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.

Hot-press sintering of MA Fe-based nanocrystalline/amorphous soft magnetic powder

Microstructures and magnetic properties of Fe84Nb7B9,Fe80Ti8B 12 and Fe32Ni36（Nb/V）7Si8B17 powders and their bulk alloys prepared by mechanical alloying（MA） method and hot-press sintering were studied. The results show that: 1) After MA for 20 h,nanocrystalline bcc singl e phase supersaturated solid solution forms in Fe84-Nb7B9 and Fe8 0Ti8B12 alloys,amorphous structure forms in Fe32Ni36Nb7 Si8B17 alloy,duplex microstructure composed of nanocrystalline γ- （FeNi） supersaturated solid solution and trace content of Fe2B phase forms in Fe32Ni36-V7Si8B17 alloy. 2) The decomposition process of supersaturated solid solution phases in Fe84Nb7B9 and Fe80Ti8B 12 alloys happens at 710780 ℃,crystallization reaction in Fe （32）Ni36Nb7Si8B17 alloy happens at 530 ℃（the temperature of peak value） and residual amorphous crystallized further happens at 760 ℃ （the temperature of peak value）,phase decomposition process of supersaturated solid solution at 780 ℃ （the temperature of peak value） and crystallization reaction at 431 ℃ （the temperature of peak value） happens in Fe32Ni36V7S i8B17 alloy. 3) under 900 ℃,30 MPa,（0.5 h） hot-press sintering conditions,bulk alloys with high relative density（94.7%95.8%） can be ob tained. Except that the grain size of Fe84Nb7B9 bulk alloy is large,s uperfine grains （grain size 50200 nm） are obtained in other alloys. Exc ept that single phase microstructure is obtained in Fe80Ti8B12 bul k alloy,multi-phase microstructures are obtained in other alloys. 4) The magne tic properties of Fe80Ti8B12bulk alloy（Bs=1.74 T,Hc= 4.35 kA/m） are significantly superior to those of other bulk alloys,which is r elated to the different phases of nanocrystalline or amorphous powder formed dur ing hot-press sintering process and grain size.

Microstructure and mechanical properties of TiAl-based alloy prepared by double mechanical milling and spark plasma sintering

A fine-grained TiAl alloy with a composition of Ti-45Al-2Cr-2Nb-1B-0.5Ta-0.225Y （mole fraction, %） was prepared by double mechanical milling（DMM） and spark plasma sintering（SPS）. The relationship among sintering temperature, microstructure and mechanical properties was studied. The results show that the morphology of double mechanical milled powder is regular with size in the range of 20-40 μm and mainly composed of TiAl and Ti3Al phases. The main phase TiAl and few phases Ti3Al, Ti2Al and TiB2 were observed in the SPSed alloys. For samples sintered at 900 ℃ the equiaxed crystal grain microstructure is achieved with size in the range of 100-200 nm. With increasing the SPS temperature from 900 ℃to 1000 ℃ the size of equiaxed crystal grain obviously increases, the microhardness decreases from HV658 to HV616, and the bending strength decreases from 781 MPa to 652 MPa. In the meantime, the compression fracture strength also decreases from 2769 MPa to 2669 MPa, and the strain to fracture in compression increases from 11.69% to 17.76%. On the base of analysis of fractographies, it shows that the compression fracture transform of the SPSed alloys is intergranular rupture.

Effect of casting vacuum on thermodynamic and corrosion properties of Fe-based glassy alloy

The effect of casting vacuum on thermodynamic and corrosion properties of Fe61Co7Zr8Mo5W2B17 in shape of cylinder of 3 mm in diameter and ribbon of 20?40μm in thickness and 2?3 mm in width were investigated with X-ray diffraction (XRD), differential scanning calorimetry (DSC), dilatometer (DIL), scanning electron microscopy (SEM) and electrochemical station. It is found that high casting vacuum can improve the glass forming ability (GFA), the contraction degree during heating, and the pitting resistance of the glassy alloy, which can be ascribed to the fact that the dissolution of tungsten in the melt is improved under the high casting vacuum.

Microstructure and mechanical properties of Ti-43Al-9V alloy fabricated by spark plasma sintering

A fine-grained TiAl alloy with the composition of Ti-43Al-9V was prepared by mechanical milling and spark plasma sintering（SPS）.The relationship among sintering temperature,microstructure and mechanical properties was studied.The results show that the morphology of mechanical milling powder is regular with size in a range of 5-30 μm.Main phases of γ-TiAl,α2-Ti3Al and few B2 phase are observed in the SPS bulk samples.For samples sintered at 1150 °C,equiaxed crystal grain microstructure is achieved with size in a range of 300 nm-1 μm.With increasing SPS temperature to 1250 °C,the size of equiaxed crystal grains obviously increases,the microhardness decreases from HV592 to HV535,and the bending strength decreases from 605 to 219 MPa.Meantime,the compression fracture strength also decreases from 2601 to 1905 MPa,and the strain compression decreases from 28.95% to 12.09%.

Effect of spark plasma sintering temperature on microstructure and mechanical properties of melt-spun TiAl alloys

A TiAl alloy from pulverized rapidly solidified ribbons with the composition of Ti-46Al-2Cr-4Nb-0.3Y（mole fraction,%） was processed by spark plasma sintering（SPS）.The effects of sintering temperature on the microstructure and mechanical properties were studied.The results show that the microstructure and phase constitution vary with sintering temperature.Sintering the milled powders at 1200 ℃ produces fully dense compact.Higher sintering temperature does not improve the densification evidently.The dominant phases are γ and α2 in the bulk alloys sintered at 1200 ℃.With higher sintering temperature,the fraction of α2 phase decreases and the microstructure changes from equiaxed near γ grain to near lamellar structure,together with a slight coarsening.The bulk alloy sintered at 1260 ℃ with refined and homogeneous near lamellar structure reveals the best overall mechanical properties.The compressional fracture stress and compression ratio are 2984 MPa and 41.5%,respectively,at room temperature.The tensile fracture stress and ductility are 527.5 MPa and 5.9%,respectively,at 800 ℃.

Investigation on sintering and deformation strengthening of Mo-Cu alloy

Mo-Swt%Cu nanocomposite powders were fabricated by mechanical alloying, and full density alloy was obtained via liquid-phase sintering and post-treatment process. The microstructure of Mo-8wt%Cu alloy was investigated by scanning elec-tron microscope （SEM） , and the effects of process parameters on relative density, tensile strength and elongation were stud-ied. The results indicate that the relative density of Mo-Cu alloy is 98. 6% after sintering at 1 250℃ for 30 min, and its micro-structure is composite network The full density of Mo-Cu alloy can be obtained when specimens are treated through deforma-tion strengthening process of rotating forging and hydrostatic extrusion The tensile strength and elongation rate are 576 MPa and 5. 8% ,respectively, when hydrostatic extrusion deformation degree is 40%.

Effect of mechanical alloying and sintering process on microstructure and mechanical properties of Al-Ni-Y-Co-La alloy

Al86Ni7Y4.5Co1La1.5 （mole fraction, %） alloy powder was produced by argon gas atomization process. After high-energy ball milling, the powder was consolidated by vacuum hot press sintering and spark plasma sintering （SPS） under different process conditions. The microstructure and morphology of the powder and consolidated bulk sample were examined by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. It is shown that amorphous phase appears when ball milling time is more than 100 h, and the bulk sample consolidated by SPS can maintain amorphous/ nanocrystalline microstructure but has lower relative density. A compressive strength of 650 MPa of Al86Ni7Y4.5Co1La1.5 nanostructured samples is achieved by vacuum hot extrusion （VHE）.

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.

Structural characteristics and magnetic properties of bulk nanocrystalline Fe_(84)Zr_2Nb_4B_(10) alloy prepared by mechanical alloying and spark plasma sintering consolidation

Magnetic properties of Fe84Zr2Nb4B10 sample were investigated. The sample was produced from nanocrystalline powders made by the mechanical alloying (MA) and consolidation using the spark plasma sintering (SPS) technique. Effects of milling time on phase transformation, structural characteristics, and magnetic properties of powders were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and physical property measure system (PPMS), respectively. Results show that nanostructured α-Fe supersaturated solid solution is obtained in the final MAed products. The saturation magnetization (Ms) increased with increasing milling time and became constant at 130 h, but the coercivity (Hc) increased firstly and then decreased. The consolidated bulk sample exhibited a high density of 6.893 g·cm-3, there was no phase change during SPS process, and the saturation magnetization and susceptibility of the SPSed bulk sample improved in comparison with the milled powders. The variation of magnetic parameters can be explained by nano-scale effect and Herzer model.

Surface hardening of Fe-based alloy powders by Nd:YAG laser cladding followed by electrospark deposition with WC-Co cemented carbide

This paper presents the results of a study concerned with the surface hardening of Fe-based alloys and WC-8Co cemented carbide by inte- grating laser cladding and the electrospark deposition processes. Specimens of low carbon steel were processed firstly by laser cladding with Fe-based alloy powders and then by electrospark deposition with WC-SCo cemented carbide. It is shown that, for these two treatments, the electrospark coating possesses finer microstructure than the laser coating, and the thickness and surface hardness of the electrospark coating can be substantially increased.

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℃.

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.

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.

Microstructure and properties of ultra-fine tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering

The microstructure and properties of the 93W-4Ni-2Co-1Fe(mass fraction,%) tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering from mixed elemental powders were investigated.After 15 h milling,the average W grain size in the powders is decreased to 120 nm.For the powders milled for 15 h,the density,hardness and transverse rupture strength of the alloys sintered only by an intensive pulse electric current are the maximum.When the total sintering time keeps constant,the properties of the sintered alloys can be obviously improved by optimizing the sintering time of pulse-and constant-currents.A bulk ultrafine alloy with an average W grain size of about 340 nm can be obtained by sintering 15 h-milled powders in a total sintering time of 6 min.The corresponding sintered density,hardness and transverse rupture strength reach 16.78 g /cm3,HRA84.3 and 968 MPa,respectively.

Parameter optimization of microwave sintering porous Ti-23%Nb shape memory alloys for biomedical applications

Porous Ti-23%Nb(mole fraction)shape memory alloys(SMAs)were prepared successfully by microwave sintering with excellent outer finishing(without space holder).The effects of microwave-sintering on the microstructure,phase composition,phase-transformation temperature,mechanical properties and shape-memory effect were investigated.The results show that the density and size of porosity vary based on the sintering time and temperature,in which the smallest size and the most uniform pore shape are exhibited with Ti-23%Nb SMA after being sintered at 900°C for 30 min.The microstructure of porous Ti-Nb SMA consists of predominantα',α,andβphases in needle-like and plate-like morphologies,and their volume fractions vary based on the sintering time and temperature.Theβphase represents the largest phase due to the higher content ofβstabilizer element with little intensities ofαandα'phases.The highest ultimate strength and its strain are indicated for the sample sintered at 900°C for 30 min,while the best superelasticity is for the sample sintered at 1200°C for 30 min.The low-elastic modulus enables these alloys to avoid the problem of“stress shielding”.Therefore,microwave heating can be employed to sinter Ti-alloys for biomedical applications and improve the mechanical properties of these alloys.

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.

Mechanical properties of graphene nanoplatelets reinforced 7075 aluminum alloy composite fabricated by spark plasma sintering

A 0.3wt%graphene nanoplatelets(GNPs)reinforced 7075 aluminum alloy matrix(7075 Al)composite was fabricated by spark plasma sintering and its strength and wear resistance were investigated.The microstructures of the internal structure,the friction surface,and the wear debris were characterized by scanning electron microscopy,X-ray diffraction,and Raman spectroscopy.Compared with the original 7075 aluminum alloy,the hardness and elastic modulus of the 7075 Al/GNPs composite were found to have increased by 29%and 36%,respectively.The results of tribological experiments indicated that the composite also exhibited a lower wear rate than the original 7075 aluminum alloy.