Spark Plasma Sintering of Mg-based Alloys:Microstructure,Mechanical Properties,Corrosion Behavior,and Tribological Performance

Within the past ten years,spark plasma sintering(SPS)has become an increasingly popular process for Mg manufacturing.In the SPS process,interparticle diffusion of compressed particles is rapidly achieved due to the concept of Joule heating.Compared to traditional and additive manufacturing(AM)techniques,SPS gives unique control of the structural and microstructural features of Mg components.By doing so,their mechanical,tribological,and corrosion properties can be tailored.Although great advancements in this field have been made,these pieces of knowledge are scattered and have not been contextualized into a single work.The motivation of this work is to address this scientific gap and to provide a groundwork for understanding the basics of SPS manufacturing for Mg.To do so,the existing body of SPS Mg literature was first surveyed,with a focus on their structural formation and degradation mechanisms.It was found that successful Mg SPS fabrication highly depended on the processing temperature,particle size,and particle crystallinity.The addition of metal and ceramic composites also affected their microstructural features due to the Zener pinning effect.In degradative environments,their performance depends on their structural features and whether they have secondary phased composites.In industrial applications,SPS'd Mg was found to have great potential in biomedical,hydrogen storage,battery,automotive,and recycling sectors.The prospects to advance the field include using Mg as a doping agent for crystallite size refinement and using bulk metallic Mg-based glass powders for amorphous SPS components.Despite these findings,the interactions of multi-composites on the processing-structure-property relationships of SPS Mg is not well understood.In total,this work will provide a useful direction in the SPS field and serve as a milestone for future Mg-based SPS manufacturing.

Spark plasma sintering of tungsten-based WTaVCr refractory high entropy alloys for nuclear fusion applications

W-based WTaVCr refractory high entropy alloys (RHEA) may be novel and promising candidate materials for plasma facing components in the first wall and diverter in fusion reactors. This alloy has been developed by a powder metallurgy process combining mechanical alloying and spark plasma sintering (SPS). The SPSed samples contained two phases, in which the matrix is RHEA with a body-centered cubic structure, while the oxide phase was most likely Ta2VO6through a combined analysis of X-ray diffraction (XRD),energy-dispersive spectroscopy (EDS), and selected area electron diffraction (SAED). The higher oxygen affinity of Ta and V may explain the preferential formation of their oxide phases based on thermodynamic calculations. Electron backscatter diffraction (EBSD) revealed an average grain size of 6.2μm. WTaVCr RHEA showed a peak compressive strength of 2997 MPa at room temperature and much higher micro-and nano-hardness than W and other W-based RHEAs in the literature. Their high Rockwell hardness can be retained to at least 1000°C.

Microstructure and corrosion behavior of NiTi shape memory alloys sintered in the SPS process

NiTi shape memory alloys(SMAs) was developed using the spark-plasma sintering(SPS) process with different average particle size(45 μm and 10 μm) under various temperature. The influence of particle size and temperature on the density, microstructure, and corrosion behavior of the NiTi in simulated body fluid was examined. The porosity decreased with increasing sintering temperature and decreasing particle size, which resulted in an increase in density of the alloy. Increasing the sintering temperature led to the formation of Ni-and Ti-rich intermetallic such as Ni3Ti and NiTi2. The formation of these secondary phases influenced the corrosion behavior of NiTi by changing its chemical composition. The planar structure of NiTi was transformed into a dendritic structure at 900℃, which resulted in the formation of uniform oxide and phosphate layers on the entire surface. A high corrosion potential and low corrosion current density were achieved with NiTi prepared with 10 μm particles at 900℃, which exhibited superior corrosion resistance.

Phase structure and electrochemical properties of laser sintered La_2MgNi_9 hydrogen storage electrode alloys

Phase structure and electrochemical properties of laser sintered La2MgNi9 alloys were studied. The sintered alloys contained a main phase, LaNi5, and a ternary La-Mg-Ni phase, with a PuNi3 structure and a small amount of LaMgNi4. The ternary La-Mg-Ni phase with a PuNi3 structure had the composition of La1.8Mg1.2Ni9 and La2MgNi9, for alloys laser sintered at 1000 and 1400 W, respectively. Owing to further reactions between LaNi5 and LaMgNi4, the amount of the PuNi3 phase increased for alloys sintered at 1400 W. Both alloys had good activation property （three charge/discharge cycles）. The discharge capacities of the sintered alloys were 321.8 and 344.8 mAh/g, respectively. Compared with the alloy laser sintered at 1000 W, the poor cyclic stability of the alloy sintered at 1400 W was mainly attributed to the lower corrosion resistance of the La2MgNi9 phase.

Phase component and microstructure of laser-sintered Mg-Ni alloys

The Mg-Ni hydrogen storage alloys were prepared using the laser sintering technology. The effects of laser sintering power on the phase component and the weight loss of Mg element for the Mg-Ni alloys were investigated. The samples P1, P2 and P3 consisted of five phases： Mg2Ni, MgNi2, Mg, Ni and MgO. The weight loss of Mg element remarkably increased at 1200 W. The addition of extra Mg significantly promoted the reaction between Mg and Ni. Mg2Ni, MgNi2, and a small amount of Ni and MgO phases were present in the samples PM （pestie milling） and BM （ball milling）. The sample PM has a homogeneous microstructure, and the contents of Mg2Ni and MgNi2 were approximately consistent with those of the Mg-Ni alloy under the equilibrium conditions. The maximum hydrogen storage capacity of the sample BM was 1.72 wt.% and the sample can be activated easily at 573 K （only 3 activation cycles）.

Microstructure and mechanical properties of spark plasma sintered Ti–Mo alloys for dental applications

Ti-Mo alloys with various Mo contents from 6wt% to 14wt% were processed by spark plasma sintering based on elemental pow- ders. The influence of sintering temperature and Mo content on the microstructure and mechanical properties of the resulting alloys were investigated. For each Mo concentration, the optimum sintering temperature was determined, resulting in a fully dense and uniform microstructure of the alloy. The optimized sintering temperature gradually increases in the range of 1100-1300℃ with the increase in Mo content. The microstructure of the Ti-（6-12）Mo ahoy consists of acicular α phase surrounded by equiaxed grains of 13 phase, while the Ti-14Mo al- loy only contains single 13 phase. A small amount of fine α lath precipitated from 13 phase contributes to the improvement in strength and hardness of the alloys. Under the sintering condition at 1250℃, the Ti-12Mo alloy is found to possess superior mechanical properties with the Vickers hardness of Hv 472, the compressive yield strength of 2182 MPa, the compression rate of 32.7%, and the elastic modulus of 72.1 GPa. These results demonstrate that Ti-Mo alloys fabricated via spark plasma sintering are indeed a perspective candidate alloy for dental applications.

Microstructure Analysis of Microwave Sintered Ferrous PM Alloys

The properties and microstructure of microwave and conventional sintered Fe-2Cu-0.6C powder metallurgy （PM） alloys were investigated. The experimental results show that microwave sintered alloy has the better properties （sintered density 7.20 g/cm3, Rockwell hardness 75 HRB, tensile strength 413.90 MPa and elongation 6.0%）, compared with the conventional sintered counterpart. Detailed analyses by using optical microscopy and scanning electron microscopy （SEM） reveal that microwave sintered sample has finer microstructure with small, rounded and uniformly distributed pores, and also demonstrate the presence of more flaky and granular pearlite in the mi- crowave sintered body, both of which account for the property improvement. SEM images on the fracture morphology indicate that a mixed mode containing ductile and brittle fracture is presented in microwave sintered alloy, in contrast with the brittle fracture in conventional sintered counterpart.

Consolidation and Microstructures of Microwave Sintered W-25Cu Alloys with Fe Addition

W-25Cu alloys were microwave sintered in a 2.45 GHz multimode applicator.The densification,microstructure and their dependence on sintering mode and Fe addition were investigated in detail.Owing to the volumetric heating intrinsic in microwave processing,a microstructure with larger W grain size in center regions was observed as against larger grain size in edge regions for conventional sintering.Microwave sintering demonstrates its intrinsic advantages such as rapid heating rate,densification enhancement and microstructural homogeneity;but it undesirably promotes W grain growth.Under microwave sintering,the role of Fe addition on compact consolidation is not so substantial as under conventional sintering.Moreover Fe degrades the microstructural quality,generating worse uniformity and coarser W grains.

THE RELATION BETWEEN THE TEMPERING EFFECTS AND THE INTRINSIC COERCIVITY OF SINTERED SmCo5 ALLOY AT 750℃

The relation between the tempering effects of sinterd SmCo^(5)alloy at 750℃and its intrinsic coercivity(i^(Hc))has been studied by the use of photoelectron energy spectrum.X-ray diffraction and high-voltage electron microscope.The result is that the cause of iHc dropping seriously for sintered SmCo_(5)alloy tempered at 750 t is not the eutectoid decomposition of SmCo_(5)and the increase of oxygen.In fact,iHcdropping is caused by that some defect-rich regions in Sm_(2)Co_(17)decomposed form SmC0_(5)from nucleation centers in reversed magnetization course.

Microstructure and properties of liquid-phase sintered tungsten heavy alloys by using ultra-fine tungsten powders

The microstructure and properties of liquid-phase sintered 93W-4.9Ni-2.1Fe tungsten heavy alloys using ultra-fine tungsten powders (medium particle size of 700 nm) and original tungsten powders (medium particle size of 3 μm) were investigated respectively. Commercial tungsten powders (original tungsten powders) were mechanically milled in a high-energy attritor mill for 35 h. Ultra-fine tungsten powders and commercial Ni, Fe powders were consolidated into green compacts by using CIP method and liquid-phase sintering at 1 465 ℃ for 30 min in the dissociated ammonia atmosphere. Liquid-phase sintered tungsten heavy alloys using ultra-fine tungsten powders exhibit full densification (above 99% in relative density) and higher strength and elongation compared with conventional liquid-phase sintered alloys using original tungsten powders due to lower sintering temperature at 1 465 ℃ and short sintering time. The mechanical properties of sintered tungsten heavy alloy are found to be mainly dependent on the particles size of raw tungsten powders and liquid-phase sintering temperature.

Pressure sintering of W-15wt.%Cu alloys prepared by mechanical alloying as a subsequent densification treatment method

The sintered W-15wt.%Cu alloys fabricated by mechanical alloying were re-sintered under pressure to increase the density and improve the properties of these alloys. The pressure was applied vertically along the axis of the sintered sample. Properties such as density, hardness, and bending strength were measured. The microstructures of the sintered bodies were observed. The results showed that the subsequent pressure sintering could increase the density of the sintered W-15wt.%Cu alloys. Their hardness, bending strength, and some other physical properties were also improved by this subsequent densification treatment.

Influence of sintering time on microstructure and properties of hot oscillatory pressing sintered W–Cu refractory alloys

W–Cu refractory alloys are widely used in aerospace,aviation,electronics,power,and other fi elds.However,because of its large melting point diff erence between alloy elements,the conventional powder metallurgy method required a long time of high temperature sintering is very likely to cause low density and abnormal grain size growth.Therefore,90W-10Cu refractory alloys were successfully prepared by hot oscillatory pressing(HOP)under diff erent sintering time in this work.Then the infl uence of sintering time on the microstructure,grain size,density,Vickers hardness,room-tensile property,and electrical conductivity of the W–Cu refractory alloy was systematically invested.The results showed that during the short sintering time(30–90 min),the density,Vickers hardness,tensile strength,and electrical conductivity of the W–Cu refractory alloy increased signifi cantly to 98.7%,163.29 HV 30,507.3 MPa,and 14.2%International Annealed Copper Standard with the sintering time increasing,respectively,while its grain size showed no obvious change.When the sintering time further increased to 120 min,the density was basically consistent with the sintering time of 90 min.Nevertheless,the prolonged high temperature sintering resulted in the grain growth of the samples,which caused the deterioration of the Vickers hardness,room-tensile strength,and conductivity properties of the W–Cu refractory alloy.At the same sintering time,the density,Vickers hardness,and electrical conductivity of the HOP sintered W–Cu refractory alloy were signifi cantly higher than those of the HP sintered sample.It was indicated that high density,fi ne-grain,and excellent properties W–Cu refractory alloys could be prepared by hot oscillatory pressing under appropriate sintering time.

High-temperature mechanical properties and deformation behavior of high Nb containing TiAl alloys fabricated by spark plasma sintering

A high Nb containing TiA1 alloy was prepared from the pre-alloyed powder of Ti-45Al-8.5Nb-0.2B-0.2W-0.02Y （at%） by spark plasma sintering （SPS）. Its high-temperature mechanical properties and compressive deformation behavior were investigated in a temperature range of 700 to 1050℃ and a strain rate range of 0.002 to 0.2 s 1. The results show that the high-temperature mechanical properties of the high Nb containing TiA1 alloy are sensitive to deformation temperature and strain rate, and the sensitivity to strain rate tends to rise with the deformation temperature increasing. The hot workability of the alloy is good at temperatures higher than 900℃, while fracture occurs at lower temperatures. The flow curves of the samples compressed at or above 900℃ exhibit obvious flow softening after the peak stress. Un- der the deformation condition of 900-1050℃ and 0.002-0.2 s 1, the interrelations of peak flow stress, strain rate, and deformation tempera- ture follow the Arrhenius＇ equation modified by a hyperbolic sine function with a stress exponent of 5.99 and an apparent activation energy of 441.2 kJ.mol-1.

Spark plasma and microwave sintering of Al6061 and Al2124 alloys

Despite the importance of aluminum alloys as candidate materials for applications in aerospace and automotive industries, very little work has been published on spark plasma and microwave processing of aluminum alloys. In the present work, the possibility was explored to process A12124 and A16061 alloys by spark plasma and microwave sintering techniques, and the microstructures and properties were compared. The alloys were sintered for 20 rain at 400, 450, and 500℃. It is found that compared to microwave sintering, spark plasma sintering is an effective way to obtain homogenous, dense, and hard alloys. Fully dense （100%） A16061 and A12124 alloys were obtained by spark plasma sintering for 20 rain at 450 and 500℃, respectively. Maximum relative densities were achieved for A16061 （92.52%） and A12124 （93.52%） alloys by microwave sintering at 500℃for 20 min. The Vickers microhardness of spark plasma sintered samples increases with the increase of sintering temperature from 400 to 500℃, and reaches the values of Hv 70.16 and Hv 117.10 for A16061 and A12124 alloys, respectively. For microwave siutered samples, the microhardness increases with the increase of sintering temperature from 400 to 450℃, and then decreases with the further increase of sintering temperature to 500~C.

Microstructure, thermal properties, and corrosion behaviors of FeSiBAlNi alloy fabricated by mechanical alloying and spark plasma sintering

An equiatomic FeSiBAlNi amorphous high-entropy alloy （HEA） was fabricated by mechanical alloying （MA）. A fully amorphous phase was obtained in the FeSiBAlNi HEA after 240 h of MA. The bulk FeSiBAlNi samples were sintered by spark plasma sintering （SPS） at 520 and 1080℃ under a pressure of 80 MPa. The sample sintered at 520℃ exhibited an amorphous composite structure comprising solid-solution phases （body-centered cubic （bcc） and face-centered cubic （fee） phases）. When the as-milled amorphous HEA was consoli- dated at 1080℃, another fcc phase appeared and the amorphous phase disappeared. The sample sintered by SPS at 1080℃ exhibited a slightly higher melting temperature compared with those of the as-milled alloy and the bulk sample sintered at 520℃. The corrosion behav- iors of the as-sintered samples were investigated by potentiodynamic polarization measurements and immersion tests in seawater solution. The results showed that the HEA obtained by SPS at 1080℃ exhibited better corrosion resistance than that obtained by SPS at 520℃.

Sintering behavior, microstructure and properties of TiC-FeCr hard alloy

TiC based cermets were produced with FeCr, as a binder, by conventional P/M （powder metallurgy） to near 〉97% of the theoretical density. Sintering temperature significantly affects the mechanical properties of the composite. The sintering temperature of 〉1360℃ caused severe chemical reaction between TiC particles and the binder phase. In the TiC-FeCr cermets, the mechanical properties did not vary linearly with the carbide content. Optimum mechanical properties were found in the composite containing 57wt% TiC reinforcement, when sintered at 1360℃ for 1 h. Use of carbon as an additive enhanced the mechanical properties of the composites. Cermets containing carbon as an additive with 49wt% TiC exhibited attractive mechanical properties. The microstructure of the developed composite contained less or no debonding, representing good wettabifity of the binder with TiC particles. Homogeneous distribution of the TiC particles ensured the presence of isotropic mechanical properties and homogeneous distribution of stresses in the composite. Preliminary experiments for evaluation of the oxidation resistance of FeCr bonded TiC cermets indicate that they are more resistant than WC-Co hardmetals.

Fabrication of Iron-base Alloy by Spark Plasma Sintering

Fe-2Cu-2Ni-1Mo-0.8C （wt pct） elemental mixed powders were rapidly sintered within 6 min by spark plasma sintering, and the effects of sintering parameters on the densification degree and performance of the assintered materials were investigated. Results showed that when a proper combination of pulse electric current and constant electric current was employed for sintering, the density and bend strength of the as-sintered material reached the maxima, being 7.61×10^3 kg/m^3 and 1540 MPa, respectively. Its corresponding fracture morphology was characterized as the mix of ductile, intergranular and cleavage fractures.

Microstructure and Properties of W-15Cu Alloys Prepared by Mechanical Alloying and Spark Plasma Sintering Process

W-15Cu composite powders prepared by mechanical alloying （MA） of raw powders were consolidated by spark plasma sintering （SPS） process at temperature ranged 1 230-1 300 ℃ for 10 min and under a pressure of 30 MPa. By using high energy milling, particles containing very fine tungsten grains embedded in copper, called composite particles, could be produced. The W grains were homogeneously dispersed in copper phase, which was very important to obtain W-Cu alloy with high mechanical properties, fine and homogeneous microstructure. The microstructure and properties of W-15Cu alloys prepared by SPS processes at different temperature were researched. The results show that W-15Cu alloys consolidated by SPS can reach 99.6 % relative density, and transverse rupture strength （TRS） is 1 400.9 MPa, Rockwell C hardness （HRC） is 45.2, the thermal conductivity is 196 W/m-K at room temperature, the average grain size is less than 2 μm, and W-15Cu alloy with excellent properties, homogeneous and fine microstructure is obtained.