Microstructure and mechanical properties of ZrB2-SiC composites

A ZrB₂-based composite containing 20 vol.% nanosized SiC particles (ZSN) was fabricated at 1900 °C for 30 min under a uniaxed load of 30 MPa by hot-pressing. The microstructure and mechanical properties of the composite were investigated. It was shown that the grain growth of ZrB₂ matrix was effectively suppressed by submicrosized SiC particles located along the grain boundaries. In addition, the mechanical properties of ZSN composite were strongly improved by incorporating the nanosized SiC particles into a ZrB₂ matrix, especially for flexural strength (925 ± 28 MPa) and fracture toughness (6.4 ± 0.3 MPa•m^1/2), which was much higher than that of monolithic ZrB₂ and ZrB₂-based composite with microsized SiC particles, respectively. The formation of intragranular nanostructures plays an important role in the strengthening and toughening of ZrB₂ ceramic.     

Effect of BN grain size on microstructure and mechanical properties of the ZrB2–SiC–BN composites

ZrB₂–20 vol.%SiC composites containing 10 vol.% h-BN particles (ZSB) with average grain sizes ranging from 1 μm to 10 μm were hot-pressed. The fracture toughness of the ZSB composites was higher than reported results of monolithic ZrB₂ (2.3–3.5 MPa m^1/2) and SiC particle reinforced ZrB₂ composites (4.0–4.5 MPa m^1/2). The improvement in the fracture toughness of the ZSB composites was due to the high aspect ratio of h-BN and weaker interface bonding, which could enhance crack deflection and stress relaxation near the crack-tip. Compared with the flexural strength of the ZrB₂–SiC composites, the reduction in the flexural strength of the ZSB composites was attributed to the weaker interface bonding and the lower relative density. Furthermore, improvement in toughness and the reduction in the strength were valuable to improve the thermal shock resistance of the ZSB composites. The ΔT_c of ZSB5 material is 400 °C which is higher than ZrB₂–20%SiC and ZrB₂–15%SiC–5%AlN.     

ZrB2-ceramic toughened by refractory metal Nb prepared by hot-pressing

ZrB₂–Nb (ZN) composites were prepared through hot-pressing at a temperature of 1800 °C. A contribution of Nb was believed a significant influence on the sinterability, microstructure and mechanical properties of ZN composites. The values of flexural strength of ZN composites rang from 395 to 773 MPa, who are dependent on Nb contents. The highest strength obtained for the ZN composite containing 25 vol.% Nb (773 MPa). A fracture toughness of 7.1 MPa m^1/2 of ZN was revealed, which was much higher than that of monolithic ZrB₂. The improvement in fracture toughness strongly depended on an introduction of Nb–ZrB₂ matrix. Crack deflection and branching were believed to be the toughening mechanism of ZN.     

Microstructure and mechanical properties of hot pressed ZrB2-SiCp-ZrO2 composites

The present paper investigated the microstructure and mechanical properties of ZrB₂-10 vol.%SiC_p-10 vol.%ZrO₂ composites hot pressed at three temperatures. Phase transformability from t-ZrO₂ to m-ZrO₂ during fracture was analyzed through calculating the volume fractions of m-ZrO₂ and t-ZrO₂ on polished and fracture surfaces. The densification temperature was found to have a significant effect on the microstructure, phase transformation and the properties of the composites. When the composite was hot pressed at 1950 °C, the average grain size was 9.5 µm, and the fracture toughness was 4.5 MPa·m^1/2. Comparatively, when the composite was hot pressed at 1750 °C, the average grain size was 3.4 µm, and the fracture toughness increased by ~ 50% to 6.8 MPa·m^1/2.     

The thermal shock resistance of the ZrB2–SiC–ZrC ceramic

In the present work, the thermal shock resistance of the ZrB₂–SiC–ZrC ceramic was estimated by the water quenching method and the flexural strength of the quenched specimen was measured. The measured critical temperature difference of the ZrB₂–SiC–ZrC ceramic was significantly greater than that of the ZrB₂–15 vol.% SiC ceramic. The improvement in thermal shock resistance was attributed to its higher fracture toughness (6.7 MPa m^1/2) and lower flexural strength (526 MPa) relative to the ZrB₂–15 vol.% SiC ceramic (4.1 MPa m^1/2 and 795 MPa) based on Griffith fracture criterion. Furthermore, the temperature and thermal stress distributions in the specimen during instantaneous water quenching were simulated by Finite element analysis.     

The failure mechanism of ZrB2-SiC-graphite composite heated by high electric current

The failure mechanism of the ZrB₂-SiC-graphite composite heated by high electric current was investigated. The results indicated that a large numbers of graphite flake was torn along their basal planes, which was attributed to that the thermal stress is perpendicular to graphite flake. The thermal stress resulted from the thermal expansion mismatch during rapid heating was calculated to be above 1.5 GPa using Hsueh's formula. Although the thermal stresses were relaxed through the deformation of graphite, the maximum thermal stresses were higher than the strength of < 500 MPa for the ZrB₂-SiC-graphite composite, which resulted in the destruction of the specimen.     

In situ synthesis and properties of Zr2Al3C4/ZrB2 composites

The Zr₂Al₃C₄/ZrB₂ composites are in situ synthesized by spark plasma sintering using Zr, Al, graphite, and B₄C powders as the initial materials. The introduction of ZrB₂ can not only evidently hinder the coarsening of Zr₂Al₃C₄ grains, but also benefit the densification and improve the hardness and Young’s modulus of the Zr₂Al₃C₄/ZrB₂ composites. When the ZrB₂ content is 20 vol.%, the composite shows an optimum fracture toughness value of 4.37 MPa m^1/2, about 20% higher than that of the monolithic Zr₂Al₃C₄. The unique mechanical properties can be mainly ascribed to the contribution of ZrB₂ as the reinforcing phase hindering the crack propagating. Compared with Zr₂Al₃C₄, the Zr₂Al₃C₄/20 vol.%ZrB₂ composite also exhibits a relatively higher thermal conductivity and better oxidation resistance.     

Effect of annealing treatment on mechanical properties of a ZrB2-SiC-graphite ceramic

The ZrB₂-SiC-graphite (ZSG) ceramic was annealed at 1600, 1700 and 1800 °C for different times, respectively. It was revealed that the annealing treatment is favorable to increase the interface bonding and relative density, and to decrease the thermal residual stress, to result in the crimp of the graphite flake. It was the optimal annealing treatment process conditions of 1700 °C and 90 min according to the best combination of the mechanical properties. To compare the mechanical properties of the specimen before the annealing treatment, the hardness, strength and toughness of the specimen annealed at 1700 °C for 90 min were enhanced by 20.6% and 20.2%, decreased by 8.2%, respectively.     

Microstructure and mechanical properties of titanium carbonitride whisker reinforced β-sialon matrix composites

The microstructure, hardness, fracture toughness and thermal shock resistance were investigated for 15 vol.% TiC_0.3N_0.7 whisker reinforced β-sialon (Si_6−zAl_zO₂N_8−z with z=0.6) composites with additions of three different volume fractions 2, 5 and 20 vol.%, of an yttrium-containing glass oxynitride phase. The composites were prepared by hot pressing at 1750°C for 90 min under a uniaxial pressure of 30 MPa in nitrogen atmosphere. The TiC_0.3N_0.7 whiskers were found to survive without deteriorating in morphology or reacting with the β-sialon matrix and/or the glass phase. The TiC_0.3N_0.7 whiskers had no obvious influence on the matrix microstructure, but their presence improved both the hardness and the fracture toughness of the composites. The highest hardness was obtained for the whisker composite with 2 vol.% glass phase (H_v=18.6 GPa). The fracture toughness and thermal shock resistance improved with increasing glass content. The whisker reinforced composite containing 20 vol.% glass showed the highest fracture toughness (K_1C=6.8 MPa m^1/2). No unstable crack extension occurred during the thermal shock test of the obtained composites in the temperature interval 90-700°C, but above 700°C severe oxidation of the whiskers precludes further evaluation of thermal shock properties by the indentation-quench method applied.     

Synthesis and mechanical properties of high-purity Cr2AlC ceramic

High-purity and dense Cr₂AlC has been successfully fabricated by hot-pressing, using Cr, Al and graphite as raw materials. Delamination, kink bands, monolamellar kink, transgranular crack and transgranular fracture of bulk Cr₂AlC are found during the room-temperature test. The density, Vickers hardness, flexural strength, Young's modulus, compressive strength and fracture toughness of the Cr₂AlC are 5.17 g/cm³, 4.9 GPa, 469 ± 27 MPa, 282 GPa, 949 ± 22 MPa and 6.22 ± 0.26 MPa m^1/2, respectively. The strength of Cr₂AlC could be greatly improved by second phase of Cr₇C₃. And the slipping of basal planes and slip system cold be hindered by Cr₇C₃, thus resulting in a lower toughness.     

Fracture behavior and mechanism of 2D C/SiC-BCx composite at room temperature

2D C/SiC composite was modified with partial BC_x matrix by low pressure chemical vapor infiltration technique (LPCVI), which was named as 2D C/SiC-BC_x composite. The flexural fracture behavior, mechanism, and strength distribution of 2D C/SiC-BC_x composite are investigated. The results indicate that the flexural strength, fracture toughness, and fracture work are 442.1 MPa, 22.84 MPa m^1/2, and 19.2 kJ m⁻², respectively. The flexural strength of C/SiC-BC_x composite decrease about 20% than that of C/SiC composite. However, the fracture toughness and fracture work increase about 19% and 18.5%, respectively. The properties varieties between C/SiC-BC_x composite and C/SiC composite can be attributed to the weak-bonding interface between BC_x/SiC matrices according to the results of detailed microstructure analysis. The strength distribution of 2D C/SiC-BC_x composite follows as Normal distribution or Weibull distribution with σ_u = 0, and m = 8.1393. The mean value of flexural strength for 2D C/SiC-BC_x composite is 443 MPa obtained by theory calculation, which is consistent with experiment result (442.1 MPa) very well.     

Synthesis, densification, and mechanical properties of TaB2

Tantalum diboride (TaB₂) was synthesized by reducing Ta₂O₅ using B₄C and graphite at 1600 °C under flowing Ar. The powder had an average particle size of 0.4 μm with both needle-like and rounded particles. The TaB₂ powder was hot pressed to relative densities of 97% at 2000 °C (3.6 μm grain size) and 98% at 2100 °C (5.3 μm grain size). Mechanical properties were measured for TaB₂ hot pressed at 2100 °C and were comparable to those of the commonly studied diborides, ZrB₂ and HfB₂. The Young's modulus was 551 GPa, Vickers' hardness was 25.6 GPa, flexure strength was 555 MPa, and fracture toughness was 4.5 MPa-m^1/2.     

Preparation and properties of nano-SiC strengthening Al2O3 composite ceramics

The processing and mechanical behaviors of Al₂O₃-xwt.%SiC (x = 1, 2, 5, ASx) nano-composites prepared by the in situ synthesis of SiC from polycarbosilane (PCS) were investigated. The composites were densified by hot pressing. The microstructure and mechanical properties of the sintered composites were analyzed. The results showed that a fully dense structure was obtained when a few nano-SiC were doped and that the fracture toughness and strength were highly improved compared with those of monolithic Al₂O₃. The fracture toughness reached 5.1 MPa m^1/2 in AS2 composite. The maximum flexural strength was 516 MPa obtained in AS1 composite.     

Influence of cobalt phase on thermal shock resistance of Al2O3-TiC composites evaluated by indentation technique

Cobalt-coated Al₂O₃ and TiC powders were prepared using an electroless method to improve resistance to thermal shock. The mixture of cobalt-coated Al₂O₃ and TiC powders (about 70 wt.% Al₂O₃-Co + 30 wt.% TiC-Co) was hot-pressed into an Al₂O₃-TiC-Co composite. The thermal shock properties of the composite were evaluated by indentation technique and compared with the traditional Al₂O₃-TiC composite. The composites containing 3.96 vol.% cobalt exhibited better resistance to crack propagation, cyclic thermal shock and higher critical temperature difference (ΔT_c). The calculation of thermal shock resistance parameters (R parameters) shows that the incorporation of cobalt improves the resistance to thermal shock fracture and thermal shock damage. The thermal physic parameters are changed very little but the flexure strength and fracture toughness of the composites are improved greatly by introducing cobalt into Al₂O₃-TiC (AT) composites. The better thermal shock resistance of the composites should be attributed to the higher flexure strength and fracture toughness.     

Size effect on fracture toughness of freestanding copper nano-films

We conducted fracture toughness experiments on freestanding copper films with thicknesses ranging from about 800 to 100 nm deposited by electron beam evaporation to elucidate the size effect on fracture toughness in the nano- or submicron-scale. It was found that initially, the crack propagated stably under loading, and then the crack propagation rate rapidly increased, resulting in unstable fracture. The fracture toughness K_C was estimated on the basis of the R-curve concept to be 7.81 ± 1.22 MPa m^1/2 for the 800-nm-thick film, 6.63 ± 1.05 MPa m^1/2 for the 500-nm-thick film and 2.34 ± 0.54 MPa m^1/2 for the 100-nm-thick film. Thus, a clear size effect was observed. The fracture surface suggested that the crack underwent large plastic deformation in the thicker 800-nm and 500-nm films, whereas it propagated with highly localized plastic deformation in the thinner 100-nm film. This size effect in fracture toughness might be related to a transition in deformation and fracture morphology near the crack tip.     

Influence of the microstructure evolution of ZrO2 fiber on the fracture toughness of ZrB2–SiC nanocomposite ceramics

ZrB₂–SiC nanocomposite ceramics toughened by ZrO₂ fiber were fabricated by spark plasma sintering (SPS) at 1700 °C. The content of ZrO₂ fiber incorporated into the ZrB₂–SiC nanocomposites ranged from 5 mass% to 20 mass%. The content, microstructure, and phase transformation of ZrO₂ fiber exhibited remarkable effects on the fracture toughness of the ZrO_2(f)/ZrB₂–SiC composites. Fracture toughness of the composites greatly improved to a maximum value of 6.56 MPa m^1/2 ± 0.3 MPa m^1/2 by the addition of 15 mass% of ZrO₂ fiber. The microstructure of the ZrO₂ fiber exhibited certain alterations after the SPS process, which enhanced crack deflection and crack bridging and affected fracture toughness. Some microcracks were induced by the phase transformation from t-ZrO₂ to m-ZrO₂, which was also an important reason behind the improvement in toughness.     

Preparation and mechanical properties of laminated zirconium diboride/molybdenum composites sintered by spark plasma sintering

Laminated ZrB₂/Mo composites, alternately consisting of matrix layers of 80 vol.% ZrB₂ + 10 vol.% nano-SiC whiskers + 10 vol.% SiC particles and Mo interlayers, with the addition of Si and B as interlayer adjusting agent, were prepared by roll-compaction and spark plasma sintering (at 1600°C) process. XRD and SEM techniques were used to characterize the phases and microstructure of the obtained composites. The results showed that without the addition of Si and B in the interlayer, interfacial debonding between the matrix layer and interlayer often occurred due to the thermal mismatch between the two kinds of layers. However, the interfacial mismatch could be effectively inhibited by the addition of Si and B to the Mo interlayers. The laminated ZrB₂/Mo composites with 6 at.% Si and 4 at.% B in the interlayers showed the highest bending strength at (451±20) MPa and the highest fracture toughness at (7.52±0.12) MPa·m^?. MoB, ZrB and Mo5SiB2 were formed by the reactions among ZrB₂, Mo and the additions.     

Effect of supercritical water applied to reactor on microstructure and flexural strength of ZrB2–SiC–Graphite ceramic

The ZrB₂–SiC–Graphite ceramic was immerged in the supercritical water for different times. The microcracks appeared on the surface of the specimen and the composition of the microcracks was confirmed by EDS analysis to be ZrO₂. The obvious corrosion of SiC and graphite flake on the surface of the specimen was not observed, which was attributed to the dissolution of the oxides of silicon and carbon (graphite) into the supercritical water. The corrosion of the specimen was accelerated as the pressure and temperature of the water increased. XPS analysis was carried out on the specimen corroded in water of 40 ± 1 MPa and 500 ± 10 °C for 75 min, and the significant peak of B 1s was also measured, indicating the presence of the ZrB₂ phase on the surface of the specimen. For the specimen immerged in all conditions, the Vickers’ hardness did not reduce, the fracture toughness was improved and the minimal strength of the immerged specimen was still higher than 90% of the original strength of 480 MPa, which indicated that the ZrB₂–SiC–Graphite ceramic has excellent resistance to corrosion of the supercritical water applied to reactor.     

Toughening effect of short carbon fibers in the ZrB2–ZrSi2 ceramic composites

The toughening effect of the short carbon fibers in the ZrB₂–ZrSi₂ ceramic composites were investigated, where the ZrB₂–ZrSi₂ ceramics without carbon fibers were used as the reference. The mechanical properties were evaluated by means of flexural and SENB tests, respectively. The microstructure was characterized by SEM equipped with EDS. The results found that the short carbon fibers were uniformly incorporated in the ZrB₂–ZrSi₂ matrix and the relative density was about 97.92%. The flexural strength of short carbon fiber-reinforced ZrB₂–ZrSi₂ composites is 437 MPa; the fracture toughness and the work of fracture are 6.89 MPa m^1/2 and 259 J/m², respectively, which increased significantly in comparing with composites without fibers. The microstructure analysis revealed that the improved fracture toughness could be attributed to the fiber bridging, the fiber–matrix interface debonding and the fiber pullout, which consumed more fracture energy during the fracture process.     

Effect of a weak fiber interface coating in ZrB2 reinforced with long SiC fibers

This study reports the microstructural analysis and mechanical properties of a ZrB₂ ceramic containing long BN-coated Hi-Nicalon SiC fibers. A composite was produced and thoroughly characterized by transmission electron microscopy to study the interfaces at the nanoscale level. Full densification was accomplished by hot pressing at 1450 °C. The fiber in the sintered material retained its pristine aspect, confirming that the coating was effective in preventing degradation due to interactions with the matrix. Pull-out was observed on fractured surfaces, but toughness values were about 4.5 MPa√m, which was comparable to those of ZrB₂ materials with SiC additions in the form of particles or short fibers. However, the composites exhibited a controlled fracture behavior, as confirmed by a notably higher work of fracture, 140 J/m², compared with 20–30 J/m² of unreinforced ZrB₂ or ZrB₂ containing chopped fibers.