Fracture characteristics of SiC/graphene platelet composites

Silicon carbide/graphene platelet (SiC/GPLs) composites were prepared using different weight percent of GPLs filler by hot pressing (HP) technology at 2100 °C in argon. The influence of the GPLs addition on bending strength, fracture toughness and related fracture characteristics was investigated. Both the bending strength and fracture toughness increased with increasing GPLs additives. The main fracture origins – strength degrading defects were pores at the low content of platelets and combination of pores and GPLs or clusters of GPLs particles in systems with a higher content of platelets. The fracture toughness increased due to the activated toughening mechanisms mainly in the form of crack bridging and crack branching, while the crack deflection was limited. The highest fracture toughness of 4.4 MPa m^1/2 was achieved at 6 wt.% of GPLs addition, which was ∼30% higher than the K_IC value of the reference material.     

Microstructure and fracture toughness of Si3N4 + graphene platelet composites

Silicon nitride + 1 wt% graphene platelet composites were prepared using various graphene platelets (GPLs) as filler. The influence of the addition of GPLs on the microstructure development and on the fracture toughness of Si₃N₄ + GPLs composites was investigated. The GPLs with thickness from 5 nm to 50 nm are relatively homogeneously distributed in the matrix of all composites, however overlapping/bundle formation of GPLs was found, containing 2–4 platelets as well. The single GPLs and overlapped GPLs are located at the boundaries of Si₃N₄, and hinder the grain growth and change the shape of the grains. The fracture toughness was significantly higher for all composites in comparison to the monolithic Si₃N₄ with the highest value of 9.9 MPa m^0.5 for the composite containing the GPLs with smallest dimension. The main toughening mechanisms originated from the presence of graphene platelets, and responsible for the increase in the fracture toughness values are crack deflection, crack branching and crack bridging.     

Influence of processing on fracture toughness of Si3N4 + graphene platelet composites

Silicon nitride + 1 wt% graphene platelet composites were prepared using various graphene platelets (GPL) and two processing routes; hot isostatic pressing (HIP) and gas pressure sintering (GPS). The influence of the processing route and graphene platelets’ addition on the fracture toughness has been investigated. The matrix of the composites prepared by GPS consists of Si₃N₄ grains with smaller diameter in comparison to the composites prepared by HIP. The indentation fracture toughness of the composites was in the range 6.1–9.9 MPa m^0.5, which is significantly higher compared to the monolithic silicon nitride 6.5 and 6.3 MPa m^0.5. The highest value of K_IC was 9.9 MPa m^0.5 in the case of composite reinforced by the smallest multilayer graphene nanosheets, prepared by HIP. The composites prepared by GPS exhibit lower fracture toughness, from 6.1 to 8.5 MPa m^0.5. The toughening mechanisms were similar in all composites in the form of crack deflection, crack branching and crack bridging.     

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.     

Slow crack growth and hydrothermal aging stability of an alumina-toughened zirconia composite made from La2O3-doped 2Y-TZP

A very tough zirconia matrix is interesting to fabricate alumina-toughened zirconia (ATZ) and composites generally processed from 3Y-TZP do not exhibit very high toughness. The strategy of lowering the yttria content to increase toughness however is normally associated with an increased hydrothermal aging susceptibility. In this work, a 0.4 mol% La₂O₃ doped 2Y-TZP matrix was investigated to realize a 20 wt.% alumina toughened zirconia composite with a substantially high aging resistance. The higher transformation toughening in the composite shifted the V-K_I towards higher K_I values, while preserving the slope of the curve, resulting in a threshold K_I0 of 4.0 MPa m^1/2 and fracture toughness (K_IC) of 7.1 MPa m^1/2. These composites can offer a better compromise between aging and crack resistance than traditional 3Y-TZPs and plain ATZ composites without La₂O₃ doping.     

The effect of graphene dispersion on the mechanical properties of graphene/epoxy composites

The effect of dispersion state of graphene on mechanical properties of graphene/epoxy composites was investigated. The graphene sheets were exfoliated from graphite oxide (GO) via thermal reduction (thermally reduced GO, RGO). Different dispersions of RGO sheets were prepared with and without ball mill mixing. It was found that the composites with highly dispersed RGO showed higher glass transition temperature (T_g) and strength than those with poorly dispersed RGO, although no significant differences in both the tensile and flexural moduli are caused by the different dispersion levels. In particular, the T_g was increased by nearly 11 °C with the addition of 0.2 wt.% well dispersed RGO to epoxy. As expected, the highly dispersed RGO also produced one or two orders of magnitude higher electrical conductivity than the corresponding poorly dispersed RGO. Furthermore, an improved quasi-static fracture toughness (K_IC) was measured in the case of good dispersion. The poorly and highly dispersed RGO at 0.2 wt.% loading resulted in about 24% and 52% improvement in K_IC of cured epoxy thermosets, respectively. RGO sheets were observed to bridge the micro-crack and debond/delaminate during fracture process due to the poor filler/matrix and filler/filler interface, which should be the key elements of the toughening effect.     

Effect of graphene addition on the mechanical and electrical properties of Al2O3-SiCw ceramics

This paper presents a study on graphene-reinforced Al₂O₃-SiCw ceramic composites and the relationship between graphene oxide (GO) loading and the resulting mechanical and electrical properties. Well-dispersed ceramic-GO powders were fabricated using a colloidal processing route. Dense composites were obtained via spark plasma sintering, a technique that has the ability to reduce GO to graphene in situ during the sintering process. The mechanical properties of the sintered composites were investigated. The composite with only a small amount of graphene (0.5 vol.%) showed the highest flexural strength (904 ± 56 MPa), fracture toughness (10.6 ± 0.3 MPa·m^1/2) and hardness (22 ± 0.8 GPa) with an extremely good dispersion of graphene within the ceramic matrix. In addition to these exceptional mechanical properties, the sintered composites also showed high electrical conductivity, which allows the compacts to be machined using electrical discharge machining and thus facilitates the fabrication of ceramic components with sophisticated shapes while reducing machining costs.     

Graphene reinforced alumina nano-composites

Graphene was prepared using liquid phase exfoliation and dispersed in an alumina matrix using an ultrasonication and powder processing route. Al₂O₃–graphene composites with up to 5 vol% content were densified (>99%) using SPS. The fracture toughness of the material increased by 40% with the addition of only 0.8 vol% graphene. However for higher graphene contents the improvement in fracture toughness was limited. Graphene changed the mechanism of crack propagation for the alumina matrix from inter-granular to trans-granular. The formation of an inter-connecting graphene network promoted easy fracture for concentration ⩾2 vol%. Elastic modulus remained nearly constant for up to 2 vol% and decreased significantly for 5 vol% due to the formation of the inter-connecting graphene network. Fracture toughness measured with the indentation and chevron notch methods were consistent up to 2 vol% and at 5 vol% the percolating network of graphene resulted in easy crack propagation with significant discrepancy between the results for the two methods.     

Effect of NiO additive on microstructure,mechanical behavior and electrical properties of 0.2PZN–0.8PZT ceramics

A NiO-added Pb((Zn_1/3Nb_2/3)_0.20(Zr_0.50Ti_0.50)_0.80)O₃ system is prepared and investigated. The results reveal that Ni doping induces a phase transformation from the morphotropic phase boundary to the tetragonal phase side. Above the solubility limit of 0.3 wt% in NiO form, excess Ni ions segregate at the grain boundaries and triple junctions, which facilitate the formation of a liquid phase with excess PbO and lead to remarkable grain growth. The mechanical behavior (Vickers hardness (H_v) and fracture toughness (K_IC)) can be tailored by controlling the content of additive; this is accompanied by a transition in the fracture mode changed from transgranular without NiO additive to intergranular with 1.0 wt% NiO additive. Moreover, the NiO addition weakens the dielectric relaxor behavior and improves the piezoelectric properties simultaneously. The 0.2PZN–0.8PZT with 0.5 wt% NiO addition shows good transduction coefficient (d₃₃·g₃₃ = 10,050 × 10^?15 m²/N) and large fracture toughness (K_IC = 1.35 MPa m^1/2).     

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.%.     

Tribo-mechanical characterization of spark plasma sintered chopped carbon fibre reinforced silicon carbide composites

Short carbon fibre (C_f) reinforced silicon carbide (SiC) composites with 7.5 wt% alumina (Al₂O₃) as sintering additive were fabricated using spark plasma sintering (SPS). Three different C_f concentrations i.e. 10, 20 and 30 wt% were used to fabricate the composites. With increasing C_f content from 0 to 20 wt%, micro-hardness of the composites decreased ~28% and fracture toughness (K_IC) increased significantly. The short C_f in the matrix facilitated enhanced fracture energy dissipation by the processes of crack deflection and bridging at C_f/SiC interface, fibre debonding and pullout. Thus, 20 wt% C_f/SiC composite showed >40% higher K_IC over monolithic SiC (K_IC≈4.51 MPa m^0.5). Tribological tests in dry condition against Al₂O₃ ball showed slight improvement in wear resistance but significantly reduced friction coefficient (COF, μ) with increasing C_f content in the composites. The composite containing 30 wt% C_f showed the lowest COF.     

Influence of experimental variables on fracture toughness determined on SEVNB in three points bending. Mullite a case study

The effect of testing variables on toughness of single edge “V” notched beams (4 mm × 6 mm × 50 mm, α = 0.6) of a fine grained mullite (d₅₀ = 0.7 ± 0.5 μm) in three points bending (span = 40 mm) is analysed. Mullite was selected as case material because it presents flat R-curve and subcritical crack propagation. Stable fracture was reached by using the CMOD as control variable (0.001 and 0.018 mm/min). Results for stable test and unstable displacement (0.05 mm/min) controlled tests are analysed. K_IC has been calculated from maximum loads, K_ICp, and from the total fracture energy determined in stable tests, K_ICγ. The fact that for materials with flat R-curve both K_IC values are coincident has been used as criterion for adequacy of the test. Stable fracture at high deformation rates is required to fulfil K_ICp = K_ICγ. Under such conditions, an intrinsic K_IC = 0.86 ± 0.06 MPa m^1/2, less than one half of those previously reported has been obtained.     

Role of cement content on the properties of self-flowing Al2O3 refractory castables

In this work, Al₂O₃ self-flowing castables (SFCs) were produced based on various cement contents. The SFCs were sintered at 1273 K, 1573 K and 1773 K and the exhibited properties were experimentally determined. Among the properties determined in this work are bulk density (BD), apparent porosity (AP), water absorption (WA), cold crushing strength (CCS), modulus of rupture (MOR) and fracture toughness (K_IC). It is found that additions of 5% cement lead to SFCs with maximum MOR and K_IC values after firing at 1773 K. Firing at 1573 K leads to a reduction in both, MOR and K_IC. In SFC containing 3% cement, maximum K_IC values of 3.53 MPa m^1/2 were achieved after firing at 1573 K. In the low cement SFCs (1 wt%) after firing at 1773 K the exhibited K_IC values were below those obtained in either the SFC-3 or SFC-5, but they were significantly high (3.43 MPa m^1/2).     

Investigation of fracture toughness of modified (KxNa1 − x)NbO3 lead-free piezoelectric ceramics

While most of the previous studies have focused on the processing and electrical properties of KNN-based ceramics, very little research has been carried out to evaluate their mechanical behavior. This work presents for the first time an examination of the fracture toughness, K_IC, of the most widely studied (K_xNa_1 ? x)NbO₃ (KNN)-based lead-free ceramics modified with lithium, tantalum and antimony. The samples were produced through the conventional mixed-oxide route and the K_IC values were measured using the single edge V-notched beam (SEVNB) method under four-point bending. The mean K_IC values were determined to be 0.48 ± 0.18 MPa m^1/2 for (K_0.48Na_0.48Li_0.04)NbO₃, 0.8 ± 0.18 MPa m^1/2 for (K_0.5Na_0.5)(Nb_0.9Ta_0.1)O₃, 0.86 ± 0.04 MPa m^1/2 for (K_0.48Na_0.48Li_0.04)(Nb_0.9Ta_0.1)O₃ and 1.06 ± 0.21 MPa m^1/2 for (K_0.48Na_0.48Li_0.04)(Nb_0.86Ta_0.1Sb_0.04)O₃ compositions. The microstructure, phase structure and dielectric constant values of the samples have been used to correlate the results of the K_IC values.     

Densification and mechanical properties of TiC by SPS-effects of holding time,sintering temperature and pressure condition

The influence of sintering temperature, holding time and pressure condition on densification and mechanical properties of bulk titanium carbide (TiC) fabricated by SPS sintering has been systematically investigated. Experimental data demonstrated that relative density and Vickers hardness (H_V) increase with sintering temperature and holding time, but fracture toughness (K_IC) was not significantly influenced by sintering parameters. The H_V and relative density of samples consolidated by SPS technique at 1600 °C for 5 min under 50 MPa pressure (applied entire sintering cycle) reached 30.31 ± 2.23 GPa and 99.90%, respectively. H_V values of ～24–30 GPa and K_IC of ～3.7–5 MPa m^1/2 were obtained in all bulk samples with relative densities of 95.61–99.90% when fabricated under various conditions presented above, without abnormal grain growth. More pronounced effects of pressure condition on grain growth (promoted by grain-boundary diffusion) than on densification were observed. The relationship of fracture toughness and fracture mode is also discussed.     

Hardness and fracture toughness of moissanite

Disparities prevail among the reported hardness and fracture toughness values for hard and brittle materials. A better understanding of the physical nature of hardness and fracture toughness and a standardized technique for reliable measurements of these quantities is urgently needed. We strongly recommend the use of the measured hardness after the bend in the hardness versus load (H−F_Load) curve, when the hardness approaches its asymptotic value. The present work reports a systematic study of hardness and fracture toughness on moissanite (single crystal hexagonal silicon carbide, 6H-SiC) samples. The measurements were performed over a broad load range from 0.49 to 294 N with the direct indentation method. Asymptotic values of Knoop hardness of H_K = 19 GPa and Vickers hardness of H_V = 22 GPa were reached at a high load between 50 N and 100 N. A consistent fracture toughness of K_IC = 1.8 MPa·m^1/2 was obtained across the entire load range. Our study presents experimental results for the hardness and fracture toughness of moissanite in the asymptotic-hardness region, and it raises concern regarding the application of moissanite single crystals as anvil material under shear/fracture conditions.     

Microstructure and properties of B4C-SiC composites prepared by polycarbosilane-coating/B4C powder route

B₄C-SiC composites with fine grains were fabricated with hot-pressing pyrolyzed mixtures of polycarbosilane-coated B₄C powder without or with the addition of Si at 1950 °C for 1 h under the pressure of 30 MPa. SiC derived from PCS promoted the densification of B₄C effectively and enhanced the fracture toughness of the composites. The sinterability and mechanical properties of the composites could be further improved by the addition of Si due to the formation of liquid Si and the elimination of free carbon during sintering. The relative density, Vickers hardness and fracture toughness of the composites prepared with PCS and 8 wt% Si reached 99.1%, 33.5 GPa, and 5.57 MPa m^1/2, respectively. A number of layered structures and dislocations were observed in the B₄C-SiC composites. The complicated microstructure and crack bridging by homogeneously dispersed SiC grains as well as crack deflection by SiC nanoparticles may be responsible for the improvement in toughness.     

Microstructure and mechanical properties of Ti (C,N) based cermets reinforced with different ceramic particles processed by spark plasma sintering

The addition effect of different ceramic particles such as TiB₂, TiN and nano-Si₃N₄ on the microstructure and mechanical properties of TiCN-WC-Co-Cr₃C₂ based cermets, which are prepared by spark plasma sintering, was studied. Microstructural characterization of the cermets was done by scanning electron microscope. X-ray diffraction was performed to study the crystal structures. Mechanical properties such as hardness and fracture toughness were measured for the different developed cermets. The hardness and fracture toughness of the TiCN-WC-Co-Cr₃C₂ cermets without TiN, TiB₂, and nano-Si₃N₄ were 8.4 GPa and 3.4 MPa m^1/2, respectively. It was found that 5 wt% TiB₂ addition alone improved the corresponding hardness and fracture toughness to 19.2 GPa and 6.9 MPa m^1/2, respectively. The addition of 5 wt% TiN, improved the hardness and fracture toughness to 16.7 GPa and 6.9 MPa m^1/2, respectively. With the combination of 5 wt% TiN and 5 wt% TiB₂, the hardness and fracture toughness were improved to 15.5 GPa and 6.6 MPa m^1/2, respectively. But, the addition of 5 wt% Si₃N₄ showed a balanced improvement in both hardness (17.6 GPa) and toughness (6.9 MPa m^1/2). Fracture toughness did not change much for all the above cermets with different ceramic inclusions.     

Large-area reduced graphene oxide thin film with excellent thermal conductivity and electromagnetic interference shielding effectiveness

In this work, we fabricated reduced large-area graphene oxide (rLGO) with maximum surface area of 1592 μm² through a cost-effective chemical reduction process at low temperature. The product revealed large electrical conductivity of 243 ± 12 S cm⁻¹ and thermal conductivity of 1390 ± 65 W m⁻¹ K⁻¹, values much superior to those of a conventional reduced small-area graphene oxide (with electrical conductivity of 152 ± 7.5 S cm⁻¹ and thermal conductivity of 900 ± 45 W m⁻¹ K⁻¹). The rLGO thin film also exhibited not only excellent stiffness and flexibility with Young’s modulus of 6.3 GPa and tensile strength of 77.7 MPa, but also an efficient electromagnetic interference (EMI) shielding effectiveness of ∼20 dB at 1 GHz. The excellent performance of rLGO is attributed to the fact that the larger area LGO sheets include much fewer defects that are mostly caused by the damage of graphene sp² structure around edge boundaries, resulting in large electrical conductivity. The manufacturing process of rLGO is an economical and facile approach for the large scale production of highly thermally conducting graphene thin films with efficient EMI shielding properties, greatly desirable for future portable electronic devices.     

The fabrication and mechanical properties of SiC/ZrB2 laminated ceramic composite prepared by spark plasma sintering

Laminated SiC/ZrB₂ ceramic was fabricated by roll-compaction and spark plasma sintering at 1600 °C. A maximum fracture toughness of 12.3 ± 0.3 MPa m^1/2 was measured for the sintered SiC/ZrB₂ laminated ceramic. This significant improvement in fracture toughness can be attributed to the crack deflection along the interfacial layer and the presence of residual stresses in the sample. The effect of interlayer composition on the residual stresses was discussed in detail. It is observed that the residual thermal stress could be reduced by addition of ZrB₂ particles to the SiC interlayer. The bending strength can be increased to 388 ± 44 MPa with the addition of 20 vol% ZrB₂ to the SiC interlayer.