demonstrates the crucial role of powder feedstock and sintering stage in controlling oxygen con-tent.This work provides a piece of valuable information on oxygen detecting,control,and manipulation for the powder and processing in the industry of Ti and its alloys by powder metallurgy.

Improving corrosion resistance of additively manufactured WE43 magnesium alloy by high temperature oxidation for biodegradable applications

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.

Preparation of ultra-fine fibrous Fe-Ni alloy powder by coordinated co-precipitation-direct reduction process

The precursor prepared by coordinated co-precipitation was direct reduced by hydrogen to ultra-fine fibrous Fe-Ni alloy powder. The effects of concentrations of reactants, pH value, reaction temperature and additive on the preparation of precursor were systematically investigated. The structures, thermal decomposition processes and morphologies of the precursors were characterized by X-ray diffraction (XRD), thermal gravity-differential thermal analysis (TG-DTA) and scanning electron microscoy (SEM). The results show that using 2% polyvinylpyrrolidone (PVP) (in mass fraction) as additive, a well-dispersed precursor with a uniform morphology can be obtained in a solution with Fe2+ and Ni2+ total concentration (1:1) of 0.8 mol/L, pH value of 6.2 at 60 °C, and a pure and well dispersed fibrous iron-nickel powder can be prepared by direct reduction of this precursor in a mixed atmosphere of nitrogen and hydrogen at the temperature of 420 °C.

Shape-controlled synthesis of novel precursor for fibrous Ni-Co alloy powders

A novel precursor of nickel-cobalt alloy powders with an appropriate Ni to Co molar ratio was prepared under selectively synthetic conditions. The composition and morphology of the precursor were characterized by X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared spectrometry （FT-IR） and energy dispersive spectrometry （EDS）. The effects of pH value, reaction temperature, metal ion concentrations and surfactant on the morphology and the dispersion of precursor were investigated. The results show that the morphology of precursor depends on ammonia content in the precursor. A fibriform precursor is a complicated ammonia-containing nickel-cobalt oxalate. The uniform shape-controlled fibrous precursor is obtained under the following optimum conditions： ammonia as complex agent as well as pH adjustor, oxalate as coprecipitator, 50-65 °C of reaction temperature, 0.5-0.8 mol/L of total concentration of Ni2＋ and Co2＋, PVP as dispersant, and pH 8.0-8.4.

Phase transformation and damping behavior of lightweight porous TiNiCu alloys fabricated by powder metallurgy process

Porous TiNiCu ternary shape memory alloys （SMAs） were successfully fabricated by powder metallurgy method. The microstructure, martensitic transformation behavior, damping performance and mechanical properties of the fabricated alloys were intensively studied. It is found that the apparent density of alloys decreases with increasing the Cu content, the porous Ti50Ni40Cu10 alloy exhibits wide endothermic and exothermic peaks arisen from the hysteresis of martensitic transformations, while the porous Ti50Ni30Cu20 alloy shows much stronger and narrower endothermic and exothermic peaks owing to the B2-B19 transformation taking place easily. Moreover, the porous Ti50Ni40Cu10 alloy shows a lower shape recovery rate than the porous Ti50Ni50 alloy, while the porous Ti50Ni30Cu20 alloy behaves reversely. In addition, the damping capacity （or internal friction, IF） of the porous TiNiCu alloys increases with increasing the Cu content. The porous Ti50Ni30Cu20 alloy has very high equivalent internal friction, with the maximum equivalent internal friction value five times higher than that of the porous Ti50Ni50 alloy.

Deformation behaviors and processing maps of CNTs/Al alloy composite fabricated by flake powder metallurgy

Deformation behaviors of CNTs/Al alloy composite fabricated by the method of flake powder metallurgy were investigated by hot compression tests, which were performed in the temperature range of 300?550 °C and strain rate range of 0.001? 10 s?1 with Gleeble?3500 thermal simulator system. Processing maps of the CNTs/Al alloy at different strains were calculated to study the optimum processing domain. Microstructures before and after hot compressions were characterized by electron backscattered diffraction (EBSD) method. Stress?strain curves indicate that the flow stress increases with the increase of strain rate and the decrease of temperature. The processing maps of the CNTs/Al alloy at different strains show that the optimum processing domain is 500?550 °C, 10 s?1 for hot working. EBSD analysis demonstrates that fully dynamic recrystallization occurs in the optimum processing domain (high strainrate 10 s?1), whereas the main soften mechanism is dynamic recovery at low strain rate (0.001 s?1).

扁平化Fe-Si-Al合金粉末的磁特性

采用砂磨工艺对水雾化Fe—Si—Al合金粉末进行扁平化处理，分别采用扫描电镜、红外吸收光谱表征样品结构，用振动样品磁强计测试静磁参数，并在2～18GHz范围内测试复数磁导率．结果表明。砂磨处理时间增加，粉末的扁平率增大；粉末表面存在偶联剂包覆层，饱和磁化强度增大、矫顽力降低；微波特性方面，材料在测试频率范围内具有良好的频率响应特性，随着扁平率增大，样品在同频率下的复数磁导率实部和虚部均相应提高，自然共振频率向高频移动．

Fe-Si-Al系合金粉微波吸收特性

采用扁平化工艺以及绝缘包覆工艺对铁硅铝系软磁合金粉末进行改性。对实验样品进行扫描电镜分析，观察颗粒形貌对材料性能的影响；探讨球磨时间以及不同绝缘介质含量对于材料电磁性能的影响规律。根据单层吸波材料（含导电衬底）对电磁波的反射率公式的分析以及对不同样品反射率的计算可知，球磨扁平化工艺以及绝缘包覆工艺可有效地改善铁硅铝金属粉末的微波吸收性能。经改性后的铁硅铝系软磁金属粉末在1．0～3．5GHz频段具有较好的吸波性能，可应用于抗电磁干扰领域。