A novel high-entropy alloy with multi-scale precipitates and excellent mechanical properties fabricated by spark plasma sintering

Body-centered-cubic (BCC) high entropy alloys (HEAs) usually exhibit high strength but poor ductility. To overcome such strength-ductility trade-off, a novel (FeCr)₄₅(AlNi)₅₀Co₅ HEA was presented in this paper, which was designed and fabricated with mechanical alloying (MA) followed by spark plasma sintering (SPS), and has a heterogeneous microstructure with multi-scale precipitates. Electron microscopy characterization revealed that the sizes of the precipitates range from nano (<300 nm), sub-micron (300～800 nm) to micron (>1 μm). The bulk HEA exhibits excellent mechanical properties, of which the compressive yield strength, fracture strength, and plasticity at room temperature can reach 1508 MPa, 3106 MPa and 30.4 %, respectively, which are much higher than that of most HEAs prepared by Powder Metallurgy reported in the literatures, suggesting that the HEA developed is highly promising for engineering applications. The excellent mechanical properties of the bulk HEA can be attributed to that the multi-scale precipitates are fully coherent with the matrix, which could reduce the misfit strain at the interface, and relieve the stress concentration during deformation.     

Microstructure and mechanical properties of Al-Si-Ni-Ce alloys prepared by gas-atomization spark plasma sintering and hot-extrusion

Al-Si-Ni-Ce alloys with the composition of Al_78.5Si₁₉Ni₂Ce_0.5, Al₇₆Si₁₉Ni₄Ce₁ and Al₇₃Si₁₉Ni₇Ce₁ were atomized and then sintered by using spark plasma method. The microstructure of the as-atomized powders, sintered and hot-extruded samples was analyzed. The influences of granularity and sintering parameters including time and temperature on the density of sintered alloy were also discussed. It is shown that the atomized powders are composed of Si, Al₁₁Ce₃, Al₃Ni and alpha Al. Tiny Al₃Ni particles precipitate from supersaturated matrix near the powder boundaries during SPS. Hot-extrusion process leads to the layer structure and more homogeneous distribution of precipitates. These alloys exhibit high comprehensive mechanical properties with combination of high Vicker's micro-hardness, moderate tensile properties and elongation, which provide a novel kind of promising engineering materials.     

Microstructure and mechanical properties of ultra-fine grained MoNbTaTiV refractory high-entropy alloy fabricated by spark plasma sintering

The MoNbTaTiV refractory high-entropy alloy(RHEA) with ultra-fine grains and homogeneous microstructure was successfully fabricated by mechanical alloying(MA) and spark plasma sintering(SPS).The microstructural evolutions,mechanical properties and strengthening mechanisms of the alloys were systematically investigated.The nanocrystalline mechanically alloyed powders with simple bodycentered cubic(BCC) phase were obtained after 40 h MA process.Afterward,the powders were sintered using SPS in the temperature range from 1500 ℃ to 1700 ℃.The bulk alloys were consisted of submicron scale BCC matrix and face-centered cubic(FCC) precipitation phases.The bulk alloy sintered at 1600℃ had an average grain size of 0.58 μm and an FCC precipitation phase of 0.18 μm,exhibiting outstanding micro-hardness of 542 HV,compressive yield strength of 2208 MPa,fracture strength of 3238 MPa and acceptable plastic strain of 24.9% at room temperature.The enhanced mechanical properties of the MoNbTaTiV RHEA fabricated by MA and SPS were mainly attributed to the grain boundary strengthening and the interstitial solid solution strengthening.It is expectable that the MA and SPS processes are the promising methods to synthesize ultra-fine grains and homogenous microstructural RHEA with excellent mechanical properties.     

Microstructure characteristic, mechanical properties and sintering mechanism of nanocrystalline copper obtained by SPS process

Nano-sized copper powder with an average size of 50 nm fabricated by chemical reduction method of hydrazine hydrate was consolidated using spark plasma sintering (SPS) method. The relationship between the sintering temperature and relative density of the nanocrystalline bulk copper was studied, the microstructure and the mechanical properties were examined, and the sintering mechanism was discussed. It was concluded that the nanocrystalline copper with a relative density greater than 99% and the yield strength of nearly 650 MPa could be fabricated by SPS process with the holding pressure of 600 MPa, sintering temperature of 350 °C, holding time of 5 min, and heating rate of 100 °C/min. Both refinement of the grains and formation of the extensive nanoscale twins in the NC bulk copper are the main factors to strengthen the metal.     

Synthesis of Al–Mn–Ce alloy by the spark plasma sintering

The bulk Al₉₀Mn₈Ce₂ alloy is sintered by spark plasma sintering (SPS) method. The microstructures and the hardness and wear resistance of the Al₉₀Mn₈Ce₂ samples are investigated. The results show that bulk Al₉₀Mn₈Ce₂ alloy with less than 2% porosity has been obtained at 673 K. At 723 K the Rockwell hardness of the alloy reaches 97 HRB and the wear resistance of the alloy is three times as high as that of the conventional A390 aluminum alloy. The high wear resistance of the Al₉₀Mn₈Ce₂ alloy is attributed to the existence of the large amount of the intermetallic compounds.     

Microstructure and mechanical properties of spark plasma sintered austenitic ODS steel

In this work, austenitic oxide dispersion strengthened (AODS) steel of composition Fe–16Cr–16Ni–1.5 W–0.21Ti–0.3Y₂O₃ (wt. %) was fabricated using two–stage ball milling followed by consolidation through spark plasma sintering (SPS). In the first–stage, mechanical alloying (MA) of ferritic powder and nano sized Y₂O₃ was carried out. This was followed by the addition of Ni in second–stage milling. SPS of the milled powder was carried out at 900, 950, 1000 and 1050 °C to explore the role of SPS temperature on density, microstructure as well as mechanical properties of the consolidated samples. A relative density of ～ 99% was obtained for samples sintered at 950 and 1000 °C. The as–sintered samples were subsequently solution annealed at 1075 °C for 2 h and water quenched. X–ray diffraction studies confirmed the presence of austenite in the consolidated and solution annealed samples. Electron back scatter diffraction analysis of solution annealed samples sintered at all the temperatures revealed a bimodal microstructure. The average grain size of 1.07 ± 0.72 µm was obtained for solution annealed samples sintered at 1000 °C. Yield strength and elongation of the same was measured as 851 MPa and 18%, respectively at room temperature. These values are the best combination of strength to elongation achieved on AODS alloys processed using MA and SPS, which makes this AODS steel much promising for high temperature applications.     

Fabrication of W-Cu functionally graded composites using high energy ball milling and spark plasma sintering for plasma facing components

W-Cu functionally graded composites (FGCs) up to six layers have been developed using high energy ball milling and spark plasma sintering (SPS) at a lower temperature of 900 °C. The relative density of W-Cu composites increased from 85.4% (W₈₀Cu₂₀ layer) to 95.7% (W₂₀Cu₈₀ layer) with increasing Cu content. All the W-Cu FGCs exhibited a graded structure even after SPS and showed a gradual change in hardness, Young’s modulus, and coefficient of thermal expansion (CTE). Furthermore, W-Cu composites showed a CTE and modulus between those of W and Cu and could be used as an intermediate layer between W and Cu in plasma facing components. The thermal cycle testing at 800 °C has confirmed that the W-Cu FGCs developed in this study can withstand thermal shock and showed a superior performance over directly bonded W-Cu sample. The W-Cu FGCs developed in the present study are not only suitable for plasma facing components but can also be used where the thermal stresses are introduced due to the large mismatch in CTE or elastic modulus.     

Microstructure and mechanical properties of in situ TiB reinforced titanium matrix composites based on Ti–FeMo–B prepared by spark plasma sintering

The in situ synthesized TiB reinforced titanium matrix composites have been prepared by spark plasma sintering at 800–1200 °C under 20 MPa for 5 min. The effects of sintering temperature and reinforcement volume fraction on flexural strength, Young’s modulus and fracture toughness of the composites are investigated. The titanium matrix consists of -Ti and β-Ti phases, and the volume fraction of β-Ti increases with increasing sintering temperatures. The in situ synthesized TiB reinforcements are distributed randomly and uniformly in matrix. The transverse section of TiB has a hexagonal shape aligned along [0 1 0] direction, and the crystallographic planes of the TiB needles are always of the type . The 10 vol% TiB reinforced composite sintered at 1000 °C exhibits excellent mechanical properties. The flexural strength, Young’s modulus and fracture toughness of this composite are 1560 MPa, 137 GPa and 8.64 MPa · m^1/2, respectively.     

SPS制备TiNi增强镁合金复合材料的微观结构及力学性能

以AZ31镁合金为基体,TiNi形状记忆合金丝为增强体,利用放电等离子烧结法（SPS）制备了TiNi/Mg复合材料,用OM、SEM、EDS对其微观形貌进行表征,并用XRD及DSC研究TiNi丝的相变,同时对该复合材料进行准静态拉伸实验,对其室温及高温力学性能进行研究。结果表明,所制备的TiNi/Mg复合材料中界面处存在Mg、Ti、Ni元素的互扩散现象,并形成宽度约为2 μm的互扩散层;所制备的TiNi/Mg复合材料的高温力学性能高于室温,其中其屈服强度、抗拉强度及弹性模量在100℃时（分别为157 MPa,292 MPa,22 GPa）较室温分别提高了12%、33%和29%,150℃时（分别为143 MPa,251 MPa,20 GPa）较室温分别提高了2%、14%和18%。     

Microstructural and mechanical characterisation of ODS ferritic alloys produced by mechanical alloying and spark plasma sintering

Abstract

Powders with nominal composition Fe–14Cr–2W–0·4Ti were mechanically alloyed (MA) with Y₂O₃ in a planetary ball mill at two different rotational speeds. Consolidation of the as milled powders was performed by spark plasma sintering (SPS). As milled powders showed a highly deformed microstructure with elongated nanometre grains and, depending upon the rotational speed, different stages of the nanocluster evolution were observed to be produced. In the case of consolidated materials, grain growth occurred during the SPS process and it was possible to observe the influence of the MA parameters, with larger and more homogeneously distributed grains at the higher rotational speed. Additionally, Ti was observed to be incorporated to the nanoclusters after SPS, indicating a further step in their evolution during consolidation. The mechanical behaviour of the SPS compacts was evaluated by tensile and small punch testing also showing the influence of the MA parameters in the material behaviour.     

The dynamic properties of SiCp/Al composites fabricated by spark plasma sintering with powders prepared by mechanical alloying process

The dynamic compressive properties of SiC particle reinforced pure Al matrix composites, fabricated by spark plasma sintering technique with mixture powders prepared by mechanical alloying process, were tested in this paper. Two different average SiC particle sizes of 12 μm and 45 μm were adopted, and the compressive tests of these composites at strain rates ranging from 800/s to 5200/s were conducted by split Hopkinson pressure bar. The damage mechanism of the SiC_p/Al composites was analyzed through the microstructural observations and high-precision density measurements. Results show that the dynamic properties and damage accumulation of these composites are significantly affected by the particle distribution, size, particle cracking, particle/matrix interface debonding and adiabatic heat softening. The composites containing smaller SiC particles exhibit higher flow stress, lower strain rate sensitivity, and less damage at high strain rate deformation.     

Effect of sintering temperature on microstructures and mechanical properties of spark plasma sintered nanocrystalline aluminum

Organic-coated aluminum nano-powders were consolidated by spark plasma sintering technique with low initial pressure of 1 MPa and high holding pressure of 300 MPa at different sintering temperature. The effect of sintering temperature on microstructures and mechanical properties of the compact bulks was investigated. The results indicate that both the density and the strain of the nanocrystalline aluminum increase with an increase in sintering temperature. However, the micro-hardness, compressive strength and tensile stress of the compact bulks increase initially and then decrease with increasing sintering temperature. The nanocrystalline aluminum sintered at 773 K has the highest micro-hardness of 3.06 GPa, the best compressive strength of 665 MPa and the supreme tensile stress of 282 MPa. A rapid grain growth of nanocrystalline aluminum sintered at 823 K leads to a decrease in micro-hardness, compressive strength and tensile stress. After annealing, a remarkable increase in strain and a slight rise in strength were obtained due to the relief of the residual stress in nanocrystalline Al and the formation of composite structure.     

Densification and alloying of ball milled Silicon-Germanium powder mixture during spark plasma sintering

In this research, the influence of process parameters such as sintering temperature and current during alloying and densification of silicon-germanium (Si₈₀-Ge₂₀) powder mixture using spark plasma sintering (SPS) was reported. Si₈₀-Ge₂₀ powder mixture was consolidated at the temperature range 900–1200 °C with 40 MPa pressure for 5 min. soaking. X-ray diffraction (XRD) study was made on sintered compacts to confirm the Si(Ge) alloy formation. Scanning electron microscope (SEM) was used to understand the morphology, particle size and distribution of un-milled and milled Si₈₀-Ge₂₀ powder mixture. Transmission electron microscope (TEM) study was made on milled Si₈₀-Ge₂₀ powder mixture and bulk SiGe alloy to confirm the nano-crystallinity and alloy formation. Fracture toughness of sintered bulk SiGe alloy was determined from Palmqvist cracks geometry model using Vickers hardness testing. It is understood that, during spark plasma sintering nano-structured Si₈₀-Ge₂₀ powder simultaneously increases the densification and reaction kinetics. It helps to achieve homogenous nanostructured SiGe alloy of near theoretical density. The superior hardness and benchmarked fracture toughness (K_IC) values of 630 VHN and 2.19 MPa√m was achieved for SiGe alloy sintered at 1200 °C, respectively.     

Fabrication of a biodegradable Fe-Mn-Si alloy by field assisted sintering

Biodegradable metals are emerging as novel implant materials by overcoming the drawbacks of the existing materials used commercially. This work investigates the suitability of Fe-35Mn-5Si as a biodegradable implant by examining its mechanical and corrosion behavior. The processing involves High Energy Ball Milling (HEBM) followed by Spark Plasma Sintering (SPS) and heat treatment at optimized conditions to develop a single-phase austenitic alloy. The heat-treated (HT) samples exhibited low magnetic susceptibility of 3.47x10⁻⁷ due to the austenitic phase formation. Yield strength of 500 MPa, UTS of 712 MPa, Young’s modulus of 110 GPa, and hardness of 380 HV along with 9.5% elongation was obtained in the optimized samples, which are comparable to Ti alloy and 316L stainless steel metallic implants. The corrosion tests yielded degradation rates of 0.025 mm/year for the alloy in standard Hank’s solution. This alloy could pave the way for the fabrication of low-cost biodegradable implants using the simple powder metallurgy route.     

Microstructure and mechanical properties of CNT/Ag nanocomposites fabricated by spark plasma sintering

Carbon nanotube/silver (CNT/Ag) nanocomposites include CNT volume fraction up to 10?vol.% were prepared by chemical reduction in solution followed by spark plasma sintering. Multiwalled CNTs underwent surface modifications by acid treatments, the Fourier transform infrared spectroscopy data indicated several functional groups loaded on the CNT surface by acid functionalisation. The acid-treated CNTs were sensitised and activated. Silver was deposited on the surface of the activated CNTs by chemical reduction of alkaline silver nitrate solution at room temperature. The microstructures of the prepared CNT/Ag nanocomposite powders were investigated by high-resolution scanning electron microscopy (HRSEM), transmission electron microscopy and X-ray powder diffraction analysis. The results indicated that the produced CNT/Ag nanocomposite powders have coated type morphology. The produced CNT/Ag nanocomposite powders were sintered by spark plasma sintering. It was observed from the microstructure investigations of the sintered materials by HRSEM that the CNTs were distributed in the silver matrix with good homogeneity. The hardness and the tensile properties of the produced CNT/Ag nanocomposites were measured. By increasing the volume fraction of CNTs in the silver matrix, the hardness values increased but the elongation values of the prepared CNT/Ag nanocomposites decreased. In addition, the tensile strength was increased by increasing the CNTs volume fraction up to 7.5?vol.%, but the sample composed of 10?vol.% CNT/Ag was fractured before yielding.     

Synthesis of ultra high strength Al–Mg–Si alloy sheets by differential speed rolling

The ultrafine-grained Al–Mg–Si alloy sheets, which were fabricated by severe plastic deformation (SPD) using a high-speed-ratio differential speed rolling (HRDSR) and subsequent low temperature aging, exhibited an ultra high strength (yield stress: 455 MPa, ultimate tensile strength: 489 MPa). The strengthening effect was impressive compared with the results obtained by using other SPD techniques. The achievement could be attributed to formation of very fine grains due to significantly increased dislocation density in solute supersaturated matrix, high Hall-Petch constant and particle strengthening gained by formation nano-scale precipitates during the low temperature aging after the HRDSR process.     

Rapid synthesis of Ti alloy with B addition by spark plasma sintering

The in situ TiB/Ti–4.0Fe–7.3Mo composites were fabricated by plasma spark sintering (SPS) technique using mechanical alloying of Ti, Fe65Mo and B powder. The effects of sintering temperature on densification of the composites and microstructure of the in situ synthesized TiB were investigated using scanning electron microscope (SEM) and transmission electron microscope (TEM). A dense composite was obtained after sintering at 1000 °C for 5 min. Under proper ball milling and SPS conditions in situ TiB reinforced Ti–4.0Fe–7.3Mo composites have been prepared. The in situ TiB showed a typical needle shape grow along [0 1 0] direction. The transverse cross-section of TiB grain is a hexagonal shape with the planes of (1 0 0), (1 0 1) and . The stacking faults in the (1 0 0) plane were observed in the TiB needles.     

Microstructure and mechanical properties of an ultrafine grained Ti5Si3-TiC composite fabricated by spark plasma sintering

The purpose of this study was to investigate mechanical properties, microstructure and sintering behavior of ultrafine grained Ti₅Si₃-TiC composite synthesized by mechanically activated self-propagating high-temperature synthesis method. For this purpose, the composite was sintered at 1450?°C at constant pressure of 50?MPa and reached to 97% of theoretical density by spark plasma sintering technique. The XRD pattern of the sintered sample is composed of the same peaks as the synthesized sample which means that the composite is stable at high temperature. The microstructure analyses illustrate that the composite retained its fine microstructure during the sintering process. The results also show that the amount of C atoms in the structure of titanium silicide slightly increased during the sintering process. The Young’s modulus and nanohardness of the composite reached 281?±?15.5?GPa and 16.6?±?0.8?GPa, respectively. In addition, Vickers indentation test results show that the composite possesses hardness and fracture toughness of 13.2?±?0.6?GPa and 4.7?±?0.1?MPa.m^1/2, respectively. Formation of microstructure with low microcracks and homogenous distribution of TiC through the matrix are responsible for relative high mechanical properties of the composite. The crack deflection is observed as the main toughening mechanism.     

Microstructure and thermal conductivity of spark plasma sintering AlN ceramics

Abstract

Dense aluminium nitride ceramics were prepared by spark plasma sintering at a lower sintering temperature of 1700°C with Y₂O₃, Sm₂O₃ and Dy₂O₃ as sintering additives respectively. The effects of three kinds of sintering additives on the phase composition, microstructure and thermal conductivity of AlN ceramics were investigated. The results showed that those sintering additives not only facilitated the densification via the liquid phase sintering mechanism, but also improved thermal conductivity by decreasing oxygen impurity. Sm₂O₃ could effectively improve thermal conductivity of AlN ceramics compared with Y₂O₃ and Dy₂O₃. Observation by scanning electron microscopy showed that AlN ceramics prepared by spark plasma sintering method manifested quite homogeneous microstructures, but AlN grain sizes and shapes and location of secondary phases varied with the sintering additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of secondary phases.     

Excellent mechanical properties and large magnetocaloric effect of spark plasma sintered Ni-Mn-In-Co alloy

The Ni43.75Mn37.5In12.5Co6.25 alloy was obtained by using the spark plasma sintering (SPS) technique.The martensitic transformation,magnetic and mechanical properties of the SPS alloy were investigated.Key findings demonstrate that the martensitic transformation temperature of this alloy is about 10 K lower than that of the as-cast one.Both SPS and as-cast alloys show a 7 layered modulated martensite (7M) at room temperature.The compressive fracture strength and strain of the SPS alloy increase by 176.92％ and 33.33％ compared with the as-cast alloy,achieving 1440 MPa and 14％,respectively.The maximum magnetic entropy change △Sm is 17.1 J kg-1 K-1 for the SPS alloy at the magnetic field of 5 T.