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In this study, Ni-Y2O3 powder was prepared by alloying recomposition oxidation sintering (AROS), solution combustion synthesis (SCS), and conventional mechanical alloying (MA). The microstructure and mechanical properties of the alloys were investigated by spark plasma sintering (SPS). Among the Ni-Y2O3 powders synthesized by the three methods, the AROS powder had approximately 5 nm of Y2O3 crystals uniformly distributed within the Ni particles, whereas the SCS powder contained a mixture of Ni and Y2O3 nanoparticles, and the MA powder formed small Y2O3 crystals on the surface of large Ni particles by milling the mixture of Ni and Y2O3. The average grain size of Y2O3 in the sintered alloys was approximately 15 nm, with the AROS sinter having the smallest, followed by the SCS sinter at 18 nm, and the MA sinter at 22 nm. The yield strength (YS) of the SCS- and MA-sintered alloys were 1511 and 1688 MPa, respectively, which are lower than the YS value of 1697 MPa for the AROS-sintered alloys. The AROS alloy exhibited improved strength compared to the alloys fabricated by SCS and conventional MA methods, primarily because of the increased strengthening from the finer Y2O3 particles and Ni grains.
The effects of annealing on the microstructure and mechanical properties of Al–Zn–Mg–Cu–Si alloys fabricated by high-energy ball milling (HEBM) and spark plasma sintering (SPS) were investigated. The HEBM-free sintered alloy primarily contained Mg2Si, Q-AlCuMgSi, and Si phases. Meanwhile, the HEBM-sintered alloy contains Mg-free Si and θ-Al2Cu phases due to the formation of MgO, which causes Mg depletion in the Al matrix. Annealing without and with HEBM at 500°C causes partial dissolution and coarsening of the Q-AlCuMgSi and Mg2Si phases in the alloy and dissolution of the θ-Al2Cu phase in the alloy, respectively. In both alloys, a thermally stable α-AlFeSi phase was formed after long-term heat treatment. The grain size of the sintered alloys with and without HEBM increased from 0.5 to 1.0 μm and from 2.9 to 6.3 μm, respectively. The hardness of the sintered alloy increases after annealing for 1 h but decreases significantly after 24 h of annealing. Extending the annealing time to 168 h improved the hardness of the alloy without HEBM but had little effect on the alloy with HEBM. The relationship between the microstructural factors and the hardness of the sintered and annealed alloys is discussed.
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Molybdenum-tungsten (Mo-W) alloy sputtering targets are widely utilized in fields like electronics, nanotechnology, sensors, and as gate electrodes for TFT-LCDs, owing to their superior properties such as hightemperature stability, low thermal expansion coefficient, electrical conductivity, and corrosion resistance. To achieve optimal performance in application, these targets’ purity, relative density, and grain size of these targets must be carefully controlled. We utilized nanopowders, prepared via the Pechini method, to obtain uniform and fine powders, then carried out spark plasma sintering (SPS) to densify these powders. Our studies revealed that the sintered compacts made from these nanopowders exhibited outstanding features, such as a high relative density of more than 99%, consistent grain size of 3.43 μm, and shape, absence of preferred orientation.
Metal-additive manufacturing techniques, such as selective laser sintering (SLS), are increasingly utilized for new biomaterials, such as cobalt-chrome (Co-Cr). In this study, Co-Cr gas-atomized powders are used as charge materials for the SLS process. The aim is to understand the consolidation of Co-Cr alloy powder and characterization of samples sintered using SLS under various conditions. The results clearly suggest that besides the matrix phase, the second phase, which is attributed to pores and oxidation particles, is observed in the sintered specimens. The as-built samples exhibit completely different microstructural features compared with the casting or wrought products reported in the literature. The microstructure reveals melt pools, which represent the characteristics of the scanning direction, in particular, or of the SLS conditions, in general. It also exposes extremely fine grain sizes inside the melt pools, resulting in an enhancement in the hardness of the as-built products. Thus, the hardness values of the samples prepared by SLS under all parameter conditions used in this study are evidently higher than those of the casting products.
In this study, an Al82Ni7Co3Y8 (at%) bulk metallic glass is fabricated using gas-atomized Al82Ni7Co3Y8 metallic glass powder and subsequent spark plasma sintering (SPS). The effect of powder size on the consolidation of bulk metallic glass is considered by dividing it into 5 μm or less and 20–45 μm. The sintered Al82Ni7Co3Y8 bulk metallic glasses exhibit crystallization behavior and crystallization enthalpy similar to those of the Al82Ni7Co3Y8 powder with 5 μm or less and it is confirmed that no crystallization occurred during the sintering process. From these results, we conclude that the Z-position-controlled spark plasma sintering process, using superplastic deformation by viscous flow in the supercooled liquid-phase region of amorphous powder, is an effective process for manufacturing bulk metallic glass.
We investigate the austenite stability in nanocrystalline Fe-7%Mn-X%Mo (X = 0, 1, and 2) alloys fabricated by spark plasma sintering. Mo is known as a ferrite stabilizing element, whereas Mn is an austenite stabilizing element, and many studies have focused on the effect of Mn addition on austenite stability. Herein, the volume fraction of austenite in nanocrystalline Fe-7%Mn alloys with different Mo contents is measured using X-ray diffraction. Using a disk compressive test, austenite in Fe–Mn–Mo alloys is confirmed to transform into strain-induced martensite during plastic deformation by a disk d. The variation in austenite stability in response to the addition of Mo is quantitatively evaluated by comparing the k-parameters of the kinetic equation for the strain-induced martensite transformation.
Yttria-stabilized zirconia (YSZ) has a low thermal conductivity, high thermal expansion coefficient, and excellent mechanical properties; thus, it is used as a thermal barrier coating material for gas turbines. However, during long-time exposure of YSZ to temperatures of 1200°C or higher, a phase transformation accompanied by a volume change occurs, causing the YSZ coating layer to peel off. To solve this problem, YSZ has been doped with trivalent and tetravalent oxides to obtain coating materials with low thermal conductivity and suppressed phase transformation of zirconia. In this study, YSZ is doped with trivalent oxides, Nd2O3, Yb2O3, Al2O3, and tetravalent oxide, TiO2, and the thermal conductivity of the obtained materials is analyzed according to the composition; furthermore, the relative density change, microstructure change, and m-phase formation behavior are analyzed during long-time heat treatment at high temperatures.
3Y-TZP ceramics obtained by doping 3 mol.% of Y2O3 to ZrO2 to stabilize the phase transition are widely used in the engineering ceramic industry due to their excellent mechanical properties such as high strength, fracture toughness, and wear resistance. An additional increase in mechanical properties is possible by manufacturing a composite in which a high-hardness material such as oxide or carbide is added to the 3Y-TZP matrix. In this study, composite powder was prepared by dispersing a designated percentage of WC in the 3Y-TZP matrix, and the results were compared after manufacturing the composite using the different processes of spark plasma sintering and HP. The difference between the densification behavior and porosity with the process mechanism was investigated. The correlation between the process conditions and phase formation was examined based on the crystalline phase formation behavior. Changes to the microstructure according to the process conditions were compared using field-emission scanning electron microscopy. The toughness-strengthening mechanism of the composite with densification and phase formation was also investigated.
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Changes in the mechanical properties and microstructure of an IN 939 W alloy according to the sintering heating rate were evaluated. IN 939 W alloy samples were fabricated by spark plasma sintering. The phase fraction, number density, and mean radius of the IN 939W alloy were calculated using a thermodynamic calculation. A universal testing machine and micro-Vickers hardness tester were employed to confirm the mechanical properties of the IN 939W alloy. X-ray diffraction, optical microscopy, field-emission scanning electron microscopy, Cs-corrected-field emission transmission electron microscopy, and energy dispersive X-ray spectrometry were used to evaluate the microstructure of the alloy. The rapid sintering heating rate resulted in a slightly dispersed γ' phase and chromium oxide. It also suppressed the precipitation of the η phase. These helped to reinforce the mechanical properties.
A typical trade-off relationship exists between strength and elongation in face-centered cubic metals. Studies have recently been conducted to enhance strength without ductility reduction through surface-treatment-based ultrasonic nanocrystalline surface modification (UNSM), which creates a gradient microstructure in which grains become smaller from the inside to the surface. The transformation-induced plasticity effect in Fe-Mn alloys results in excellent strength and ductility due to their high work-hardening rate. This rate is achieved through strain-induced martensitic transformation when an alloy is plastically deformed. In this study, Fe-6%Mn powders with different sizes were prepared by high-energy ball milling and sintered through spark plasma sintering to produce Fe-6%Mn samples. A gradient microstructure was obtained by stacking the different-sized powders to achieve similar effects as those derived from UNSM. A compressive test was performed to investigate the mechanical properties, including the yielding behavior. The deformed microstructure was observed through electron backscatter diffraction to determine the effects of gradient plastic deformation.
The low-temperature sinterability of TiO2-CuO systems was investigated using a solid solution of SnO2. Sample powders were prepared through conventional ball milling of mixed raw powders. With the SnO2 content, the compositions of the samples were Ti1-xSnxO2-CuO(2 wt.%) in the range of x ≤ 0.08. Compared with the samples without SnO2 addition, the densification was enhanced when the samples were sintered at 900°C. The dominant mass transport mechanism seemed to be grain-boundary diffusion during heat treatment at 900°C, where active grain-boundary diffusion was responsible for the improved densification. The rapid grain growth featured by activated sintering was also obstructed with the addition of SnO2. This suggested that both CuO as an activator and SnO2 dopant synergistically reduced the sintering temperature of TiO2.
An alternative fabrication method for carburizing steel using spark plasma sintering (SPS) is investigated. The sintered carburized sample, which exhibits surface modification effects such as carburizing, sintered Fe, and sintered Fe–0.8 wt.%C alloys, is fabricated using SPS. X-ray diffraction and micro Vickers tests are employed to confirm the phase and properties. Finite element analysis is performed to evaluate the change in hardness and analyze the carbon content and residual stress of the carburized sample. The change in the hardness of the carburized sample has the same tendency to predict hardness. The difference in hardness between the carburized sample and the predicted value is also discussed. The carburized sample exhibits a compressive residual stress at the surface. These results indicate that the carburized sample experiences a surface modification effect without carburization. Field emission scanning electron microscopy is employed to verify the change in phase. A novel fabrication method for altering the carburization is successfully proposed. We expect this fabrication method to solve the problems associated with carburization.
In this study, we report the microstructure and characteristics of Ag-SnO2-Bi2O3 contact materials using a controlled milling process with a subsequent compaction process. Using magnetic pulsed compaction (MPC), the milled Ag-SnO2-Bi2O3 powders have been consolidated into bulk samples. The effects of the compaction conditions on the microstructure and characteristics have been investigated in detail. The nanoscale SnO2 phase and microscale Bi2O3 phase are well-distributed homogeneously in the Ag matrix after the consolidation process. The successful consolidation of Ag-SnO2-Bi2O3 contact materials was achieved by an MPC process with subsequent atmospheric sintering, after which the hardness and electrical conductivity of the Ag-SnO2-Bi2O3 contact materials were found to be 62–75 HV and 52–63% IACS, respectively, which is related to the interfacial stability between the Ag matrix, the SnO2 phase, and the Bi2O3 phase.
In this study, a nanocrystalline FeNiCrMoMnSiC alloy was fabricated, and its austenite stability, microstructure, and mechanical properties were investigated. A sintered FeNiCrMoMnSiC alloy sample with nanosized crystal was obtained by high-energy ball milling and spark plasma sintering. The sintering behavior was investigated by measuring the displacement according to the temperature of the sintered body. Through microstructural analysis, it was confirmed that a compact sintered body with few pores was produced, and cementite was formed. The stability of the austenite phase in the sintered samples was evaluated by X-ray diffraction analysis and electron backscatter diffraction. Results revealed a measured value of 51.6% and that the alloy had seven times more austenite stability than AISI 4340 wrought steel. The hardness of the sintered alloy was 60.4 HRC, which was up to 2.4 times higher than that of wrought steel.
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The effect of sintering conditions on the austenite stability and strain-induced martensitic transformation of nanocrystalline FeCrC alloy is investigated. Nanocrystalline FeCrC alloys are successfully fabricated by spark plasma sintering with an extremely short densification time to obtain the theoretical density value and prevent grain growth. The nanocrystallite size in the sintered alloys contributes to increased austenite stability. The phase fraction of the FeCrC sintered alloy before and after deformation according to the sintering holding time is measured using X-ray diffraction and electron backscatter diffraction analysis. During compressive deformation, the volume fraction of strain-induced martensite resulting from austenite decomposition is increased. The transformation kinetics of the strain-induced martensite is evaluated using an empirical equation considering the austenite stability factor. The hardness of the S0W and S10W samples increase to 62.4-67.5 and 58.9-63.4 HRC before and after deformation. The hardness results confirmed that the mechanical properties are improved owing to the effects of grain refinement and strain-induced martensitic transformation in the nanocrystalline FeCrC alloy.
We fabricate the non-equiatomic high-entropy alloy (NE-HEA) Fe49.5Mn30Co10Cr10C0.5 (at.%) using spark plasma sintering under various sintering conditions. Each elemental pure powder is milled by high-energy ball milling to prepare NE-HEA powder. The microstructure and mechanical properties of the sintered samples are investigated using various methods. We use the X-ray diffraction (XRD) method to investigate the microstructural characteristics. Quantitative phase analysis is performed by direct comparison of the XRD results. A tensile test is used to compare the mechanical properties of small samples. Next, electron backscatter diffraction analysis is performed to analyze the phase fraction, and the results are compared to those of XRD analysis. By combining different sintering durations and temperature conditions, we attempt to identify suitable spark plasma sintering conditions that yield mechanical properties comparable with previously reported values. The samples sintered at 900 and 1000°C with no holding time have a tensile strength of over 1000 MPa.
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High-entropy alloys have excellent mechanical properties under extreme environments, rendering them promising candidates for next-generation structural materials. It is desirable to develop non-equiatomic high-entropy alloys that do not require many expensive or heavy elements, contrary to the requirements of typical high-entropy alloys. In this study, a non-equiatomic high-entropy alloy powder Fe49.5Mn30Co10Cr10C0.5 (at.%) is prepared by high energy ball milling and fabricated by spark plasma sintering. By combining different ball milling times and ball-topowder ratios, we attempt to find a proper mechanical alloying condition to achieve improved mechanical properties. The milled powder and sintered specimens are examined using X-ray diffraction to investigate the progress of mechanical alloying and microstructural changes. A miniature tensile specimen after sintering is used to investigate the mechanical properties. Furthermore, quantitative analysis of the microstructure is performed using electron backscatter diffraction.
The purpose of this study is to investigate the densification behavior and the corresponding microstructural evolution of tantalum and tantalum-tungsten alloy powders for explosively formed liners. The inherent inhomogeneous microstructures of tantalum manufactured by an ingot metallurgy might degrade the capability of the warhead. Therefore, to overcome such drawbacks, powder metallurgy was incorporated into the near-net shape process in this study. Spark plasma-sintered tantalum and its alloys with finer particle sizes exhibited higher densities and lower grain sizes. However, they were contaminated from the graphite mold during sintering. Higher compaction pressures in die and isostatic compaction techniques also enhanced the sinterability of the tantalum powders; however, a full densification could not be achieved. On the other hand, the powders exhibited full densification after being subjected to hot isostatic pressing over two times. Consequently, it was found that the hot isostatic-pressed tantalum might exhibit a lower grain size and a higher density as compared to those obtained in previous studies.
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Predicting the quality of materials after they are subjected to plasma sintering is a challenging task because of the non-linear relationships between the process variables and mechanical properties. Furthermore, the variables governing the sintering process affect the microstructure and the mechanical properties of the final product. Therefore, an artificial neural network modeling was carried out to correlate the parameters of the spark plasma sintering process with the densification and hardness values of Ti-6Al-4V alloys dispersed with nano-sized TiN particles. The relative density (%), effective density (g/cm3), and hardness (HV) were estimated as functions of sintering temperature (°C), time (min), and composition (change in % TiN). A total of 20 datasets were collected from the open literature to develop the model. The high-level accuracy in model predictions (>80%) discloses the complex relationships among the sintering process variables, product quality, and mechanical performance. Further, the effect of sintering temperature, time, and TiN percentage on the density and hardness values were quantitatively estimated with the help of the developed model.
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W2C is synthesized through a reaction-sintering process from an ultrafine-W and WC powder mixture using spark plasma sintering (SPS). The effect of various parameters, such as W:WC molar ratio, sintering temperature, and sintering time, on the synthesis behavior of W2C is investigated through X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) analysis of the microstructure, and final sintered density. Further, the etching properties of a W2C specimen are analyzed. A W2C sintered specimen with a particle size of 2.0 μm and a relative density over 98% could be obtained from a W-WC powder mixture with 55 mol%, after SPS at 1700°C for 20 min under a pressure of 50 MPa. The sample etching rate is similar to that of SiC. Based on X-ray photoelectron spectroscopy (XPS) analysis, it is confirmed that fluorocarbon-based layers such as C-F and C-F2 with lower etch rates are also formed.
The grain growth behavior of M-type Sr hexaferrite (SrM) grains is investigated with the addition of MnCO3. First, the SrM powder is synthesized by a conventional solid-state reaction. The powder compacts of SrM are sintered at 1250°C for 2 h with various amounts of MnCO3 (0, 0.5, 1.0, and 4.0 mol%). There is no secondary solid phase in any of the sintered samples. Relative density increases when MnCO3 is added to the SrM. Obvious abnormal grain growth does not appear in any of the SrM samples with MnCO3. The average grain size increases when 0.5 mol% MnCO3 is added to the SrM. However, as the amount of MnCO3 increase to over 0.5 mol%, the average grain size decreases. These observations allow us to conclude that the growth of SrM grains is governed by the two-dimensional nucleation grain growth mechanism, and the critical driving force for the growth of a grain decreases as the amount of MnCO3 increases.
In this study, we report the microstructure and characterization of Ta20Nb20V20W20Ti20 high-entropy alloy powders and sintered samples. The effects of milling time on the microstructure and mechanical properties were investigated in detail. Microstructure and structural characterization were performed by scanning electron microscopy and X-ray diffraction. The mechanical properties of the sintered samples were analyzed through a compressive test at room temperature with a strain rate of 1 × 10−4 s−1. The microstructure of sintered Ta20Nb20V20W20Ti20 high-entropy alloy is composed of a BCC phase and a TiO phase. A better combination of compressive strength and strain was achieved by using prealloyed Ta20Nb20V20W20Ti20 powder with low oxygen content. The results suggest that the oxide formed during the sintering process affects the mechanical properties of Ta20Nb20V20W20Ti20 high-entropy alloys, which are related to the interfacial stability between the BCC matrix and TiO phase.
Phosphorus is an element that plays many important roles in powder metallurgy as an alloy element. The purpose of this study is to investigate the influence of phosphorus addition on the microstructures and mechanical properties of sintered low-alloy steel. The sintered low-alloy steels Fe-0.6%C-3.89%Ni-1.95%Cu-1.40%Mo-xP (x=0, 0.05, 0.10, 0.15, 0.20%) were manufactured by compacting at 700 MPa, sintering in H2-N2 at 1260 °C, rapid cooling, and low-temperature tempering in Ar at 160 °C. The microstructure, pore, density, hardness, and transverse rupture strength (TRS) of the sintered low-alloy steels were evaluated. The hardness increased as the phosphorus content increased, whereas the density and TRS showed maximum values when the content of P was 0.05%. Based on microstructure observation, the phase of the microstructure changed from bainite to martensite as the content of phosphorus is increased. Hence, the most appropriate addition of phosphorus in this study was 0.05%.
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Recently, the amount of heat generated in devices has been increasing due to the miniaturization and high performance of electronic devices. Cu-graphite composites are emerging as a heat sink material, but its capability is limited due to the weak interface bonding between the two materials. To overcome these problems, Cu nanoparticles were deposited on a graphite flake surface by electroless plating to increase the interfacial bonds between Cu and graphite, and then composite materials were consolidated by spark plasma sintering. The Cu content was varied from 20 wt.% to 60 wt.% to investigate the effect of the graphite fraction and microstructure on thermal conductivity of the Cu-graphite composites. The highest thermal conductivity of 692 W m−1K−1 was achieved for the composite with 40 wt.% Cu. The measured coefficients of thermal expansion of the composites ranged from 5.36 × 10−6 to 3.06 × 10−6 K−1. We anticipate that the Cu-graphite composites have remarkable potential for heat dissipation applications in energy storage and electronics owing to their high thermal conductivity and low thermal expansion coefficient.
Piezoelectric ceramic specimens with the Pb(Mg1/3Nb2/3)0.65Ti0.35O3 (PMN-PT) composition are prepared by the solid state reaction method known as the “columbite precursor” method. Moreover, the effects of the Li2O-Bi2O3 additive on the microstructure, crystal structure, and piezoelectric properties of sintered PMN-PT ceramic samples are investigated. The addition of Li2O-Bi2O3 lowers the sintering temperature from 1,200°C to 950°C. Moreover, with the addition of >5 wt.% additive, the crystal structure changes from tetragonal to rhombohedral. Notably, the sample with 3 wt.% additive exhibits excellent piezoelectric properties (d33 = 596 pC/N and Kp = 57%) and a sintered density of 7.92 g/cm3 after sintering at 950°C. In addition, the sample exhibits a curie temperature of 138.6°C at 1 kHz. Finally, the compatibility of the sample with a Cu electrode is examined, because the energy-dispersive X-ray spectroscopy data indicate the absence of interdiffusion between Cu and the ceramic material.
Aluminum nitride (AlN) has excellent electrical insulation property, high thermal conductivity, and a low thermal expansion coefficient; therefore, it is widely used as a heat sink, heat-conductive filler, and heat dissipation substrate. However, it is well known that the AlN-based materials have disadvantages such as low sinterability and poor mechanical properties. In this study, the effects of addition of various amounts (1-6 wt.%) of sintering additives Y2O3 and Sm2O3 on the thermal and mechanical properties of AlN samples pressureless sintered at 1850°C in an N2 atmosphere for a holding time of 2 h are examined. All AlN samples exhibit relative densities of more than 97%. It showed that the higher thermal conductivity as the Y2O3 content increased than the Sm2O3 additive, whereas all AlN samples exhibited higher mechanical properties as Sm2O3 content increased. The formation of secondary phases by reaction of Y2O3, Sm2O3 with oxygen from AlN lattice influenced the thermal and mechanical properties of AlN samples due to the reaction of the oxygen contents in AlN lattice.
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In the present study, we have investigated the effect of sintering process conditions on the stability of the austenite phase in the nanocrystalline Fe-5wt.%Mn-0.2wt.%C alloy. The stability and volume fraction of the austenite phase are the key factors that determine the mechanical properties of FeMnC alloys, because strain-induced austenitemartensite transformation occurs under the application of an external stress at room temperature. Nanocrystalline Fe-5wt.%Mn-0.2wt.%C samples are fabricated using the spark plasma sintering method. The stability of the austenite phase in the sintered samples is evaluated by X-ray diffraction analysis and hardness test. The volume fraction of austenite at room temperature increases as the sample is held for 10 min at the sintering temperature, because of carbon diffusion in austenite. Moreover, water quenching effectively prevents the formation of cementite during cooling, resulting in a higher volume fraction of austenite. Furthermore, it is found that the hardness is influenced by both the austenite carbon content and volume fraction.
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The objective of this study is to investigate the influence of powder shape and densification mechanism on the microstructure and mechanical properties of Ti-6Al-4V components. BE powders are uniaxially and isostatically pressed, and PA ones are injection molded because of their high strengths. The isostatically compacted samples exhibit a density of 80%, which is higher than those of other samples, because hydrostatic compression can lead to higher strain hardening. Owing to the higher green density, the density of BE-CS (97%) is found to be as high as that of other samples (BE-DS (95%) and P-S (94%)). Furthermore, we have found that BE powders can be consolidated by sintering densification and chemical homogenization, whereas PA ones can be consolidated only by simple densification. After sintering, BE-CS and P-S are hot isostatically pressed and BE-DS is hot forged to remove residual pores in the sintered samples. Apparent microstructural evolution is not observed in BE-CSH and P-SH. Moreover, BE-DSF exhibits significantly fine grains and high density of low-angle grain boundaries. Thus, these microstructures provide Ti-6Al-4V components with enhanced mechanical properties (tensile strength of 1179 MPa).
Nb-Si-B alloys with Nb-rich compositions are fabricated by spark plasma sintering for high-temperature structural applications. Three compositions are selected: 75 at% Nb (Nb0.7), 82 at% Nb (Nb1.5), and 88 at% Nb (Nb3), the atomic ratio of Si to B being 2. The microstructures of the prepared alloys are composed of Nb and T2 phases. The T2 phase is an intermetallic compound with a stoichiometry of Nb5Si3-xBx (0 ≤ x ≤ 2). In some previous studies, Nb-Si-B alloys have been prepared by spark plasma sintering (SPS) using Nb and T2 powders (SPS 1). In the present work, the same alloys are prepared by the SPS process (SPS 2) using Nb powders and hypereutectic alloy powders with composition 67at%Nb-22at%Si-11at%B (Nb67). The Nb67 alloy powders comprise T2 and eutectic (T2 + Nb) phases. The microstructures and hardness of the samples prepared in the present work have been compared with those previously reported; the samples prepared in this study exhibit finer and more uniform microstructures and higher hardness.
TiO2-particles containing Co grains are fabricated via thermal hydrogenation and selective oxidation of Ti-Co alloy. For comparison, TiO2-Co composite powders are prepared by two kinds of methods which were the mechanical carbonization and oxidation process, and the conventional mixing process. The microstructural characteristics of the prepared composites are analyzed by X-ray diffraction, field-emission scattering electron microscopy, and transmission electron microscopy. In addition, the composite powders are sintered at 800°C by spark plasma sintering. The flexural strength and fracture toughness of the sintered samples prepared by thermal hydrogenation and mechanical carbonization are found to be higher than those of the samples prepared by the conventional mixing process. Moreover, the microstructures of sintered samples prepared by thermal hydrogenation and mechanical carbonization processes are found to be similar. The difference in the mechanical properties of sintered samples prepared by thermal hydrogenation and mechanical carbonization processes is attributed to the different sizes of metallic Co particles in the samples.
In this study, lanthanum oxide (La2O3) dispersed molybdenum (Mo–La2O3) alloys are fabricated using lanthanum nitrate solution and nanosized Mo particles produced by hydrogen reduction of molybdenum oxide. The effect of La2O3 dispersion in a Mo matrix on the fracture toughness at room temperature is demonstrated through the formation behavior of La2O3 from the precursor and three-point bending test using a single-edge notched bend specimen. The relative density of the Mo–0.3La2O3 specimen sintered by pressureless sintering is approximately 99%, and La2O3 with a size of hundreds of nanometers is uniformly distributed in the Mo matrix. It is also confirmed that the fracture toughness is 19.46 MPa·m1/2, an improvement of approximately 40% over the fracture toughness of 13.50 MPa·m1/2 on a pure-Mo specimen without La2O3, and this difference in the fracture toughness occurs because of the changes in fracture mode of the Mo matrix caused by the dispersion of La2O3.
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Tungsten carbide (WC) hard materials are used in various industries and possess a superior hardness compared to other hard materials. They have particularly high melting points, high strength, and abrasion resistance. Accordingly, tungsten carbide hard materials are used for wear-resistant tools, cutting tools, machining tools, and other tooling materials. In this study, the WC-5wt.%Co, Fe, Ni hard materials are densified using the horizontal ball milled WC-Co, WC-Fe, and WC-Ni powders by a spark plasma sintering process. The WC-5Co, WC-5Fe, and WC-5Ni hard materials are almost completely densified with a relative density of up to 99.6% after simultaneous application of a pressure of 60 MPa and an electric current for about 15 min without any significant change in the grain size. The average grain size of WC-5Co, WC-5Fe, and WC-5Ni that was produced through SPS was about 0.421, 0.779, and 0.429 μm, respectively. The hardness and fracture toughness of the dense WC-5Co, WC-5Fe, WC-5Ni hard materials were also investigated.
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In this study, the effect of the content of MgO-CaO-Al2O3-SiO2 (MCAS) glass additives on the properties of AlN ceramics is investigated. Dilatometric analysis and isothermal sintering for AlN compacts with MCAS contents varying between 5 and 20 wt% are carried out at temperatures ranging up to 1600°C. The results showed that the shrinkage of the AlN specimens increases with increasing MCAS content, and that full densification can be obtained irrespective of the MCAS content. Moreover, properties of the AlN-MCAS specimens such as microhardness, thermal conductivity, dielectric constant, and dielectric loss are analyzed. Microhardness and thermal conductivity decrease with increasing MCAS content. An acceptable candidate for AlN application is obtained: an AlN-MCAS composite with a thermal conductivity over 70 W/m·K and a dielectric loss tangent (tan δ) below 0.6 × 10−3, with up to 10 wt% MCAS content.
The impact of different mixing methods and sintering temperatures on the microstructure and piezoelectric properties of PZNN-PZT ceramics is investigated. To improve the sinterability and piezoelectric properties of these ceramics, the composition of 0.13Pb((Zn0.8Ni0.2)1/3Nb2/3)O3-0.87Pb(Zr0.5Ti0.5)O3 (PZNN-PZT) containing a Pb-based relaxor component is selected. Two methods are used to create the powder for the PZNN-PZT ceramics. The first involves blending all source powders at once, followed by calcination. The second involves the preferential creation of columbite as a precursor, by reacting NiO with Nb2O5 powder. Subsequently, PZNN-PZT powder can be prepared by mixing the columbite powder, PbO, and other components, followed by an additional calcination step. All the PZNNPZT powder samples in this study show a nearly-pure perovskite phase. High-density PZNN-PZT ceramics can be fabricated using powders prepared by a two-step calcination process, with the addition of 0.3 wt% MnO2 at even relatively low sintering temperatures from 800°C to 1000°C. The grain size of the ceramics at sintering temperatures above 900°C is increased to approximately 3 μm. The optimized PZNN-PZT piezoelectric ceramics show a piezoelectric constant (d33) of 360 pC/N, an electromechanical coupling factor (kp) of 0.61, and a quality factor (Qm) of 275.
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In this study, MgO–CaO–Al2O3–SiO2 (MCAS) nanocomposite glass powder having a mean particle size of 50 nm and a specific surface area of 40 m2/g is used as a sintering additive for AlN ceramics. Densification behaviors and thermal properties of AlN with 5 wt% MCAS nano-glass additive are investigated. Dilatometric analysis and isothermal sintering of AlN-5wt% MCAS compact demonstrates that the shrinkage of the AlN specimen increases significantly above 1,300°C via liquid phase sintering of MCAS additive, and complete densification could be achieved after sintering at 1,600°C, which is a reduction in sintering temperature by 200°C compared to conventional AlN-Y2O3 systems. The MCAS glass phase is satisfactorily distributed between AlN particles after sintering at 1,600°C, existing as an amorphous secondary phase. The AlN specimen attained a thermal conductivity of 82.6 W/m·K at 1,600°C.
Citations
Molybdenum silicide has gained interest for high temperature structural applications. However, poor fracture toughness at room temperatures and low creep resistance at elevated temperatures have hindered its practical applications. This study uses a novel powder metallurgical approach applied to uniformly mixed molybdenum silicidebased composites with silicon carbide. The degree of powder mixing with different ball milling time is also demonstrated by Voronoi diagrams. Core-shell composite powder with Mo nanoparticles as the shell and β-SiC as the core is prepared via chemical vapor transport. Using this prepared core-shell composite powder, the molybdenum silicide-based composites with uniformly dispersed β-SiC are fabricated using pressureless sintering. The relative density of the specimens sintered at 1500°C for 10 h is 97.1%, which is similar to pressure sintering owing to improved sinterability using Mo nanoparticles.
Nanoparticles of PbTe are prepared via chemical reaction of the equimolar aqueous solutions of Pb(CH3COO)2 and Te at 120°C. The size of the obtained particles is 100 nm after calcination in a hydrogen atmosphere. Dense specimens for the thermoelectric characterization are produced by spark plasma sintering of prepared powders at 400°C to 500°C under 80 MPa for 5 min. The relative densities of the prepared specimens reach approximately 97% and are identified as cubic based on X-ray diffraction analyses. The thermoelectric properties are evaluated between 100°C and 300°C via electrical conductivity, Seebeck coefficient, and thermal conductivity. Compared with PbTe ingot, the reduction of the thermal conductivities by more than 30% is verified via phonon scattering at the grain boundaries, which thus contributes to the increase in the figure of merit.
Citations
In this study, the compound Li3BO3 (LBO) is intended to be prepared by a polymeric complex method as a sintering aid for the densification of Li7La3Zr2O12 (LLZ) solid electrolyte. A polymeric precursor containing Li and B is heat-treated in an air atmosphere at a temperature range between 600°C and 800°C. Instead of LBO, the compound Li2+xC1-xBxO3 (LCBO) is unexpectedly synthesized after a heat-treatment of 700°C. The effect of LCBO addition on sintering behavior and ion conductivity of LLZ is studied. It is found that the LCBO compound could lead to significant improvements in the densification and ionic conductivity of LLZ compared to pure LLZ. After sintering at 1100°C, the density of the LLZ-12wt%LBO composite is 3.72 g/cm3, with a high Li-ion conductivity of 1.18 × 10−4 Scm-1 at 28°C, while the pure LLZ specimen had a densify of 2.98 g/cm3 and Li-ion conductivity of 5.98 × 10−6 Scm-1.
Citations
The objective of this study is to reveal the sintering mechanism of mixed Ti-6Al-4V powders considering the densification and the homogenization between Ti and Al/V particles. It is found that the addition of master alloy particles into Ti enhances densification by the migration of Al into the Ti matrix prior to the self-diffusion of Ti. However, as Ti particles become coarser, sintering of the powders appears to be retarded due to slower inter-diffusion of the particles due to the reduced surface energies of Ti. Such phenomena are confirmed by a series of dilatometry tests and microstructural analyses in respect to the sintering temperature. Furthermore, the results are also consistent with the predicted activation energies for sintering. The energies are found to have decreased from 299.35 to 135.48 kJ·mol-1 by adding the Al/V particles because the activation energy for the diffusion of Al in α-Ti (77 kJ·mol-1) is much lower than that of the self-diffusion of α-Ti. The coarser Ti powders increase the energies from 135.48 to 181.16 kJ·mol-1 because the specific surface areas of Ti decrease.