Citations
Citations
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.
Citations
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.
YAG phosphor powders were fabricated by the atmospheric plasma spraying method with the spray-dried spherical YAG precursor. The YAG precursor slurry for the spray drying process was prepared by the PVA solution chemical processing utilizing a domestic easy-sintered aluminum oxide (Al2O3) powder as a seed. The homogenous and viscous slurry resulted in dense granules, not hollow or porous particles. The synthesized phosphor powders demonstrated a stable YAG phase, and excellent fluorescence properties of approximately 115% compared with commercial YAG:Ce3+ powder. The microstructure of the phosphor powder had a perfect spherical shape and an average particle s ize of a pprox imately 30 μm. As a r esult of t he PKG t est of t he YAG p hosphor p owder, t he s ynthesized phosphor powders exhibited an outstanding luminous intensity, and a peak wavelength was observed at 531 nm.
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.
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.
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, 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.
Citations
The effects of different spray angles (90°, 85°, 80°) on the microstructure and mechanical properties of a Y2O3 coating layer prepared using the atmospheric plasma spray (APS) process were studied. The powders employed in this study had a spherical shape and included a cubic Y2O3 phase. The APS coating layer exhibited the same phase as the powders. Thickness values of the coating layers were 90°: 203.7 ± 8.5 μm, 85°: 196.4 ± 9.6 μm, and 80°: 208.8 ± 10.2 μm, and it was confirmed that the effect of the spray angle on the thickness was insignificant. The porosities were measured as 90°: 3.9 ± 0.85%, 85°: 11.4 ± 2.3%, and 80°: 12.7 ± 0.5%, and the surface roughness values were 90°: 5.9 ± 0.3 μm, 85°: 8.5 ± 1.1 μm, and 80°: 8.5 ± 0.4 μm. As the spray angle decreased, the porosity increased, but the surface roughness did not show a significant difference. Vickers hardness measurements revealed values of 90°: 369.2 ± 22.3, 85°: 315.8 ± 31.4, and 80°: 267.1 ± 45.1 HV. It was found that under the condition of a 90° angle with the lowest porosity exhibited the best hardness value. Based on the aforementioned results, an improved method for the APS Y2O3 coating layer was also discussed.
Citations
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.
Citations
Powder quality, including high flowability and spherical shape, determines the properties of additively manufactured products. Therefore, the cheap production of high-quality powders is critical in additive manufacturing. Radio frequency plasma treatment is an effective method to fabricate spherical powders by melting the surface of irregularly shaped powders; in the present work, mechanically milled Zr powders are spheroidized by radio frequency plasma treatment and their properties are compared with those of commercial Zircaloy-2 alloy powder. Spherical Zr particles are successfully fabricated by plasma treatment, although their flowability and impurity contents are poorer than those of the commercial Zircaloy-2 alloy powder. This result shows that radio-frequency plasma treatment with mechanically milled powders requires further research and development for manufacturing low-cost powders for additive manufacturing.
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 enamel powders used traditionally in Korea are produced by a ball-milling process. Because of their irregular shapes, enamel powders exhibit poor flowability. Therefore, polygonal enamel powders are only used for handmade cloisonné crafts. In order to industrialize or automate the process of cloisonné crafts, it is essential to control the size and shape of the powder. In this study, the flowability of the enamel powders was improved using the spheroidization process, which employs the RF plasma treatment. In addition, a simple grid structure and logo were successfully produced using the additive manufacturing process (powder bed fusion), which utilizes spherical enamel powders. The additive manufacturing technology of spherical enamel powders is expected to be widely used in the field of cloisonné crafting in the future.
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.
Citations
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.
Citations
In this study, we fabricate a thin- and dense-BCuP-5 coating layer, one of the switching device multilayers, through a plasma spray process. In addition, the microstructure and macroscopic properties of the coating layer, such as hardness and bond strength, are investigated. Both the initial powder feedstock and plasma-sprayed BCuP-5 coating layer show the main Cu phase, Cu-Ag-Cu3P ternary phases, and Ag phase. This means that microstructural degradation does not occur during plasma spraying. The Vickers hardness of the coating layer was measured as 117.0 HV, indicating that the fine distribution of the three phases enables the excellent mechanical properties of the plasma-sprayed BCuP-5 coating layer. The pull-off strength of the plasma-sprayed BCuP-5 coating layer is measured as 16.5 kg/cm2. Based on the above findings, the applicability of plasma spray for the fabrication process of low-cost multi-layered electronic contact materials is discussed and suggested.
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.
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.
In the present work, spheroidization of angular vanadium powders using a radio frequency (RF) thermal plasma process is investigated. Initially, angular vanadium powders are spheroidized successfully at an average particle size of 100 μm using the RF-plasma process. It is difficult to avoid oxide layer formation on the surface of vanadium powder during the RF-plasma process. Titanium/vanadium/stainless steel functionally graded materials are manufactured with vanadium as the interlayer. Vanadium intermediate layers are deposited using both angular and spheroidized vanadium powders. Then, 17-4PH stainless steel is successfully deposited on the vanadium interlayer made from the angular powder. However, on the surface of the vanadium interlayer made from the spheroidized powder, delamination of 17-4PH occurs during deposition. The main cause of this phenomenon is presumed to be the high thickness of the vanadium interlayer and the relatively high level of surface oxidation of the interlayer.
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.
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.
Citations
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
Al2O3-SiC ceramic composites are produced using pressureless sintering, and their plasma resistance, electrical resistance, and mechanical properties are evaluated to confirm their applicability as electrostatic-discharge-safe components for semiconductor devices. Through the addition of Mg and Y nitrate sintering aids, it is confirmed that even if SiC content exceeded 10%, complete densification is possible by pressureless sintering. By the uniform distribution of SiC, the total grain growth is suppressed to about 1 μm; thus an Al2O3-SiC sintered body with a high strength over 600 MPa is obtained. The optimum amount of SiC to satisfy all the desired properties of electrostaticdischarge-safe ceramic components is obtained by finding the correlation between the plasma resistance and the electrical resistivity as a function of SiC amount.
Boron nitride nanotubes (BNNTs) are receiving great attention because of their unusual material properties, such as high thermal conductivity, mechanical strength, and electrical resistance. However, high-throughput and highefficiency synthesis of BNNTs has been hindered due to the high boiling point of boron (~ 4000°C) and weak interaction between boron and nitrogen. Although, hydrogen-catalyzed plasma synthesis has shown potential for scalable synthesis of BNNTs, the direct use of H2 gas as a precursor material is not strongly recommended, as it is extremely flammable. In the present study, BNNTs have been synthesized using radio-frequency inductively coupled thermal plasma (RF-ITP) catalyzed by solid-state ammonium chloride (NH4Cl), a safe catalyst materials for BNNT synthesis. Similar to BNNTs synthesized from h-BN (hexagonal boron nitride) + H2, successful fabrication of BNNTs synthesized from h-BN+NH4Cl is confirmed by their sheet-like properties, FE-SEM images, and XRD analysis. In addition, improved dispersion properties in aqueous solution are found in BNNTs synthesized from h-BN +NH4Cl.
SiC-based composite materials with light weight, high durability, and high-temperature stability have been actively studied for use in aerospace and defense applications. Moreover, environmental barrier coating (EBC) technologies using oxide-based ceramic materials have been studied to prevent chemical deterioration at a high temperature of 1300°C or higher. In this study, an ytterbium silicate material, which has recently been actively studied as an environmental barrier coating because of its high-temperature chemical stability, is fabricated on a sintered SiC substrate. Yb2O3 and SiO2 are used as the raw starting materials to form ytterbium disilicate (Yb2Si2O7). Suspension plasma spraying is applied as the coating method. The effect of the mixing method on the particle size and distribution, which affect the coating formation behavior, is investigated using a scanning electron microscope (SEM), an energy dispersive spectrometer (EDS), and X-ray diffraction (XRD) analysis. It is found that the originally designed compounds are not effectively formed because of the refinement and vaporization of the raw material particles, i.e., SiO2, and the formation of a porous coating structure. By changing the coating parameters such as the deposition distance, it is found that a denser coating structure can be formed at a closer deposition distance.
Citations
Microstructure, electric, and thermal properties of the Ta-Cu composite is evaluated for the application in electric contact materials. This material has the potential to be used in a medium for a high current range of current conditions, replacing Ag-MO, W, and WC containing materials. The optimized SPS process conditions are a temperature of 900°C for a 5 min holding time under a 30 MPa mechanical pressure. Comparative research is carried out for the calculated and actual values of the thermal and electric properties. The range of actual thermal and electric properties of the Ta-Cu composite are 50~300W/mk and 10~90 %IACS, respectively, according to the compositional change of the 90 to 10 wt% Ta-Cu system. The results related to the electric contact properties, suggest that less than 50 wt% of Ta compositions are possible in applications of electric contact materials.
Citations
In this study, Bi-Sb-Te thermoelectric materials are produced by mechanical alloying (MA) and spark plasma sintering (SPS). To examine the influence of the milling atmosphere on the microstructure and thermo-electric (TE) properties, a p-type Bi-Sb-Te composite powder is mechanically alloyed in the presence of argon and air atmospheres. The oxygen content increases to 55% when the powder is milled in the air atmosphere, compared with argon. All grains are similar in size and uniformly, distributed in both atmospheric sintered samples. The Seebeck coefficient is higher, while the electrical conductivity is lower in the MA (Air) sample due to a low carrier concentration compared to the MA (Ar) sintered sample. The maximum figure of merit (ZT) is 0.91 and 0.82 at 350 K for the MA (Ar) and MA (Air) sintered samples, respectively. The slight enhancement in the ZT value is due to the decrease in the oxygen content during the MA (Ar) process. Moreover, the combination of mechanical alloying and SPS process shows a higher hardness and density values for the sintered samples.
Citations
Tin dioxide nanoparticles are prepared using a newly developed synthesis method of plasma-assisted electrolysis. A high voltage is applied to the tin metal plate to apply a high pressure and temperature to the synthesized oxide layer on the metal surface, producing nanoparticles in a low concentration of sulfuric acid. The particle size, morphology, and size distribution is controlled by the concentration of electrolytes and frequency of the power supply. The as-prepared powder of tin dioxide nanoparticles is used to fabricate a gas sensor to investigate the potential application. The particle-based gas sensor exhibits a short response and recovery time. There is sensitivity to the reduction gas for the gas flowing at rates of 50, 250, and 500 ppm of H2S gas.
Citations
In this study, Fe-Cu-C alloy is sintered by spark plasma sintering (SPS). The sintering conditions are 60 MPa pressure with heating rates of 30, 60 and 9°C/min to determine the influence of heating rate on the mechanical and microstructure properties of the sintered alloys. The microstructure and mechanical properties of the sintered Fe-Cu-C alloy is investigated by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The temperature of shrinkage displacement is changed at 450°C with heating rates 30, 60, and 90°C/min. The temperature of the shrinkage displacement is finished at 650°C when heating rate 30°C/min, at 700°C when heating rate 60oC/min and at 800°C when heating rate 90oC/min. For the sintered alloy at heating rates of 30, 60, and 90oC/min, the apparent porosity is calculated to be 3.7%, 5.2%, and 7.7%, respectively. The hardness of the sintered alloys is investigated using Rockwell hardness measurements. The objective of this study is to investigate the densification behavior, porosity, and mechanical properties of the sintered Fe-Cu-C alloys depending on the heating rate.
Citations
In this work, p-type Bi−Sb−Te alloys powders are prepared using gas atomization, a mass production powder preparation method involving rapid solidification. To study the effect of the sintering temperature on the microstructure and thermoelectric properties, gas-atomized powders are consolidated at different temperatures (623, 703, and 743 K) using spark plasma sintering. The crystal structures of the gas-atomized powders and sintered bulks are identified using an X-ray diffraction technique. Texture analysis by electron backscatter diffraction reveals that the grains are randomly oriented in the entire matrix, and no preferred orientation in any unique direction is observed. The hardness values decrease with increasing sintering temperature owing to a decrease in grain size. The conductivity increases gradually with increasing sintering temperature, whereas the Seebeck coefficient decreases owing to increases in the carrier mobility with grain size. The lowest thermal conductivity is obtained for the bulk sintered at a low temperature (603 K), mainly because of its fine-grained microstructure. A peak ZT of 1.06 is achieved for the sample sintered at 703 K owing to its moderate electrical conductivity and sustainable thermal conductivity.
Citations
We fabricate fine (<20 μm) powders of Bi0.5Sb1.5Te3 alloys using a large-scale production method and subsequently consolidate them at temperatures of 573, 623, and 673 K using a spark plasma sintering process. The microstructure, mechanical properties, and thermoelectric properties are investigated for each sintering temperature. The microstructural features of both the powders and bulks are characterized by scanning electron microscopy, and the crystal structures are analyzed by X-ray diffraction analysis. The grain size increases with increasing sintering temperature from 573 to 673 K. In addition, the mechanical properties increase significantly with decreasing sintering temperature owing to an increase in grain boundaries. The results indicate that the electrical conductivity and Seebeck coefficient (217 μV/K) of the sample sintered at 673 K increase simultaneously owing to decreased carrier concentration and increased mobility. As a result, a high
Citations
In this study, bulk nickel-carbon nanotube (CNT) nanocomposites are synthesized by a novel method which includes a combination of ultrasonication, electrical explosion of wire in liquid and spark plasma sintering. The mechanical characteristics of the bulk Ni-CNT composites synthesized with CNT contents of 0.7, 1, 3 and 5 wt.% are investigated. X-ray diffraction, optical microscopy and field emission scanning electron microscopy techniques are used to observe the different phases, morphologies and structures of the composite powders as well as the sintered samples. The obtained results reveal that the as-synthesized composite exhibits substantial enhancement in the microhardness and values more than 140 HV are observed. However an empirical reinforcement limit of 3 wt.% is determined for the CNT content, beyond which, there is no significant improvement in the mechanical properties.
Citations
In this study, Fe-Cu-Ni-Mo-C low alloy steel powder is consolidated by spark plasma sintering (SPS) process. The internal structure and the surface fracture behavior are studied using field-emission scanning electron microscopy and optical microscopy techniques. The bulk samples are polished and etched in order to observe the internal structure. The sample sintered at 900°C with holding time of 10 minutes achieves nearly full density of 98.9% while the density of the as-received conventionally sintered product is 90.3%. The fracture microstructures indicate that the sample prepared at 900°C by the SPS process is hard to break out because of the presence of both grain boundaries and internal particle fractures. Moreover, the lamellar pearlite structure is also observed in this sample. The samples sintered at 1000 and 1100°C exhibit a large number of tiny particles and pores due to the melting of Cu and aggregation of the alloy elements during the SPS process. The highest hardness value of 296.52 HV is observed for the sample sintered at 900°C with holding time of 10 minutes.
Citations
Composite materials consisting of pure aluminum matrix reinforced with different amounts of graphite particles are successfully fabricated by mechanical ball milling and spark plasma sintering (SPS) processes. The shrinkage rates of the composite powders vary with the amount of graphite particles and the lowest shrinkage value is observed for the composite with the highest amount of graphite particles. The current slopes of time increase with increase in the amount of graphite particles whereas the current slopes of temperature show the opposite trend. The highest thermal conductivity is achieved for the composite with the least amount of graphite particles. Therefore, the thermal properties of the composite materials can be controlled by controlling the amount of the graphite particles during the SPS process.
Citations
Citations
Waste SiC powders obtained from silicon wafer sludge have very low density and a narrow particle size distribution of 10-20 μm. A scarce yield of C and Si is expected when SiC powders are incorporated into the Fe melt without briquetting. Here, the briquetting variables of the SiC powders are studied as a function of the sintering temperature, pressure, and type and contents of the binders to improve the yield. It is experimentally confirmed that Si and C from the sintered briquette can be incorporated effectively into the Fe melt when the waste SiC powders milled for 30 min with 20 wt.% Fe binder are sintered at 1100°C upon compaction using a pressure of 250 MPa. XRF-WDS analysis shows that an yield of about 90% is obtained when the SiC briquette is kept in the Fe melt at 1650°C for more than 1 h.
Microstructural examination of the Nb-Si-B alloys at Nb-rich compositions is performed. The Nb-rich corner of the Nb-Si-B system is favorable in that the constituent phases are Nb (ductile and tough phase with high melting temperature) and T2 phase (very hard intermetallic compound with favorable oxidation resistance) which are good combination for high temperature structural materials. The samples containing compositions near Nb-rich corner of the Nb- Si-B ternary system are prepared by spark plasma sintering (SPS) process using T2 and Nb powders. T2 bulk phase is made in arc furnace by melting the Nb slug and the Si-B powder compact. The T2 bulk phase was subsequently ballmilled to powders. SPS is performed at 1300°C and 1400°C, depending on the composition, under 30 MPa for 600s, to produce disc-shaped specimen with 15 mm in diameter and 3 mm high. Hardness tests (Rockwell A-scale and micro Vickers) are carried out to estimate the mechanical property.
Citations
Lanthanum zirconate, La2Zr2O7, is one of the most promising candidates for next-generation thermal barrier coating (TBC) applications in high efficient gas turbines due to its low thermal conductivity and chemical stability at high temperature. In this study, bulk specimens and thermal barrier coatings are fabricated via a variety of sintering processes as well as suspension plasma spray in lanthanum zirconates with reduced rare-earth contents. The phase formation, microstructure, and thermo-physical properties of these oxide ceramics and coatings are examined. In particular, lanthanum zirconates with reduced rare-earth contents in a La2Zr2O7-4YSZ composite system exhibit a single phase of fluorite or pyrochlore after fabricated by suspension plasma spray or spark plasma sintering. The potential of lanthanum zirconate ceramics for TBC applications is also discussed.
Citations
Fe-30 wt% TiC composite powders are fabricated by in situ reaction synthesis after planetary ball milling of (Fe, TiH2, Carbon) powder mixture. Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-30 wt% TiC composite powder compacts. Pressureless sintering is performed at 1100, 1200 and 1300°C for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of 1050°C, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of 50°C/min, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts are not densified even after sintering at 1300°C for 3 h, which shows a relative denstiy of 66.9%. Spark-plasma sintering at 1050°C for 10 min exhibits nearly full densification of 99.6% relative density under the sintering pressure of 50 MPa.
Citations
Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe- TiC composite powders which are fabricated by high-energy ball-milling. A powder mixture of Fe and TiC is prepared in a planetary ball mill at a rotation speed of 500 rpm for 1h. Pressureless sintering is performed at 1100, 1200 and 1300°C for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of 1050°C, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of 50°C, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts show incomplete densification with a relative denstiy of 86.1% after sintering at 1300°C for 3h. Spark-plasma sintering at 1050°C for 10 min exhibits nearly complete densification of 98.6% relative density under the sintering pressure of 50 MPa.
Citations