Reactive Spark Plasma Sintering Research Articles

Reactive Spark Plasma Sintering and Oxidation of ZrB2-SiC and ZrB2-HfB2-SiC Ceramic Materials

This study presents the fabrication possibilities of ultra-high-temperature ceramics of ZrB2-30 vol.%SiC and (ZrB2-HfB2)-30 vol.% SiC composition using the reaction spark plasma sintering of composite powders ZrB2(HfB2)-(SiO2-C) under two-stage heating conditions. The phase composition and microstructure of the obtained ceramic materials have been subjected to detailed analysis, their electrical conductivity has been evaluated using the four-contact method, and the electron work function has been determined using Kelvin probe force microscopy. The thermal analysis in the air, as well as the calcination of the samples at temperatures of 800, 1000, and 1200 °C in the air, demonstrated a comparable behavior of the materials in general. However, based on the XRD data and mapping of the distribution of elements on the oxidized surface (EDX), a slightly higher oxidation resistance of the ceramics (ZrB2-HfB2)-30 vol.% SiC was observed. The I-V curves of the sample surfaces recorded with atomic force microscopy demonstrated that following oxidation in the air at 1200 °C, the surfaces of the materials exhibited a marked reduction in current conductivity due to the formation of a dielectric layer. However, data obtained from Kelvin probe force microscopy indicated that (ZrB2-HfB2)-30 vol.% SiC ceramics also demonstrated enhanced resistance to oxidation.

Reactive spark plasma sintering and luminescence properties of Gd2O2S:Tb nanocrystalline phosphor

Gd2O2S:Tb is promising for energy-efficient lighting and display applications. This work explores the use of reactive spark plasma sintering (SPS) to synthesis Gd2O2S:Tb nanocrystalline phosphor. It allows to significantly simplify the technological process in comparison with traditional multi-stage liquid-phase synthesis. As-sintered Gd2O2S:Tb demonstrated average crystallite size of 26 nm and secondary particle size of 26 μm. Bright green emission occurs at 545 nm under UV excitation of 245 nm. Average fluorescence lifetime was 0.656 ms. Further consolidation of the Gd2O2S:Tb prepared via reactive SPS can also be expected to yield highly dense ceramics. The innovative reactive synthesis strategies provide valuable insights into the design and development of high-performance luminescent ceramics.

Microstructure and Mechanical Properties of Diamond–Ceramic Composites Fabricated via Reactive Spark Plasma Sintering

In order to prepare diamond composites with excellent mechanical properties under non-extreme conditions, in this study, a diamond–ceramic composite was successfully prepared via reactive spark plasma sintering using a diamond–Ti–Si powder mixture as the raw material. The microstructures and mechanical properties of the diamond–ceramic composite sintered at different temperatures were studied. When the sintering temperature was 1500 °C, the diamond–ceramic composite exhibited a volume density of 3.65 g/cm3, whereas the bending strength and fracture toughness were high at 366 MPa and 6.17 MPa·m1/2, respectively. In addition, variable-temperature sintering activated the chemical reaction at a higher temperature, whereas lowering the temperature prevented excessive graphitisation, which is conducive to optimising the microstructure and mechanical properties of the composite.

Effect of processing parameters and carbon to metal ratio on microstructure and mechanical properties of (MoTaTiVW)Cx high entropy carbide produced by reactive spark plasma sintering

(MoTaTiVW)Cx high entropy ceramics with varying carbon to metal ratio in the range of 0.75-0.97 were synthesized by by reactive spark plasma sintering. The effect of ball milling time on particle size, phase evolution and carbon pick-up due to toluene decomposition were studied. Formation of single-phase high entropy carbide having face-centered cubic (FCC) crystal structure was confirmed by X-ray diffraction (XRD), electron backscattered diffraction (EBSD) and Selected area diffraction pattern (SAED) analysis of the sintered compacts. Transmission Kikuchi Diffraction images revealed presence of equiaxed nature of the grains. Transmission electron microscopy images revealed the presence of an intergranular phase at grain boundaries and triple junctions. 3D-Atom Probe Tomography studies showed uniform distribution of elements within the grains with some segregation of impurity elements Fe and Co to the grain boundaries indicating minor contribution of liquid phase sintering to densification. The grain size of single-phase sintered compacts ranged between 1.69 ± 0.60 μm to 4.6 ± 1.0 μm. A low sintering temperature and higher milling time resulted in finer grain size The microhardness was found to increase with milling time and C/M ratio. The microhardness, Young’s modulus and indentation fracture toughness lied between 2221 HV0.1 to 2732 HV0.1, 370 GPa to 473 GPa, 3.6 MPa.m1/2 to 4.4 MPa.m1/2, respectively. The highest microhardness and indentation fracture toughness was found to be 2732 ± 80 HV0.1 and 4.4 MPa.m1/2 on par with reported literature for other high entropy carbides.

Processing and microstructure development of reactive sintered (Ti-Zr-Nb-Hf-Ta)B2 + (Ti-Zr-Nb-Hf-Ta)C high-entropy ceramics

A novel dual-phase (Ti-Zr-Nb-Hf-Ta)B2 + (Ti-Zr-Nb-Hf-Ta)C high-entropy, compositionally complex composite was synthesized by reactive spark plasma sintering using commercial ZrB2, NbB2, HfB2, TaB2 and TiC powders as starting materials. The composite with high density, consists predominantly of boride (∼39.7 vol%) and carbide (∼56.4 vol%) phases and with residual amount of (Hf-Zr)O2. The microstructure is homogenous and relatively fine due to the reaction and solid solution coupling effect with average grain sizes of 3.4 μm and 2.2 μm of the boride and carbide phases, respectively. Large-area SEM analyses confirmed no microcracks or micropore formation and no presence of large grains or clusters. Investigation from micro to nano and atomic level, focused on local chemical composition and spatial distribution of constituent elements, revealed that Ti preferentially dissolves into the boride and all other elements to the carbide phase creating a (Ti0.82Zr0.04Nb0.08Hf0.03Ta0.03)B2 + (Ti0.49Zr0.12Nb0.13Hf0.11Ta0.15)C system. The analysis of grain and phase boundary interfaces revealed a continuous, <1.5 nm wide, segregation of impurity atoms of Fe and Co. Continuous (>20 nm) and atomically flat basal interfacial termination planes (001) decorated with monoatomic Zr enriched layer in the boride phase were observed. Triple points at grain and phase boundaries exhibit metal-rich composition due to impurities from the starting raw powders.

Kinetics-controlled reaction pathway and microstructure development of Ti3SiC2-TiC composite processed through reactive spark plasma sintering

Reactive spark plasma sintering of ternary Ti-Si-C system was performed using three different powder precursors systems 3Ti/Si/2C, 3Ti/SiC/C and 2Ti/TiC/Si, to explore the fundamental physics behind Ti3SiC2 MAX phase formation, its stability and microstructure development, and, finally linked with its hardening and contact induced damage tolerance. Phase evolution in Ti-Si-C system is a complex phenomenon, and, present experimental conditions never yield a phase pure Ti3SiC2 MAX phase, rather results in varying volume fractions of Ti3SiC2-(Tix,Si1-x)C solid solution due to non-equilibrium processing conditions exerted by SPS processing which restricts coherent site specific diffusional jumps and promotes the formation of (Ti, Si)C solid-solution instead of well reported non-stoichiometric TiCx. 3Ti/SiC/C precursor was the best candidate for processing composite with highest yields of Ti3SiC2. Phase evolution is guided by the free energy of formation of different phases and chemical affinity amongst the constituent elements rather than the equilibrium phase diagram of the Ti-Si-C system. Presence of free carbon, low temperature liquid phase and slow heating rate are the key requirements for forming phase pure Ti3SiC2, where excess free carbon reduces the stability of Ti3SiC2 via decarburization. Non-equilibrium processing conditions impart nano-precipitation of coherent hexagonal Ti3SiC2 precipitates within a cubic (Ti, Si)C matrix with a distinct orientation relation of (220)matrix ║(0004)precipitate and <114>matrix ║<2–1–10>precipitate that has never been reported, instead of growing highest density plane of hcp-on-fcc matrix. Coherency strain and fine interlocking microstructure of the as-processed composite experiences ≈36 % of enhancement in hardness followed by an improved contact damage for the as-processed composite.

Spark plasma sintering of hard wear‐resistant graphene nanoplatelet–reinforced TiB2 + SiC composites from TiC–B4C–SiC

AbstractGraphene nanoplatelet (GNP)–reinforced TiB2 + SiC composites were fabricated by reactive spark plasma sintering (SPS) from a TiC–B4C–SiC powder mixture with equal‐volume percentages, optimizing their SPS temperature and evaluating their unlubricated sliding wear against diamond. First, it is shown that during the heating ramp of the SPS cycle, TiC and B4C react according to the chemical reaction 2TiC + B4C → 2TiB2 + 3C, and that the thus‐formed C is graphenized as GNPs, leading to composites with microstructures consisting of a ceramic matrix of fine TiB2 and SiC grains with abundant randomly oriented GNPs at grain boundaries. It is also shown that this reactive SPS is optimal at 2000°C (under 75 MPa pressure and 5 min soaking), resulting in a very hard (∼28.5–29.9 GPa) and very tough (∼6.7(3) MPa m1/2) composite. And second, it is shown that these two properties and its proneness to develop an oxide tribolayer make this composite very resistant to unlubricated sliding wear against diamond (∼2.8(1)·108 (N m)/mm3), undergoing only very mild two‐body abrasion. Finally, opportunities for the fabrication of toughened and very hard ceramic composites for contact‐mechanical and tribological applications are discussed.

Phase and microstructure formation during reactive spark plasma sintering of AlxCoCrFeNi (x=0.3 and 1) high entropy alloys

This paper is one of the first studies focusing on phase and microstructure formation mechanisms during reactive sintering of AlxCoCrFeNi (x = 0.3, 1) high entropy alloys (HEAs). The alloys have been prepared by mechanical activation followed by spark plasma sintering (SPS). Both powders are subjected to gluing to the milling vials and the phenomenon intensifies with Al content, resulting in a more important mechanical alloying delay for the equiatomic composition. The temperature influence on phase and microstructure formation was investigated by SPS from 550 to 1100 °C. Al0.3CoCrFeNi reactive sintering led to a face-centered cubic (FCC) solid solution with a grain size around hundreds of nanometers with nanometric intergranular B2 precipitates which content and size reduced with the temperature increase. Grain growth was observed at prior particle boundaries due to dynamic recrystallization, a phenomenon that can be controlled through modification of the milling and sintering steps, leading thus to tailored grain sizes. For the AlCoCrFeNi composition, temperature increase favors secondary FCC formation and leads to sigma phase precipitation. A dual homogeneous-heterogeneous microstructure is obtained due to the important gluing leading to insufficient milling. The dynamic recrystallization at prior particle boundaries promotes also body-centered cubic (BCC) to FCC phase transition. Therefore, the proposed reactive sintering route allows to obtain, for the equiatomic composition, alloys exhibiting very fine microstructures, with higher FCC fraction content than by conventional metallurgy processes.

Correlative characterization of plasma etching resistance of various aluminum garnets

AbstractPlasma etching is a crucial step in semiconductor manufacturing. High cleanliness and wafer‐to‐wafer reproducibility in the etching chamber are essential in order to successfully achieve nanometer‐sized integrated functions on the wafer. The trend toward the application of more aggressive plasma compositions leads to higher demands on the plasma resistance of the materials used in the etching chamber. Due to its excellent etch resistance, yttrium aluminum garnet Y3Al5O12 (YAG) is starting to replace established materials like SiO2 or Al2O3 in this kind of application. In this study, reactive spark plasma sintering (SPS) was used to manufacture highly dense YAG ceramics from the respective oxides. In addition, yttrium was replaced with heavier lanthanoids (Er, Lu), intending to investigate the role of the A‐site cation in the garnet type structure on the plasma erosion behavior. The produced materials were exposed to fluorine‐based etching plasmas mimicking the conditions in the semiconductor manufacturing apparatus and the erosion behavior was characterized by atomic force microscopy (AFM), secondary ion mass spectrometry (SIMS), transmission electron microscopy (TEM), and profilometry. The induced chemical gradient in the samples is limited to a few nanometers below the surface, which makes its characterization challenging. For advanced analysis, we developed a correlative characterization method combining SIMS and scanning TEM (STEM)–energy‐dispersive spectroscopy (EDS) enabling us to examine the structural and chemical changes in the reaction layer locally resolved. In the case of lanthanoid aluminates, an altered reaction layer and reduced fluorine penetration compared to YAG were found. However, a correlation between the characteristics of the induced chemical gradient and the determined physical erosion rates was not evident.

Fabrication, microstructure, and properties of Dy‐doped (Y1−xDyx)3Si2C2 ceramics fabricated by in situ reactive spark plasma sintering

AbstractDysprosium (Dy)‐doped (Y1−xDyx)3Si2C2 (x = 0, 0.1, 0.3, 0.5) solid solution ceramics were successfully fabricated using an in situ reaction spark plasma sintering technology, for the first time. The effect of various Dy doping contents (x) on the microstructure, mechanical, and thermal properties of (Y1−xDyx)3Si2C2 ceramics was investigated. The (0 2 0) crystal plane spacing of (Y0.5Dy0.5)3Si2C2 was 7.813 Å, which was smaller than that of Y3Si2C2, due to the fact that the atomic radius of Dy is smaller than that of Y. The Dy doping facilitated the consolidation of (Y1−xDyx)3Si2C2, thus a highly dense (Y0.5Dy0.5)3Si2C2 ceramic material with a low open porosity of 0.14% was successfully obtained at a relatively low temperature of 1 200°C. As the content of Dy doping (x) increased from 0 to 0.5, the purity of (Y1−xDyx)3Si2C2 ceramics increased from 88.3 to 90.7 wt.%, while the grain size of (Y1−xDyx)3Si2C2 ceramics decreased from 0.59 to 0.46 µm. As a result, the Vickers hardness and thermal conductivity of the (Y0.5Dy0.5)3Si2C2 material was 7.1 GPa and 9.8 W·m−1·K−1, respectively.

On the potential of Transparent Rare-Earth-Free ZnAl2O4 Ceramics targeted at the UV-C to UV-B emission

Materials capable of emitting in the ultraviolet UV-C to UV-B spectral range have received considerable attention due to their potential applications in biophotonics, plant lighting, optical cleaning, sterilization, and disinfection. However, progress in the development of phosphors that emit in this short-wavelength range has been relatively sluggish. Most UV-C phosphors developed to date are based on hosts doped with the rare-earth cation Pr3+ due to its bright UV luminescence originating from the 4f15d1 → 4f2 interconfigurational transitions. In this study, we explore how the UV emission can be tailored to different wavelength ranges by developing rare-earth-free materials. Specifically, we demonstrate that UV-C to UV-B emission can be achieved in transparent ZnAl2O4 – based ceramics. For the first time, such transparent ceramics have been successfully produced with the help of reactive spark plasma sintering with SiO2 or LiF additives, which modified the process of grain growth resulting in an increase in the average grain size from 250 nm to 4 µm. Moreover, these additives also improved the optical transmission properties, with in-line transmission measurements at a wavelength of 550 nm reaching values of 50 % and nearly 65 % in the infrared region. Depending on the addition of SiO2 and LiF, the excitation by photons with energy exceeding 6.2 eV has generated the deep UV emission peaks in the range from 230 to 300 nm. Based on the analysis of the results of luminescence spectroscopy and EPR studies, the observed UV-C emission is suggested to originate from the excitons localised near oxygen vacancies. The number of vacancies is the highest in undoped ZnAl2O4 ceramics, whereas adding SiO2 and LiF suppresses their number and modifies their local environment due to changes in charge compensation, which in turn allows tuning the spectral position of the UV-C band. The quantum yield of the UV-C emission reached 5 % for undoped ZnAl2O4 ceramics. The sintered ZnAl2O4 transparent ceramic shows a versatile solution for next-generation rare-earth-free deep-UV devices.

The Microstructure, Mechanical, and Friction-Wear Properties of Boron Carbide-Based Composites with TiB2 and SiC Formed In Situ by Reactive Spark Plasma Sintering.

The paper presents the influence of the temperature of the sintering process on the microstructure and selected properties of boron carbide/TiB2/SiC composites obtained in situ by spark plasma sintering (SPS). The homogeneous mixture of boron carbide and 5% vol. Ti5Si3 micropowders were used as the initial material. Spark plasma sintering was conducted at 1700 °C, 1800 °C, and 1900 °C for 10 min after the initial pressing at 35 MPa. The heating and cooling rate was 200 °C/min. The obtained boron carbide composites were subjected to density measurement, an analysis of the chemical and phase composition, microstructure examination, and dry friction-wear tests in ball-on-disc geometry using WC as a counterpart material. The phase compositions of the produced composites differed from the composition of the initial powder mixture. Instead of titanium silicide, two new phases appeared: TiB2 and SiC. The complete disappearance of Ti5Si3 was accompanied by a decrease in the boron carbide content of the stoichiometry formula B13C2 and an increase in the content of TiB2, while the SiC content was almost constant. The relative density of the obtained boron carbide composites, as well as their hardness and resistance to wear, increased with the sintering temperature and TiB2 content. Unfortunately, the reactions occurring during sintering did not allow us to obtain composites with high density and hardness. The relative density was 76-85.2% of the theoretical one, while the Vickers hardness was in the range of 4-12 GPa. The mechanism wear of boron carbide composites tested in friction contact with WC was abrasive. The volumetric wear rate (Wv) of composites decreased with increasing sintering temperature and TiB2 content. The average value of coefficient of friction (CoF) was in the range of 0.54-0.61, i.e., it did not differ significantly from the value for B4C sinters.

Dual plate-like grains of (Ti, Zr)B2 and W2B5 toughened solid solution composites fabricated via in-situ reaction spark plasma sintering of (Ti, W)C and ZrB2 powders

Novel dual plate-like grains of (Ti, Zr)B2 and W2B5 toughened solid solution composites were fabricated by the in-situ reaction spark plasma sintering at 1800 °C using (Ti, W)C and ZrB2 powders. The composites were predominated and composed of the (Zr, Ti, W)C solid solutions and plate-like (Ti, Zr)B2. In the (Ti, W)C-ZrB2 reaction system, W promotes the anisotropic growth of (Ti, Zr)B2 grains, while Ti makes the formation reactions of WxBy thermodynamically feasible. When the addition of ZrB2 exceeds 40 mol%, W begins to be boronized into WxBy which is mainly composed of plate-like W2B5. The (Ti, W)C-50 mol% ZrB2 composite with dual plate-like grains of (Ti, Zr)B2 and W2B5 exhibited the best comprehensive mechanical properties of hardness of 26.5 GPa, flexural strength of 620 MPa, and fracture toughness of 6.6 MPa·m1/2, which provide a new approach for the enhanced toughness without the introducing of metal impurities.

B4C ceramics with increased dislocation density fabricated by reactive spark plasma sintering via carbon nanotubes–boron mixture

Boron carbide with high relative density was prepared in situ using spark plasma sintering. Research on the in-situ reaction of boron and carbon nanotubes reveals that the reaction exhibits high reactivity at 1200 °C. Beyond this temperature, increasing the external pressure was beneficial for particle rearrangement, gas release, and dislocation formation. The result of mechanical properties shows that, the flexural strength and fracture toughness of the boron carbides are 656 ± 9 MPa and 5.0 ± 0.3 MPa m1/2, respectively, when sintered at 1750 °C under continuous pressure ramping conditions–an increase of 64.1% and 46.6% compared to that prepared under constant pressure conditions. Increasing the magnitude of the external stress during the in-situ reaction process can also enhance the particle rearrangement efficiency, inducing the formation of twinning and stacking faults in boron carbide ceramics. High–density twinning and stacking faults dominated the toughening mechanisms of ceramic materials.

High-entropy boride-carbide based composite prepared by reactive spark plasma sintering

(Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)C-(Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2-SiC (HEBC-SiC) and (Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2-SiC (HEB-SiC) high-entropy boride-carbide composites were prepared by reactive spark plasma sintering with high-entropy carbides, B4C and Si as starting materials. Compared to monolithic (Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)C ceramics, both HEBC-SiC and HEB-SiC samples exhibited lower porosity and finer grain size due to mutual phase pinning effect. Also, the HEBC-SiC sample possessed superior mechanical properties compared to (Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)C ceramics, which demonstrated a hardness of 24.95 GPa (vs 20.18 GPa) and fracture toughness of 4.16 MPa·m1/2 (vs 2.94 MPa·m1/2). The present study provided a new approach to obtain dense (Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)C-(Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2-SiC composites with enhanced mechanical properties.

Structural and mechanical optimization of porous alumina structures fabricated by carbon sacrificial template

The Taguchi method is used to optimize the manufacture of porous alumina made through reactive spark plasma sintering and carbon sacrificial template. The goal is to design a new versatile procedure that allows the fabrication of porous alumina with tailored physical properties. The structural and mechanical properties taken as target parameters were the subtle combination of porosity and Young’s modulus of the human cortical bone: typical pore size ¿100μm, and Young’s modulus in the range of 3–30 GPa. The input factors of the Taguchi method are wt.% of carbon, sintering time, calcination heating rate, and final heat treatment. Hg porosimetry, electron microscopy, uniaxial compression and computer aided tomography were used for the characterization of the porosity, pore size distribution, pore interconnectivity, and Young’s modulus. Finally, according to the conclusions of the Taguchi analysis, the parameters of the process were changed for the fabrication of the new samples with optimized properties. Highly porous structures with 90% interconnectivity, Young modulus of 5.5 ± 1.1 GPa, and compression strength of 49 ± 20 MPa, were obtained, successfully emulating the targeted properties.

In-situ formation of CrB minor phase during reactive spark plasma sintering leads to the enhancement in the electrical transport performance of boron doped chromium disilicide

The present study focuses on the synergistic effect of substitution and in-situ composite formation of CrB in B-doped CrSi2. The samples of CrSi2.05-xBx have been synthesized in a single step employing reactive spark plasma sintering process (SPS) at 1423 K and 60 MPa. The diffusion process accelerates at high temperature and pressure and leads to the formation of the CrSi2 major phase and CrB minor phase. The X-ray diffraction technique was used to determine the phase purity of the synthesized samples. A field emission scanning electron microscope was used to examine the surface morphology of the CrSi1.85B0.20 sample. The elemental mapping confirms the presence of the CrB phase in the CrSi2 matrix. A significant enhanced power factor ≃ 1.95 × 10−3 W/mK2 at 473 K for CrSi1.85B0.20 was observed, which is primarily due to the formation of in-situ secondary metallic CrB phase which leads to the enhancement in the electrical conductivity. Further, the Vickers microhardness was also determined which is increasing with increasing B-concentration and exhibits a maximum value of ≃ 13 GPa for CrSi1.85B0.20. To comprehend the underlying physics of the enhancement of electronic transport characteristics of B-doped CrSi2, we employed density functional theory to calculate the projected density of states, electronic transport properties, and electronic band structure of B-doped CrSi2 at different temperatures and B-concentrations.

High-Entropy Diborides-Silicon Carbide Composites by Reactive and Non-Reactive Spark Plasma Sintering: A Comparative Study.

The reactive spark plasma sintering (R-SPS) method was compared in this work with the two-step SHS-SPS route, based on the combination of the self-propagating high-temperature synthesis (SHS) with the SPS process, for the fabrication of dense (Hf0.2Mo0.2Ti0.2Ta0.2Nb0.2)B2-SiC and (Hf0.2Mo0.2Ti0.2Ta0.2Zr0.2)B2-SiC ceramics. A multiphase and inhomogeneous product, containing various borides, was obtained at 2000 °C/20 min by R-SPS from transition metals, B4C, and Si. In contrast, if the same precursors were first reacted by SHS and then processed by SPS under the optimized condition of 1800 °C/20 min, the desired ceramics were successfully attained. The resulting sintered samples possessed relative densities above 97% and displayed uniform microstructures with residual oxide content <2.4 wt.%. The presence of SiC made the sintering temperature milder, i.e., 150 °C below that needed by the corresponding additive-free system. The fracture toughness was also markedly improved, particularly when considering the Nb-containing system processed at 1800 °C/20 min, whereas the fracture toughness progressively decreased (from 7.35 to 5.36 MPa m1/2) as the SPS conditions became more severe. SiC addition was found to inhibit the volatilization of metal oxides like MoO3 formed during oxidation experiments, thus avoiding mass loss in the ceramics. The benefits above also likely took advantage of the fact that the two composite constituents were synthesized in parallel, according to the SHS-SPS approach, rather than being produced separately and combined subsequently, so that strong interfaces between them were formed.

Novel (Ti, W)C–SiC–WSi2 ceramics fabricated via in situ reaction spark plasma sintering at 1600 °C

Novel (Ti, W)C–SiC–WSi2 ceramics were fabricated by in situ reaction spark plasma sintering (SPS) at 1600 °C using (Ti, W)C and Si powders. The effect of Si content on densification behavior, microstructures, and mechanical properties was investigated. The in situ reaction and the formation of carbon vacancies reduced the sintering temperature. The densification mechanism of (Ti, W)C-based ceramics transforms from reaction to grain-boundary sliding and diffusion. The WSi2 and primary SiC generated by in situ reactions are distributed along the grain boundaries and have a specific crystallographic orientation relationship. Intragranular secondary SiC formed because of rapid densification, grain-boundary diffusion, and (Ti, W1−y)C1−x particle migration. This multiscale particle-reinforced microstructure can improve the mechanical properties of (Ti, W)C ceramics, giving the TW10S (4.80 wt% SiC–5.01 wt% WSi2) good sintering performance, a fine-grained microstructure, high hardness (23.3 ± 1.6 GPa), and flexural strength (425 ± 24 MPa). The SiC and WSi2 produced through in situ reactions have exceptional intrinsic oxidation resistance, allowing the ceramics to achieve outstanding oxidation resistance.

Reactive spark plasma sintering of Si2N2O ceramic: Reaction process, microstructure, mechanical and dielectric properties

Dense Si2N2O ceramic was successfully prepared through the spark plasma sintering method at 1750 °C with nano-sized amorphous Si3N4 powder as raw material. The reaction sintering process, mechanical and dielectric properties of the Si2N2O ceramic were investigated in detail. The results revealed that the amorphous Si3N4 was initially crystallized to β-Si3N4, then oxidized to Si2N2O during the sintering process. With prolonging the dwell time, the grain orientation of Si2N2O gradually developed to the c-axis direction of the orthorhombic crystal. Meanwhile, the density of as-sintered ceramic was improved significantly, which greatly influenced the mechanical and dielectric properties of Si2N2O ceramic. In this work, the optimal dwell time of sintering process was 20 min, which is obviously shorter than the ordinary sintering methods. The Si2N2O ceramic fabricated at the above conditions exhibited the most favorable mechanical and dielectric properties with a bulk density of 2.80 ± 0.01 g cm−3, Vickers hardness of 13.1 ± 0.1 GPa, flexural strength of 214.1 ± 15.8 MPa, fracture toughness of 2.8 ± 0.3 MPa m1/2, and combined with low dielectric constant of around 3.5 to 4.5 at 8.2−12.4 GHz. Thus, the spark plasma sintering method is potentially regarded as a rapid way to prepare Si2N2O ceramic used as the structural and wave-transmitting functional material.