Anisotropy of functional properties of SiC composites with GNPs,GO and in-situ formed graphene

This paper reports on anisotropy of functional properties of different silicon carbide-graphene composites due to preferential orientation of graphene layers during sintering. Dense silicon carbide/graphene nanoplatelets (SiC/GNPs) and silicon carbide/graphene oxide (SiC/GO) composites were sintered in the presence of yttria (Y₂O₃) and alumina (Al₂O₃) sintering additives at 1800 °C in vacuum by the rapid hot pressing (RHP) technique. It is found that electrical conductivity of SiC/GNPs and SiC/GO composites increases significantly in the perpendicular direction to the RHP pressing axis, reached up to 1775 S/m in the case of SiC/GO (for 3.15 wt.% of rGO). Also, thermal diffusivity was found to increase slightly by the addition of GNPs in the SiC/GNPs composites in the perpendicular direction to the RHP pressing axis. But, in the parallel direction, the addition of GNPs showed a negative effect. The formation of graphene domains was observed in reference sample SiC-Y₂O₃-Al₂O₃ sintered by RHP, without any addition of graphene. Their presence was confirmed indirectly by increasing electrical conductivity about three orders of magnitude in comparison to the reference sample sintered by conventional hot press (HP). Raman, SEM and TEM analysis were used for direct evidence of presence of graphene domains in RHP reference sample.     

Alumina/zirconia composites toughened by the addition of graphene flakes

The effect of added graphene flakes on the mechanical properties of a composite containing 20 wt% Al₂O₃ and 80 wt% ZrO₂ (stab. 3 mol% Y₂O₃) was studied. To obtain samples, a commercial ceramic powder produced by Tosoh (Japan), and graphene oxide (GO) made at the Institute of Electronic Materials Technology (Poland) were used. The obtained composites were based on aqueous mixtures of both components. After drying, they were sintered in an uniaxial pressure (HP) furnace. The composites contained from 0% to 3% of GO by weight. Results showed the influence of GO content i.e. fracture toughness has a maximum for 0.02% GO (increase by 42% in comparison to GO-free matrix) and afterwards decreased, strength decreased in the whole GO content range. Young's modulus and Vickers hardness remained constant up to 0.2% GO, and then decreased.     

Comparison of the homemade and commercial graphene in heightening mechanical properties of Al2O3 ceramic

Graphene has been successfully fabricated by a novel method, using graphite powder and NMP (N-Methyl Pyrrolidone) as the raw materials based on the principles of liquidoid exfoliation and mechanical milling. SEM, TEM and Raman spectrum were utilized to characterize the morphology of the homemade graphene, illustrating the few defects and rare layers were endowed in this study. Afterwards, the homemade and commercial graphene were doped into Al₂O₃ powder with the mass ratio of 0%, 1%, 2%, and 3% to reinforce the mechanical properties of the matrix. The composites were processed at 1600 °C, pressure of 30 MPa and soaking time of 1 h by vacuum hot pressing. The test results illustrated the bending strength and fracture toughness tended to be intensive at first and subdued afterwards, achieving the optimal performance of 625.4±18.2 MPa and 6.07±0.22 MPa m^1/2 at 2 wt% prepared graphene additive, and the commercial grapheme owned the best heighten effect in 3 wt% graphene/Al₂O₃ composites. Compared to the blank Al₂O₃ sintered samples, the graphene/Al₂O₃ specimens (both prepared and commercial additive) behaved evident increase in mechanical properties, even upon 30% enhanced in fracture toughness and bending strength generally by the prepared grapheme. Moreover, the prepared graphene had better improvement effect than commercial graphene in enhancing mechanical properties of Al₂O₃ ceramic.     

Grafting of epoxy chains onto graphene oxide for epoxy composites with improved mechanical and thermal properties

Epoxy composites filled with both graphene oxide (GO) and diglycidyl ether of bisphenol-A functionalized GO (DGEBA–f–GO) sheets were prepared at different filler loading levels. The correlations between surface modification, morphology, dispersion/exfoliation and interfacial interaction of sheets and the corresponding mechanical and thermal properties of the composites were systematically investigated. The surface functionalization of DGEBA layer was found to effectively improve the compatibility and dispersion of GO sheets in epoxy matrix. The tensile test indicated that the DGEBA–f–GO/epoxy composites showed higher tensile modulus and strength than either the neat epoxy or the GO/epoxy composites. For epoxy composite with 0.25 wt% DGEBA–f–GO, the tensile modulus and strength increased from 3.15 ± 0.11 to 3.56 ± 0.08 GPa (∼13%) and 52.98 ± 5.82 to 92.94 ± 5.03 MPa (∼75%), respectively, compared to the neat epoxy resin. Furthermore, enhanced quasi-static fracture toughness (K_IC) was measured in case of the surface functionalization. The GO and DGEBA–f–GO at 0.25 wt% loading produced ∼26% and ∼41% improvements in K_IC values of epoxy composites, respectively. Fracture surface analysis revealed improved interfacial interaction between DGEBA–f–GO and matrix. Moreover, increased glass transition temperature and thermal stability of the DGEBA–f–GO/epoxy composites were also observed in the dynamic mechanical properties and thermo-gravimetric analysis compared to those of the GO/epoxy composites.     

Development and evaluation of TiB2–AlN ceramic composites sintered by spark plasma

Titanium diboride (TiB₂) is a ceramic material with high mechanical resistance, chemical stability, and hardness at high temperatures. Sintering this material requires high temperatures and long sintering times. Non-conventional sintering techniques such as spark plasma sintering (SPS) can densify materials considered difficult to sinter. In this study, TiB₂–AIN (aluminum nitride) composites were sintered by using the SPS technique at different sintering temperatures (1500 °C, 1600 °C, 1700 °C, 1800 °C, and 1900 °C). x-ray diffraction was used to identify the phases in the composites. mechanical properties such as hardness and indentation fracture toughness was obtained using a vickers indenter. Different toughening mechanisms were identified, and good densification results were obtained using shorter times and lower temperatures than those previously reported.     

Spark plasma sintered BaTiO3/graphene composites for thermoelectric applications

The viability of spark plasma sintered graphene/barium titanate ceramic matrix composites as thermoelectric materials is investigated. The temperature dependence of electrical conductivity, thermal conductivity and Seebeck coefficient was analyzed. The addition of low amounts of graphene oxide combined with the spark plasma sintering process increases electrical conductivity of pure BaTiO₃ several orders of magnitude, whereas the thermal conductivity shows only a moderate enhancement. The composites display a semiconducting behaviour, with the resistivity decreasing with increasing temperature and following a thermally activated temperature dependence at high T. A strong dependence of ZT figure of merit with the graphene concentration and the measurement temperature was found. Optimal values are found for 1.7 wt% graphene oxide at the maximum experimental temperature (600 K).     

HfB2-CNTs composites with enhanced mechanical properties prepared by spark plasma sintering

HfB₂-x vol%CNTs (x=0, 5, 10, and 15) composites are prepared by spark plasma sintering. The influence of CNTs content and sintering temperature on densification, microstructure and mechanical properties is studied. Compared with pure HfB₂ ceramic, the sinterability of HfB₂-CNTs composites is remarkably improved by the addition of CNTs. Appropriate addition of CNTs (10 vol%) and sintering temperature (1800 °C) can achieve the highest mechanical properties: the hardness, flexural strength and fracture toughness are measured to be 21.8±0.5 GPa, 894±60 MPa, and 7.8±0.2 MPa m^1/2, respectively. This is contributed to the optimal combination of the relative density, grain size and the dispersion of CNTs. The crack deflection, CNTs debonding and pull-out are observed and supposed to exhaust more fracture energy during the fracture process.     

Improvement of electrical conductivity of silicon nitride/carbon nano-fibers composite using magnesium silicon nitride and ytterbium oxide as sintering additives

In order to find out the influence of sintering additives on the electrical conductivity of Si₃N₄-based ceramics composites with dispersed carbon nano-fibers (CNFs) two different mixtures of sintering additives were tested – Al₂O₃/Yb₂O₃ and MgSiN₂/Yb₂O₃, respectively. Optimization of hot-pressing conditions was performed for each mixture. The results show that the electrical conductivity can be effectively increased up to 1315 S/m by replacement of traditional sintering aid – alumina, with magnesium silicon nitride, while the mechanical properties remained on the same level. Other advantages of using MgSiN₂ instead of alumina are the preservation of higher amounts of CNFs in the ceramic composite and lower densification temperature (1500 °C) compared to samples sintered with alumina-based sintering aids (1550 °C).     

Improvement of wetability,sinterability, mechanical and electrical properties of Al2O3-Ni nanocomposites prepared by mechanical alloying

The wetability improvement and particle size reduction of alumina/Ni composites through mechanical alloying were addressed. Their effect on the sinterability (at high temperature), mechanical and electrical properties were studied. Al₂O₃ matrix nanocomposites reinforced with different volume fractions of Ni up to 10 vol% were prepared by mechanical alloying. The milled powders were cold pressed and sintered at different firing temperatures up to 1600 °C. The morphology of powders and the microstructure of sintered bodies were investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), respectively. Furthermore, relative density, apparent porosity, mechanical properties and electrical resistivity of the sintered composites were investigated. The results revealed that Al₂O₃ matrix was successfully coated with Ni thin film through mechanical alloying; the thickness of coat was increased with increasing the Ni content. Moreover, the increasing of both Ni content and sintering temperature up 1600 °C, led to a remarkable increase in the relative density and facture toughness of the sintered specimen. On the other hand, microhardness and elastic modulus were decreased with increasing of Ni content, while they increased significantly with the increase of sintering temperature. The electrical resistivity was decreased with increasing Ni content and sintering temperature.     

Sintering behaviour of silicon carbide matrix composites reinforced with multilayer graphene

The scope of this paper includes preparation and characterisation of dense silicon carbide matrix composites reinforced with multilayer graphene (MLG). Application of graphene as a reinforcement phase should simultaneously improve mechanical properties of SiC matrix composites and act as one of the sintering activators. In the present work the mechanical properties and the microstructure changes of samples sintered with different additions of graphene (0.5, 1, 2, 3, 4 wt%) and boron (0.3, 1 and 2 wt%) were examined. The composites were consolidated at two different temperatures (1800 °C and 1900 °C) using the Spark Plasma Sintering method (SPS). Reference samples with the addition of graphite as a source of carbon (1 and 3 wt%) were also sintered in the same conditions. The abovementioned amounts of graphite are an optimal content which is essential to obtain high density of samples [1], [2], [3], [4], [5], [6], [7], [8], [9]. The influence of MLG on density, mechanical properties and phase structure of the sintered samples were investigated. A high rate of densification for the composites with 0.3 wt% of B and 1 wt% of MLG sintered at 1900 °C was observed. Moreover, these composites showed the highest average of microhardness (2663 HV0.5) and single-phase structure.     

Sintering behaviour and properties of magnesium orthosilicate-hydroxyapatite ceramic

The effect of pressureless sintering on the properties of magnesium orthosilicate-hydroxyapatite (MO-HA) ceramic has been studied. The amount of MO composition in the green body was varied from 10 wt% to 50 wt% through mechanical ball milling and was subsequently sintered at varying temperatures in air atmosphere from 1000 °C to 1300 °C for 2 h. The magnesium orthosilicate phase was stable during sintering but the hydroxyapatite phase decomposed to tricalcium phosphate. The MO-HA composites generally exhibited lower mechanical properties across all the investigated composition. Nevertheless, a high fracture toughness of 2.5 MPam^1/2 was recorded for sintered body that contained 20 wt% MO. This finding indicates the potential of this ceramic composite to be used for biomedical applications.     

Fabrication and properties of reduced graphene oxide reinforced yttria-stabilized zirconia composite ceramics

Fully dense yttria-stabilized zirconia (YSZ) ceramics reinforced with reduced graphene oxide (RGO) were fabricated by spark plasma sintering (SPS), and their electrical, thermal, and mechanical properties were investigated. Graphene oxide (GO) was exfoliated by a short sonification in dimethylformamide (DMF)/water solution and uniformly mixed with ZrO₂ powders. The microstructure of the composites showed that undamaged RGO sheets were homogeneously distributed throughout matrix grains. The electrical conductivity of YSZ composites drastically increased with the addition of RGO, and it reached 1.2 × 10⁴ S/m at 4.1 vol.%. However, the thermal diffusivity increased only 12% with RGO addition. The hardness decreased slightly with RGO addition, whereas the fracture toughness significantly increased from 4.4 to 5.9 MPa^1/2. The RGO pull-out and crack bridging contributed to the improved fracture toughness.     

The effect of graphene nanoplatelets on the thermal and electrical properties of aluminum nitride ceramics

The thermal conductivity (κ) of AlN (2.9 wt.% of Y₂O₃) is studied as a function of the addition of multilayer graphene (from 0 to 10 vol.%). The κ values of these composites, fabricated by spark plasma sintering (SPS), are independently analyzed for the two characteristic directions defined by the GNPs orientation within the ceramic matrix; that is to say, perpendicular and parallel to the SPS pressing axis. Conversely to other ceramic/graphene systems, AlN composites experience a reduction of κ with the graphene addition for both orientations; actually the decrease of κ for the in-plane graphene orientation results rather unusual. This behavior is conveniently reproduced when an interface thermal resistance is introduced in effective media thermal conductivity models. Also remarkable is the change in the electrical properties of AlN becoming an electrical conductor (200 S m⁻¹) for graphene contents above 5 vol.%.     

Spark plasma sintering of silicon nitride/barium aluminum silicate composite

Si₃N₄ based composites were successfully sintered by spark plasma sintering using low cost BaCO₃, SiO₂ and Al₂O₃ as additives. Powder mixtures were sintered at 1600–1800 °C for 5 and 10 min. Displacement-temperature-time (DTT) diagrams were used to evaluate the sintering behavior. Shrinkage curve revealed that densification was performed between 1100 and 1700 °C. The specimen sintered at 1700 °C showed the maximum relative density (99.8±0.1%), flexural strength (352±16 MPa), Vickers harness (11±0.1 GPa) and toughness (5.6±0.05 MPa m^1/2).     

Graphene for tough and electroconductive alumina ceramics

A simple, fast and upscalable method is described to produce graphene/alumina (G/Al₂O₃) composites by spark plasma sintering (SPS) with a significant improvement on both mechanical and electrical properties of monolithic Al₂O₃. Graphene oxide (GO) was mixed with Al₂O₃ using a colloidal method obtaining an excellent dispersion of GO in the alumina matrix. The material was consolidated by SPS that allowed, in one-step, the in situ reduction of the GO during the sintering process. A detailed Raman analysis was found to be very useful to study the orientation of the graphene in the composite and to evaluate and optimise its thermal reduction. Graphene platelets acted as elastic bridges avoiding crack propagation and providing this material with a crack bridging reinforcement mechanism. A very low graphene loading (0.22 wt%) led to a 50% improvement on the mechanical properties of the alumina and to an increase of the electrical conductivity up to eight orders of magnitude.     

Preparation and characterization of Si3N4-based composite ceramic tool materials by microwave sintering

Si₃N₄-based composite ceramic tool materials with (W,Ti)C as particle reinforced phase were fabricated by microwave sintering. The effects of the fraction of (W,Ti)C and sintering temperature on the mechanical properties, phase transformation and microstructure of Si₃N₄-based ceramics were investigated. The frictional characteristics of the microwave sintered Si₃N₄-based ceramics were also studied. The results showed that the (W,Ti)C would hinder the densification and phase transformation of Si₃N₄ ceramics, while it enhanced the aspect-ratio of β-Si₃N₄ which promoted the mechanical properties. The Si₃N₄-based composite ceramics reinforced by 15 wt% (W,Ti)C sintered at 1600 °C for 10 min by microwave sintering exhibited the optimum mechanical properties. Its relative density, Vickers hardness and fracture toughness were 95.73 ± 0.21%, 15.92 ± 0.09 GPa and 7.01 ± 0.14 MPa m^1/2, respectively. Compared to the monolithic Si₃N₄ ceramics by microwave sintering, the sintering temperature decreased 100 °C,the Vickers hardness and fracture toughness were enhanced by 6.7% and 8.9%, respectively. The friction coefficient and wear rate of the Si₃N₄/(W,Ti)C sliding against the bearing steel increased initially and then decreased with the increase of the mass fraction of (W,Ti)C., and the friction coefficient and wear rate reached the minimum value while the fraction of (W,Ti)C was 15 wt%.     

Preparation and characterization of novel bioactive dicalcium silicate ceramics

The beta- and gamma-dicalcium silicate (β- and γ-Ca₂SiO₄) ceramics were prepared by sintering β-Ca₂SiO₄ greens at 1100, 1300, and 1450 °C, respectively, after compacting with cold isostatic pressure. The phase transition from β- to γ-phase of polymorphic ceramics occurred at 1100–1300 °C. Bending strength and Vickers hardness of β-Ca₂SiO₄ ceramic sintered at 1100 °C were only 25.6 ± 3.8 MPa and 0.41 ± 0.05 GPa. In contrast, the mechanical properties of the γ-Ca₂SiO₄ were improved remarkably when the ceramics were sintered at 1450 °C, corresponding to bending strength, 97.1 ± 6.7 MPa; Vickers hardness, 4.34 ± 0.35 GPa, respectively. The ceramics were soaked in the simulated body fluid (SBF) for various periods were characterized by SEM, XRD, FTIR, and EDS analysis, and the results indicated that the carbonated hydroxyapatite (CHA) was formed on the surface of the ceramics within 3 days. In addition, cell attachment assay showed that the ceramics supported the mesenchymal stem cells adhesion and spreading, and the cells established close contacts with the ceramics after 1 day of culture. These findings indicate that the γ-Ca₂SiO₄ ceramic possesses good bioactivity, biocompatibility and mechanical properties, and might be a promising bone implant material.     

Electrically conductive porous alumina/graphite composite synthesized by starch consolidation with reductive sintering

This paper reports a facile and environment-friendly process to synthesize electrically conductive porous alumina/graphite composites by starch consolidation technique followed by reductive sintering. Green ceramic composites were consolidated with different starches and sintered at different temperatures in an argon atmosphere. Electrical measurements, carbon contents and Raman analyses of carbon structures determined an optimal sintering temperature of 1700 °C, which lead to a uniform formation of conductive graphitic networks at an optimal concentration of about 3.8 vol% in the porous composites. These carbon networks resulted into porous composites having high electrical conductivities measured in the range from 3 to 7 S/cm, which depended on the starch types and their porous properties. Correspondingly, the bulk porosities of the sintered composites were measured from 42 to 46%, with rounded micropores having diameters ranging from 14 to 39 μm. These porous properties of the sintered composites offer promising applications for conductive membrane and porous electrode.     

Properties of Si3N4–TiN composites fabricated by spark plasma sintering by using a mixture of Si3N4 and Ti powders

Si₃N₄–TiN composites were successfully fabricated via planetary ball milling of 70 mass% Si₃N₄ and 30 mass% Ti powders, followed by spark plasma sintering (SPS) at 1250–1350 °C. The sintering mechanism for SPS was a hybrid of dissolution–reprecipitation and viscous flow. The electrical resistivity decreased with increasing sintering temperature up to a minimum at 1250 °C and then increased with the increasing sintering temperature. The composites prepared by SPS at 1250–1350 °C could be easily machined by electrical discharge machining. Composite prepared by SPS at 1300 °C showed a high hardness (17.78 GPa) and a good machinability.     

Dielectric and electrical conductivity properties of multi-stage spark plasma sintered HA–CaTiO3 composites and comparison with conventionally sintered materials

One of the different issues limiting the wider application of monolithic hydroxyapatite (HA) as an ideal bone replacement material is the lack of reasonably good electrical transport properties. The comprehensive electrical property characterization to evaluate the efficacy of processing parameters in achieving the desired combination of electroactive properties is considered as an important aspect in the development of HA-based bioactive material. In this perspective, the present work reports the temperature (RT-200 °C) and frequency (100 Hz–1 MHz) dependent dielectric properties and AC conductivity for a range of HA–CaTiO₃ (HA–CT) composites, densified using both conventional pressureless sintering in air as well as spark plasma sintering in vacuum. Importantly, the AC conductivity of spark plasma sintered ceramics [～upto 10^?5 (Ω cm)^?1] are found to be considerably higher than the corresponding pressureless sintered ceramics [～upto 10^?8 (Ω cm)^?1]. Overall, the results indicate the processing route dependent functional properties of HA–CaTiO₃ composites as well as related advantages of spark plasma sintering route.