High‐Hardness Diamond Composite Consolidated by Spark Plasma Sintering

A high‐hardness diamond‐based composite was synthesized by spark plasma sintering (SPS) under 100 MPa, using SiC‐coated diamond powder prepared via chemical vapor deposition (CVD). SiC layers 20–40 nm were uniformly deposited on diamond powders by a rotary CVD technique. The SiC‐coated diamond powder was consolidated with SiO powder by SPS at the sintering temperature of 1873 K, resulting in the formation of fully compacted mosaic microstructure with the Vickers hardness of 36 GPa.     

ZrB2–SiC Nano‐Powder Mixture Prepared Using ZrSi2 and Modified Spark Plasma Sintering

ZrB₂–SiC nano‐powder mixture was synthesized using ZrSi₂ source material and a modified spark plasma sintering apparatus. The particle size of ZrB₂ and SiC was about 80 and 20 nm, respectively. The molecular‐level homogeneity of Zr/Si source and fast heating/cooling rate by SPS caused the formation of homogeneously intermixed nano‐powders. A strong exothermal reaction occurred at around 860°C, which caused strong agglomeration and growth of the synthesized powder mixture. The rapid reaction could be controlled by adding 20 wt% of NaCl, which acted as an inert filler.     

Effect of graphite content on properties of B4C‐W2B5 ceramic composites by in situ reaction of B‐Gr‐WC

Strip‐shaped W₂B₅ reinforced B₄C ceramic composites were prepared via in situ reaction of boron(B)‐graphite(Gr)‐WC system by powder metallurgy (P/M). In order to study the effect of the graphite content on the properties of the as‐fabricated ceramic composites, the powder mixture of B‐Gr‐WC with various amounts of Gr powder were blended and consolidated by spark plasma sintering (SPS). The sintering parameters were shown as following: sintering pressure was set as 30 MPa; The three‐step sintering temperature was 1100‐1550‐1700°C and the duration time was set as 5‐5‐6 minutes, respectively. In situ formed strip‐shaped W₂B₅ particles were dispersed homogeneously in B₄C matrix, which resulted in a remarkable improvement on the fracture toughness and mechanical properties. Appropriate 5vol% residual Gr in the composite shows positive effect on the mechanical properties which achieved an optimal counter‐balance of fracture toughness and hardness, the relative density was 99.8%, the Vickers hardness can reach 30.2 GPa, and the fracture toughness was 11.9 MPa·m^1/2 when the sintering temperature was set at 1700°C.     

Polymer precursor‐derived HfC–SiC ultrahigh‐temperature ceramic nanocomposites

Due to poor mechanical properties and antioxidation properties, etc of single phase ultrahigh‐temperature ceramics (UHTCs), the second phase such as SiC was usually introduced for improving those properties. Herein, a novel stratagem for synthesis of binary HfC–SiC ceramics has been presented. A Hf–O–Hf polymer as a HfO₂ precursor has been synthesized for preparing soluble HfC–SiC precursors with high solid content and low viscosity solutions without additional organic solvents. The structure of PHO was characterized by FTIR and ¹H‐NMR, the crystalline behavior and morphologies of polymer‐derived ceramics were identified by XRD, SEM‐EDS, and TEM. It was shown that PHO firstly transformed into HfO₂, and then reacted with in situ carbon derived from DVB and PCS thus producing cubic HfC through carbothermal reduction. In addition, the obtained HfC–SiC nanopowders exhibited spherical morphology with a diameter less than 100 nm, while the Hf, Si, and C are homogeneously distributed.     

Translucent Yttria‐ and Silica‐Doped Mullite Ceramics with Anisotropic Grains Produced by Spark Plasma Sintering

Translucent, high‐performance, mullite ceramics with anisotropic grains were prepared by the spark plasma sintering (SPS) of a powder mixture consisting of commercial mullite powder, which already contained small amounts of alumina (θ and α) and silica (cristobalite) (≤3 wt% in total), to which 2 and 1 wt% of yttria and amorphous silica was admixed, respectively. The combination of low‐viscosity Y₂O₃–Al₂O₃–SiO₂ transient liquid formation and SPS sintering provided enhanced densification, also provoking anisotropic grain growth (which became exaggerated after 20 min of SPS dwell time), at a relatively low sintering temperature of 1370°C. In this way, it was possible to meet the conflicting demands for obtaining a dense mullite ceramic with anisotropic grains, ensuring good mechanical properties, while preserving a noticeable light transmittance. In terms of mechanical and optical properties, the best results were obtained when SPS dwell times of 5 and 10 min were employed. The as‐sintered samples possessed densities in the range 3.16–3.18 g/cm³, anisotropic grains with an aspect ratio (AR) of 7 and a grain thickness of approximately 0.45 μm, a flexural strength between 350 and 420 MPa, a Vickers indentation toughness and a hardness of approximately 2.45 MPa·m^1/2 and 15 GPa, respectively, and an optical transmittance of between 30% and almost 50% in the IR range.     

Fabricating eco-friendly nanocomposites of SiC with morphologically-different nano-carbonaceous phases

A route based on aqueous colloidal processing followed by liquid-phase assisted spark-plasma-sintering (SPS) is described for fabricating eco-friendly nanocomposites of SiC with nano-carbonaceous phases (nanotubes, nanoplatelets, or nanoparticles). To this end, the conditions optimizing the aqueous colloidal co-dispersion of SiC nanoparticles, Y₃Al₅O₁₂ nanoparticles (acting as sintering additives), and carbon nanotubes (CNTs), graphene oxide (GO) nanoplatelets, or carbon black (CB) nanoparticles were first identified. Next, homogeneous powder mixtures were prepared by freeze-drying, and densified by liquid-phase assisted SPS, thus obtaining nanocomposites of SiC with CNTs, reduced GO (rGO) nanoplatelets, or pyrolized?+?graphitized CB (p?+?gCB) nanoparticles. It is also shown that these nanocomposites are dense and have a high hardness of ～20?GPa regardless of the nano-carbonaceous phase chosen, but are markedly tougher with CNTs and rGO (i.e., with high aspect ratio nano-carbonaceous phases). Finally, arguments are provided for the appropriate choice of nano-carbonaceous phases for engineering ceramic nanocomposites.     

Mechanical properties of nano-grain SiO2 glass prepared by spark plasma sintering

Silicon carbide (SiC) layers were deposited on silica (SiO₂) glass powder by rotary chemical vapor deposition (RCVD) to form SiO₂ glass (core)/SiC (shell) powder; this powder was consolidated by spark plasma sintering (SPS). SiO₂ glass powder with a particle size of 250 nm was coated with 5–10-nm-thick SiC layers. The resultant SiO₂ glass (core)/SiC (shell) powder was consolidated to form a nano-grain SiO₂ glass composite at a relative density above 90% by SPS in the sintering temperature range of 1573–1823 K. The Vickers hardness and fracture toughness of the SiO₂ glass composite at 1723 K were found to be 14.2 GPa and 5.4 MPa m^1/2, respectively.     

Fabrication and properties of Cf/ZrC‐SiC‐based composites by an improved reactive melt infiltration

C_f/ZrC‐SiC composites with a density of 2.52 g/cm³ and a porosity of 1.68% were fabricated via reactive melt infiltration (RMI) of Si into nano‐porous C_f/ZrC‐C preforms. The nano‐porous C_f/ZrC‐C preforms were prepared through a colloid process, with a ZrC “protective coating” formed surrounding the carbon fibers. Consequently, highly dense C_f/ZrC‐SiC composites without evident fiber/interphase degradation were obtained. Moreover, abundant needle‐shaped ZrSi₂ grains were formed in the composites. Benefiting from this unique microstructure, flexural strength, and elastic modulus of the composites are as high as 380 MPa and 61 GPa, respectively, which are much higher than C_f/ZrC‐SiC composites prepared by conventional RMI.     

High Hardness and Ductile Mosaic SiC/SiO2 Composite by Spark Plasma Sintering

SiC powder was coated with SiO₂ layer by chemical vapor deposition, and the SiC(core)/SiO₂(shell) composite powder was consolidated to a SiC/SiO₂ composite with a mosaic microstructure by spark plasma sintering (SPS) at 1923 K for 1.8 ks. The SiC(core)/SiO₂(shell) powder with a 80–100 nm thick SiO₂ layer resulted in a SiC/SiO₂ composite with a relative density of 97% and hardness and fracture toughness of 17.1 GPa and 8.4 MPa m^1/2, respectively.     

Mechanical,electrical and thermal properties of HfC-HfB2-SiC ternary eutectic composites prepared by arc melting

HfC-HfB₂-SiC composites were prepared by arc melting using HfC, HfB₂ and SiC powder as raw materials. The ternary eutectic composition of 16HfC-17HfB₂-67SiC (mol%) was first identified, showing a complicated maze microstructure of HfC, HfB₂ and SiC approximately 500 nm in thickness. The eutectic temperature of the HfC-HfB₂-SiC composite was nearly 2760 K. The Vickers hardness and fracture toughness of the HfC-HfB₂-SiC ternary eutectic composite were 20.8 GPa and 7.7 MPa m^1/2, respectively. With increasing temperature from 300 to 800 K, the electrical conductivity decreased from 8.8 × 10⁵ to 4.3 × 10⁵ Sm⁻¹, whereas the thermal conductivity increased from 28 to 32 W m⁻¹ K⁻¹.     

Reaction-bond composite synthesis of SiC-TiB2 by spark plasma sintering/field-assisted sintering technology (SPS/FAST)

High-density SiC-TiB₂ composites were fabricated using the displacement reaction spark plasma sintering/field-assisted sintering technology (SPS/FAST) and SiC, B₄C, TiC, and Si powders. The reaction process was performed in a narrow time frame compared hot pressing. The SiC-TiB₂ composites were sintered with precursor SiC at various pressures to determine the effects of processing with SPS/FAST. The composites completed synthesis during SPS/FAST processing, which occurs more quickly than hot pressing. SEM, STEM, and Raman spectroscopy are used to show the conversion and microstructure. The composite of 53.6 wt.% SiC and 46.4 wt.% TiB₂ has 99 % theoretical density, hardness of 26.4 GPa, and fracture toughness of 5.12 MPa m^1/2.     

Effect of temperature on the structure and mechanical properties of SiC–TiB2 composite ceramics by solid-phase spark plasma sintering

SiC composite ceramics have good mechanical properties. In this study, the effect of temperature on the microstructure and mechanical properties of SiC–TiB₂ composite ceramics by solid-phase spark plasma sintering (SPS) was investigated. SiC–TiB₂ composite ceramics were prepared by SPS method with graphite powder as sintering additive and kept at 1700 °C, 1750 °C, 1800 °C and 50 MPa for 10min.The experimental results show that the proper TiB₂ addition can obviously increase the mechanical properties of SiC–TiB₂ composite ceramics. Higher sintering temperature results in the aggregation and growth of second-phase TiB₂ grains, which decreases the mechanical properties of SiC–TiB₂ composite ceramics. Good mechanical properties were obtained at 1750 °C, with a density of 97.3%, Vickers hardness of 26.68 GPa, bending strength of 380 MPa and fracture toughness of 5.16 MPa m^1/2.     

High‐Strength B4C–TaB2 Eutectic Composites Obtained via In Situ by Spark Plasma Sintering

The in situ synthesis/consolidation of B₄C–TaB₂ eutectic composites by spark plasma sintering (SPS) is reported. Samples for the evaluation of bending strength were cut from specimens with diameters of 30 mm. The sample prepared for the three‐point flexural strength test had fibers of tantalum diboride with diameter of 1.3 ± 0.4 μm distributed in the B₄C matrix, thereby reducing composites brittleness and yielding an indentation fracture toughness of up to 4.5 MPa·m^1/2. Furthermore, the Vickers hardness of B₄C–TaB₂ eutectics formed by SPS was as high as 26 GPa at an indentation load of 9.8 N. The flexural strength of the B₄C–TaB₂ system has been reported for the first time. Some steps were identified in the load–displacement curve, suggesting that micro‐ and macrocracking occurred during the flexural test. Ceramic composites with a eutectic structure exhibited a room‐temperature strength of 430 ± 25 MPa. Compared with other eutectic composites of boron carbide with transition‐metal diborides, room‐temperature strength the B₄C–TaB₂ was 40% higher than that of B₄C–TiB₂ ceramics, demonstrating advantage of the in situ synthesis/consolidation of eutectic composites by SPS.     

Microstructural,electrical, and mechanical properties of conductive SiC ceramics fabricated by spark plasma sintering

Nitrogen (N)-doped conductive silicon carbide (SiC) of various electrical resistivity grades can satisfy diverse requirements in engineering applications. To understand the mechanisms that determine the electrical resistivity of N-doped conductive SiC ceramics during the fast spark plasma sintering (SPS) process, SiC ceramics were synthesized using SPS in an N₂ atmosphere with SiC powder and traditional Al₂O₃–Y₂O₃ additive as raw materials at a sintering temperature of 1850–2000°C for 1–10 min. The electrical resistivity was successfully varied over a wide range of 10⁻³–10¹ Ω cm by modifying the sintering conditions. The SPS-SiC ceramics consisted of mainly Y–Al–Si–O–C–N glass phase and N-doped SiC. The Y–Al–Si–O–C–N glass phase decomposed to an Si-rich phase and N-doped Y_xSi_yC_z at 2000°C. The Vickers hardness, elastic modulus, and fracture toughness of the SPS-SiC ceramics varied within the ranges of 14.35–25.12 GPa, 310.97–400.12 GPa, and 2.46–5.39 MPa m^1/2, respectively. The electrical resistivity of the obtained SPS-SiC ceramics was primarily determined by their carrier mobility.     

Synthesis and Properties of MoSi2–MoB–SiC Ceramics

MoB and SiC particulate reinforced MoSi₂ matrix composites were synthesized in situ from Mo, Si, and B₄C powder mixtures by self‐propagating high‐temperature synthesis (SHS). The SHS MoSi₂–MoB–SiC products were vacuum hot‐pressed (HPed) at 1400°C for 90 min to fabricate high‐density (> 97.5% relative density) bulk composites. Microstructure refinement and improvements in the Vickers hardness and fracture toughness of the HPed composites were observed with increasing B₄C content in the reaction mixture. The HPed composite of composition MoSi₂–0.4MoB–0.1SiC exhibited grain size of 1–5 μm, Vickers hardness of 12.5 GPa, bending strength of 537 MPa, and fracture toughness of 3.8 MPa.m^1/2. These excellent mechanical properties indicate that MoB and SiC particulate reinforced MoSi₂ composites could be promising candidates for structural applications.     

Ferrite‐Based Exchange‐Coupled Hard–Soft Magnets Fabricated by Spark Plasma Sintering

Ferrite‐based, hard‐soft magnetic nanocomposites with the composition (100%?x)SrFe₁₂O₁₉–xCoFe₂O₄, where x = 5, 10, and 15 wt%, were prepared by mixing the constituent powders, followed by spark plasma sintering. In order to control the particle size of the constituent materials, the SrFe₁₂O₁₉ and CoFe₂O₄ powders were synthesized using the hydrothermal method, mixed and then consolidated with spark plasma sintering. The conditions during the spark plasma sintering process (sintering temperature, time, and applied pressure) were varied in order to prepare composites with a high density and exchange‐coupled hard and soft magnetic phases, leading to an increase in the maximum energy product, when compared with pure SrFe₁₂O₁₉. The microstructural analysis revealed that the relative density of the sintered composite exceeded 90% of the theoretical value and that the CoFe₂O₄ was uniformly distributed in the SrFe₁₂O₁₉ matrix. Magnetic measurements of the sintered composites showed a single‐phase magnetic behavior. When compared with the single‐phase SrFe₁₂O₁₉ used in this study, the SPS composites exhibited a 22% increase in the maximum energy product (26.1 kJ/m³).     

In Situ Fabrication of B4C–NbB2 Eutectic Composites by Spark–Plasma Sintering

This contribution reports, for the first time, the sintering, microstructure and properties of in situ synthesized/consolidated eutectic composites by spark–plasma sintering (SPS). SPS involves a number of processing parameters that may be used to tailor the composition of eutectic composites. It was shown that pressure may be used as a means of controlling the eutectic formation. By changing the pressure, temperature and composition, we propose a processing route that results in the in situ formation of strengthened eutectic composites, consisting of a matrix (B₄C, and B₄C–NbB₂ composite) and also containing regularly distributed whiskers of NbB₂. The composites with the eutectic composition of 35 mol.% NbB₂ obtained by SPS exhibit a high Vickers hardness (26–27 GPa) and indentation fracture toughness (~6 MPa·m^1/2).     

Preparation and high‐temperature behavior of HfC–SiC nanocomposites derived from a non‐oxygen single‐source‐precursor

A single‐source precursor for the preparation of HfC‐SiC ceramics was synthesized via a Grignard reaction using bis(cyclopentadienyl)hafnium(IV) dichloride, trans‐1,4‐dibromo‐2‐butene, and (chloromethyl)trimethylsilane as raw materials. The composition, structure, pyrolysis process and high‐temperature behavior of the precursor were investigated. The results show that the precursor with a backbone comprising Hf–C, Si–C and CH=CH groups exhibits good solubility in common solvents, such as tetrahydrofuran, dimethylbenzene, and chloroform. Pyrolysis of the precursor at 1000°C yielded a microcrystalline HfC phase with a ceramic yield of 63.86 wt%. The pyrolytic products at 1600°C were HfC–SiC nanocomposite ceramics, which exhibited good thermal stability up to 2400°C. The formation of a (Hf,Si)C solid‐solution would be beneficial for densification during the sintering process. The non‐oxygen structure, high ceramic yield, homogeneous composition and excellent high‐temperature behavior of the pyrolytic products make the as‐prepared precursor a promising material for the preparation of high‐performance ultra‐high‐temperature ceramics.     

Mechanical Properties and Microstructure of Nano-SiC–Al2O3 Composites Densified by Spark Plasma Sintering

Heterogeneous precipitation method has been used to produce 5 vol% SiC–Al₂O₃ powder, from aqueous suspension of nano-SiC, aqueous solution of aluminium chloride and ammonia. The resulting gel was calcined at 700°C. Nano-SiC–Al₂O₃ composites were densified using spark plasma sintering (SPS) process by heating to a sintering temperature at 1350, 1400, 1450, 1500 and 1550°C, at a heating rate of 600 °/min, with no holding time, and then fast cooling to 600°C within 2–3 min. High density composites could be achieved at lower sintering temperatures by SPS, as compared with that by hot-press sintering process. Bending strength of 5 vol% SiC–Al₂O₃ densified by SPS at 1450°C reached as high as 1000 MPa. Microstructure studies found that the nano-SiC particles were mainly located within the Al₂O₃ grains and the fracture mode of the nanocomposites was mainly transgranular fracture.     

Development of WC–ZrO2 Nanocomposites by Spark Plasma Sintering

In the present work, we report the processing of ultrahard tungsten carbide (WC) nanocomposites with 6 wt% zirconia additions. The densification is conducted by the spark plasma sintering (SPS) technique in a vacuum. Fully dense materials are obtained after SPS at 1300°C for 5 min. The sinterability and mechanical properties of the WC–6 wt% ZrO₂ materials are compared with the conventional WC–6 wt% Co materials. Because of the high heating rate, lower sintering temperature, and short holding time involved in SPS, extremely fine zirconia particles (∼100 nm) and submicrometer WC grains are retained in the WC–ZrO₂ nanostructured composites. Independent of the processing route (SPS or pressureless sintering in a vacuum), superior hardness (21–24 GPa) is obtained with the newly developed WC–ZrO₂ materials compared with that of the WC–Co materials (15–17 GPa). This extremely high hardness of the novel WC–ZrO₂ composites is expected to lead to significantly higher abrasive-wear resistance.