Fracture toughness enhancement via sub-micro silver-precipitation in silica glass fabricated by spark plasma sintering

Sub-micro silver (Ag) precipitated in silica (SiO₂) glass was prepared via spark plasma sintering (SPS), and the microstructure, mechanical properties, and thermal conductivity were investigated. The in situ formation of Ag sub-micro particles through decomposition of silver nitrate (AgNO₃) was homogeneously distributed within the SiO₂ matrix. By precipitation of Ag particles, larger steady-state creep deformation and plastic deformation were observed owing to the ductility of the Ag particles. Moreover, crack bridging and pull-out of Ag particles were observed during crack propagation. As a result, the fracture toughness of SiO₂ glass improved with increasing Ag content. The sample with 1.4 vol% Ag sintered at 1200°C showed the highest toughness value of 2.15 ± 0.2 MPa m^1/2. Larger Ag particles in the samples sintered at higher temperatures tend to deform easily, resulting in larger ductility. In addition, incorporation of Ag particles improved thermal conductivity.     

Power-controlled flash spark plasma sintering of gadolinia-doped ceria

Electric field-assisted sintering (FAST) is a rapidly growing scientific and engineering domain. In the present paper, we describe the process of flash sintering (FS) in a configuration of classical spark plasma sintering (SPS) (graphite punch and boron nitride (BN) die), also called flash spark plasma sintering (FSPS). The densification process of Gd_0.1Ce_0.9O_2-x powder is studied in detail with a focus on the transition from FAST to FS. We discuss the electrical, geometrical, and thermal evolution of the process and the characteristics of the final compacts. Low electrical fields are sufficient for the onset of FS. Ceria is a material difficult to sinter by FAST techniques due to its known mechanochemical transformations. We observed the disintegration of pellets after experiments with well-pronounced flash event.     

放电等离子烧结合成单相MgAlON材料

以氮化铝、富铝镁铝尖晶石和氧化铝为原料 ,用放电等离子烧结 (SPS)技术合成了单相MgAlON,研究了其显微结构 ,并与用传统的无压烧结 (PLS)技术制备的单相MgAlON材料在显微结构和断裂行为上做了比较。结果表明 :用SPS法在 170 0℃保温 1min的条件下合成出的单相MgAlON材料 ,显微结构比用PLS法合成的更加均匀致密 ,且晶粒细小 ;前者的断裂模式主要是穿晶断裂 ,后者的断裂模式则主要是沿晶断裂。     

Densification behaviour and physico-mechanical properties of porcelains prepared using spark plasma sintering

Porcelain powder was consolidated using spark plasma sintering (SPS) at a constant heating rate of 100°C?min^?1 to peak temperatures ranging from 1000 to 1200°C and was observed to sinter at relatively low temperature ～920°C under the SPS conditions while conventional sintering requires ～1050°C. SPS produced densification rates about 10 times greater than conventional sintering. The dwelling step at the optimal peak temperature was negligible due to rapid flow of the molten glass assisted by applied pressure. SPSed samples exhibited denser microstructures, resulting in improved physico-mechanical properties compared with conventionally sintered samples such as apparent bulk density improved from 2.38 to 2.48?g?cm^?3, Vickers hardness improved from 3–5 to 6–7?GPa, and fracture toughness improved from 2–3 to 4–6?MPa?m^1/2.     

Fabrication of translucent AlN ceramics with MgF2 additive by spark plasma sintering

Translucent AlN ceramics with 0‐2 wt.% MgF₂ additive were prepared by spark plasma sintering. AlN powder was heated temporarily up to 2000°C, before holding at 1850°C for 20 minutes in N₂ gas. The sintered ceramics consisted of a single phase of hexagonal AlN, and showed a transgranular fracture mode. The total transmittance was improved remarkably by the additive, to reach 74% at a wavelength of 800 nm for 1 wt.% MgF₂. For 2 wt.% MgF₂, the transmittance was slightly lower than that for 1 wt.% MgF₂, and an absorption band was observed apparently at around 400 nm. The addition of MgF₂ along with the temporary heating at higher temperatures than the sintering temperature contributed to improve the transmittance remarkably.     

Consolidation by spark plasma sintering of polyimide and polyetheretherketone

This article presents two high‐temperature thermoplastic powders which were sintered by spark plasma sintering in order to get homogeneous mechanical properties. Dense polyimide (PI) and polyetheretherketone (PEEK) specimens were obtained at temperatures as low as 320°C for PI and 200°C for PEEK, respectively. Relative densities higher than 99% were reached for both materials. In order to characterize their properties, in situ measurements with compression and hardness tests were carried out on sintered samples. This method allowed to obtain polymeric materials with improved mechanical properties. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40783.     

Oxidation effects on spark plasma sintering of molybdenum nanopowders

Surface-oxidized molybdenum nanopowders are compacted by spark plasma sintering (SPS). The oxide impurity behavior is analyzed under various sintering temperatures. The densification mechanism of the nanopowders with a melted oxide phase is identified in situ by regression analysis of the experimental data on the temperature-dependent porosity change and on the SPS multistep pressure dilatometry. To increase the density of the compacted pellets, the nanopowders with the oxide phase are consolidated by SPS using the two in situ oxide removal methods: carbothermic reduction and particle surface cleaning by the electric current flow through the powders. The advantages and disadvantages of these methods in terms of the density, grain size, and mechanical properties of the final products are discussed.     

Synthesis of dense NiZn ferrites by spark plasma sintering

Dense NiZn ferrites were fabricated by spark plasma sintering (SPS) at 900 °C and 20 MPa in short periods. The powder was densified to 98% of the theoretical density by the SPS process. The SPS disks exhibited a higher saturation magnetization (Ms), up to 272 emu/cm³, than did the disks sintered by the conventional process. A higher coercivity (Hci) was obtained when the green bodies were sintered by the SPS process for 5 min. A modest holding time is essential to obtain fine grain and uniformity in the SPS process. Secondary crystallization, inhomogeneous microstructure and intragranular pores were found as a result of the rapid sintering and relatively longer holding time in the SPS process. Infrared (IR) spectra were also measured in the range from 350 to 700 cm⁻¹ to study the efforts of the SPS process on NiZn ferrites.     

Consolidation by spark plasma sintering (SPS) of polyetheretherketone

The present study deals with the consolidation of an ultra‐high performance polymer, the poly(ether ether ketone) (PEEK), for structural applications, using the powder metallurgy (PM) way, and more precisely the Spark Plasma Sintering (SPS) processing. The effects of SPS parameters such as temperature, pressure, and dwell time on density and mechanical properties of PEEK were investigated via a Design of Experiments (DoE). A temperature of 250 °C, a pressure of 40 MPa, and a dwell time of 20 min have been identified as the optimal SPS process parameters. In these conditions, a density of 1.31 g / cm³ was reached and homogeneous mechanical properties in the volume determined by means of compression tests were found with a compressive modulus of 2.75 GPa, a yield strength of 134 MPa, and a maximum compressive strain of 43%. These results are better than those of commercial products obtained by injection molding. The pressure appears to be a significant parameter on PEEK properties and plays positive or negative roles according to the responses of DoE studied. To our knowledge, it is one of the first studies based on the application of the PM techniques for PEEK consolidation showing the possibility to process below its melting point. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44911.     

Microstructure and properties of WC-8Co cemented carbides prepared by multiple spark plasma sintering

In this study, WC-8Co cemented carbides were prepared by spark plasma sintering. When the samples sintered at 1300℃ were cooled to room temperature, the samples were sintered multiple times at 1250℃. The changes in microstructure and mechanical properties of WC-8Co cemented carbides prepared by multiple spark plasma sintering were studied. The hardness of cemented carbides increased in the first two sintering, reaching 16.5 GPa. However, the hardness decreased seriously in the last two sintering. The attenuation rates of hardness were 6.2% and 2.5% due to the abnormal coarse grains. Furthermore, the crack path along the grain boundary was almost straight, causing a decrease in the indentation fracture toughness of cemented carbides. Additionally, the grains of cemented carbides were abnormally coarsened, and the morphologies of grains became unstable due to multiple sintering.     

The thermal stability and consolidation of perovskite variant Cs2SnCl6 using spark plasma sintering

Defect perovskites, a category of air and moisture stable perovskite molecular salts, have gained attention for photovoltaics in the search of alternatives to the organic lead‐based photovoltaics which show exceptional photovoltaic performance but suffer significant environmental instability and toxicity of Pb. Defect perovskites also have exceptional structural flexibility and diverse crystal chemistry, and thus, display potentials as host phases for incorporating high amounts of halides such as iodine and chorine. In this study, pure Cs₂SnCl₆, a lead‐free defect perovskite variant, was synthesized through a solution‐based route that produced particles ranging from 200 to 500 nm. The thermal stability of the as‐synthesized Cs₂SnCl₆ powders was investigated using thermogravimetric analysis (TGA), demonstrating stability up to 615°C, above which a phase decomposition occurs leading to the loss of constituent component of SnCl₄. Consolidation of Cs₂SnCl₆ into dense pellets (≥94% theoretical density) was achieved via spark plasma sintering (SPS) at a low sintering temperature of 350°C. X‐ray diffraction confirms no phase decomposition in the SPS‐densified perovskite pellets as a result of rapid consolidation of the SPS sintering at a short duration and lower temperature, and the TGA analysis suggest a comparable thermal stability up to 627°C for the densified pellet, slightly better than the as‐synthesized powders. The thermal diffusivity of Cs₂SnCl₆ at room temperature was determined as 0.388 mm²·s^?1 by laser flash measurement. This work further discussed the potential applications of the SPS‐densified Cs₂SnCl₆ beyond perovskite photovoltaics, introducing potential nuclear separations and waste forms for chlorine.     

Microstructure evolution during spark plasma sintering of FJS-1 lunar soil simulant

A spark plasma sintering (SPS) process has been explored to densify FJS-lunar soil simulants for structural applications in space explorations. The effect of SPS conditions, such as temperature and pressure, on the densification behavior, phase transformation, microstructural evolution, and mechanical properties of FJS-1 have been examined by conducting the X-ray diffraction analysis, electron microscopy imaging, and nano/micro indentation testing. Test analysis results were also compared to results from the FJS-1 powder and sintered samples without pressure. The FJS-1 powder was composed of sodian anorthite, augite, pigeonite, and iron titanium oxide. When FJS-lunar soil simulants were sintered without pressure, the main phase evolved from sodian anorthite to the intermediate sodian anorthite, jadeite and glass, and iron titanium oxide at 1000°C, which were further transformed into filiform and feather-shaped augite and schorlomite at 1100°C. Most densification processes in pressureless sintering occurred at 1050°C-1100°C. During the SPS process, the main phases were sodian anorthite, pigeonite, and iron titanium oxide at 900°C. These phases were transformed to sodian anorthite, glass, and feather-shaped augite at 1000°C and 1050°C, with the nucleation of dendritic schorlomite at 1050°C. Significant densification by SPS can be observed as low as 900°C, which indicates that the application of pressure can substantially lower the sintering temperature. The SPSed samples showed higher Vickers microhardness than the pressureless sintered samples. The mechanical properties of the local phases were represented by the contour maps of elastic modulus and nanohardness. Multiscale mechanical test results along with the microstructural characteristics further imply that the SPS can be considered a promising in-situ resource utilization (ISRU) method to densify lunar soils.     

Impact of spark plasma sintering (SPS) on mullite formation in porcelains

The effect of the spark plasma sintering (SPS) process on mullite formation in porcelains was studied using X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy. SPS affected the kinetics and morphology of formed mullite. After sintering at 1100°C, unlike conventional sintering, SPS promoted the formation of mullite due to the combination of vacuum and applied pressure. Mullite crystal growth was altered by the atmosphere (vacuum), dwell time (0‐15 minutes), and temperature (1000‐1200°C). The applied pressure caused the mullite needles to orient perpendicular to the direction of the applied load. Depending on SPS dwell time, the mullite formed after sintering at 1100°C also had different crystal structure (tetragonal for short dwell time of 0‐5 minutes and orthorhombic for a long dwell time of 10‐15 minutes). Dissolution of mullite was observed at 1100°C by extending the dwell time by up to 15 minutes and the dissolved mullite reprecipitated on the small needles (~40 nm) and coarsened via Oswald ripening resulting in larger mullite needles (~60 nm).     

Pressure-enhanced densification of TaC ceramics during flash spark plasma sintering

Flash spark plasma sintering (FSPS) offers extremely high heating rates to consolidate ceramics at a short time. However, significant grain growth sometimes occurs accompanied by rapid densification. In this work, a FSPS apparatus available for applying pressure was used to sinter TaC ceramics from powder compacts without preheating. It is found that the use of a higher pressure can efficiently promote densification and retard significant grain growth. Dense bulk TaC ceramics (95.18%) with average grain size of 4.09 μm were obtained in 90 seconds under 80 MPa. Such a process should facilitate the fast preparation of refractory ceramics with fine-grained microstructure.     

Effect of titanium diboride on the homogeneity of boron carbide ceramic by flash spark plasma sintering

A novel method, namely flash spark plasma sintering (FSPS), combining flash sintering and electric field assisted sintering, was utilized to densify boron carbide/titanium diboride (B₄C/TiB₂) composites. Further, sintering homogeneity of the composites with different contents of TiB₂ was systematically investigated and theoretical model was built. Results indicated that addition of 50?wt% TiB2 led to the densification of B₄C/TiB₂ composite by up to 97.7% with regional range 1.9% at 1872?°C under pressure of 4?MPa in 60?s. The preferential pathway of TiB₂ network proves to disperse the central current and distribute thermal flow throughout the specimen possibly via tunneling, electronic field emission effect at first stage and lower-resistance composite pathway latter, contributing to the increased homogeneity.     

Ultraviolet emission transparent Gd:YAG ceramics processed by solid-state reaction spark plasma sintering

Transparent 1% Gd-doped YAG and YAG ceramics were synthesized via solid-state reaction spark plasma sintering using commercially available powder and TESO as a sintering additive. The highest in-line transmission values achieved were 77.1% at 550 nm and 80.6% at 800 nm in the 1% (at.%) Gd-doped YAG transparent ceramic with 99.90% relative density. Ultraviolet emission at 312.5 nm was observed in 1% Gd-doped YAG ceramic via photoluminescence excitation, making it a promising material for applications in solid-state UV devices.     

Low-angle twist grain boundary in SrTiO3 fabricated by spark plasma sintering techniques

A SrTiO₃ bicrystal with a low-angle twist grain boundary was fabricated using the spark plasma sintering (SPS) instrument. The atomic and electronic structure of the grain-boundary core was characterized using scanning transmission electron microscopy techniques. It was determined that the boundary is comprised of 2 types of defects with distinct electronic structures: screw dislocations and dislocations with an [001] edge component. The dislocations with an [001] edge component dissociated into 2 partial dislocations, separated by a stacking fault consisting of 2 Ti–O layers. The screw dislocations are attributed to the twist component of the grain boundary, while dislocations with an [001] edge component are attributed to surface steps on the original (100) SrTiO₃ surfaces prior to diffusion bonding. The observed repeat distances between the dislocations with edge components along the grain-boundary plane are smaller than those discovered during traditional diffusion bonding experiments. The higher planar defect density observed in this study results partly from higher heating rates, lower processing temperatures, and shorter holding times during SPS processing.     

Transparent Er2O3 ceramics fabricated by high-pressure spark plasma sintering

Fabrication of transparent Er₂O₃ ceramics was carried out by high-pressure spark plasma sintering (HP-SPS). The color and in-line transmittance of these ceramics was highly sensitive to the sintering parameters. Samples exhibited a strong pink or wine color after sintering at 1150 °C under 600 MPa or 1250 °C under 250 MPa, respectively. This was confirmed to be a result of oxygen vacancies created during the sintering process and high sensitivity of Er₂O₃ to the strong reducing atmosphere in the SPS apparatus. Post-sintering annealing in an air furnace led to elimination of oxygen vacancies and increased transparency. Additionally, the photoluminescence intensity and phosphorescence lifetime of annealed (pink) samples was higher and shorter, respectively, compared to that of the reduced (wine-colored) samples.     

Fabrication of powder components with internal channels by spark plasma sintering and additive manufacturing

A novel method of producing complex ceramic and metallic parts with designed internal channels is developed. The method utilizes a combination of the additive manufacturing technique of solvent jetting and spark plasma sintering (SPS.) The developed manufacturing approach brings benefits in producing complex shapes with internal channels. Along with geometric customization of the 3D printed mold, a major advantage of this method is the removal of the need for a long debinding process, usually necessary with other 3D printing methods, by using the SPS. High density ceramic and metallic complex parts with internal channels were successfully produced with close to theoretical densities. The conducted studies include the development of a model that can predict the evolution and/or distortions of the complex-shaped powder assembly during the sintering process. The model is based on the continuum theory of sintering formulations embedded in a finite element code.     

Optical and mechanical properties of transparent alumina fabricated by high-pressure spark plasma sintering

Transparent alumina was fabricated from untreated commercial powder by high-pressure spark plasma sintering (HPSPS) at temperatures of 1000, 1050 and 1100 °C under pressures of 250-800 MPa. It was established that transparency strongly depends on the HPSPS parameters. At all temperatures, there was a certain point when increasing the pressure led to decreasing transparency. At 1100 °C, relatively high pressure led to excessive grain growth, as well as the formation of creep-induced porosity at the center of the samples. Hardness values decreased with pressure due to grain growth, correlated with the Hall-Petch relationship. The optimal combination of optical and mechanical properties (68% in-line transmittance at a wavelength of 640 nm and a hardness value of about 2300 HV2) was achieved after sintering at 1050 °C under 600 MPa.