Microstructure and fracture toughness of SiAlCN ceramics toughened by SiCw or GNPs

Mechanical alloying and spark plasma sintering (SPS) were used to prepare dense SiAlCN ceramic and SiAlCN ceramic toughened by SiC whiskers (SiC_w) or graphene nanoplatelets (GNPs). The influences of different reinforcements on the microstructure and fracture toughness were investigated. The SiAlCN ceramic exhibited a fracture toughness of 4.4 MPa m^1/2 and the fracture characteristics of grain bridging, alternative intergranular and transgranular fracture. The fracture toughness of SiC_w/SiAlCN ceramic increased to 5.8 MPa m^1/2 and toughening mechanisms were crack deflection, SiC_w bridging and pull-out. The fracture toughness of GNP/SiAlCN ceramic increased significantly, which was up to 6.6 MPa m^1/2. GNPs played an important role in grain refinement, which resulted in the smallest grain size. Multiple toughening mechanisms, including crack deflection, crack branch, GNP bridging and pull-out could be found. The better toughening effect could be attributed to the larger specific surface area of GNPs and the appropriate interface bonding between GNPs and matrix.     

Ultrafine-grained B6O–diamond composites with superb mechanical properties

We report here the high-pressure and high-temperature (HPHT) synthesis of well-sintered B₆O–diamond composites from B₆O and carbon black nanopowders. The carbon black was transformed into diamond nanograins at HPHT conditions, and simultaneously formed high-strength B₆O–diamond interfaces. The ultrafine B₆O and diamond nanograins and the high-strength B₆O–diamond interfaces synergistically construct excellent mechanical properties for the synthesized composites. The B₆O–diamond composites possess a hardness (avg. 52 GPa) comparable to that of polycrystalline diamond (40–60 GPa), whereas the fracture toughness (avg. 7.2 MPa m^1/2) is increased several times compared to previously synthesized polycrystalline B₆O ceramics (1.7–3.1 MPa m^1/2) and B₆O-based composites (3–4 MPa m^1/2). Fracture behavior analysis demonstrates that the main toughening mechanisms in this B₆O–diamond composite are nanotwin toughening, crack deflection, and crack bridging.     

Microstructure and mechanical properties of boron carbide/graphene nanoplatelets composites fabricated by hot pressing

In this study, boron carbide (B₄C)-graphene nanoplatelets (GNPs) composites, with enhanced strength and toughness, were fabricated by hot pressing at 1950 °C under a pressure of 30 MPa for 1 h. Microstructure analysis revealed that the GNPs are homogenously dispersed within the B₄C matrix. Raman spectroscopy and electron microscopy showed the orientation of the GNPs in the composites. The effects of the amount of GNPs on the microstructure and mechanical properties of the composites were also investigated. The optimal mechanical properties were achieved using 1 wt% GNPs. The relative density, Vickers hardness, flexure strength, and fracture toughness of the B₄C-GNPs composite ceramic were found to be 99.12%, 32.8 GPa, 508 MPa, and 4.66 MPa m^1/2, respectively. The main toughening mechanisms included crack deflection in three dimensions, GNPs pull-out, and crack bridging. The curled and semi-wrapped GNPs encapsulated individual B₄C grains to resist GNPs pull-out and to deflect propagating cracks.     

Preparation and mechanical properties of laminated B4C–TiB2/BN ceramics

Laminated B₄C–TiB₂ ceramics with h-BN interface layers were successfully prepared by roll forming and tape casting, and samples with different numbers of stacked layers were obtained. Scanning electron microscopy and X-ray diffraction were used to analyze the microstructure and interlayer crystal phases of the composites, and the bending strength, fracture toughness, and work of fracture were measured. As the number of h-BN layers increased, the fracture toughness increased from 7.38 ± 0.5 MPa m^1/2 to 9.01 ± 0.61 MPa m^1/2, which is 2–3 times higher than that of monolithic B₄C ceramics. As the fracture toughness increased, the hardness remained at a high level (31.67 GPa). Bending tests showed that cracks deflected when they encountered the h-BN interfacial layers. The toughening mechanisms included the deflection and branching of cracks and generation of new microcracks, which increased the length of the propagation path and work of fracture.     

Design of crack deflection induced high toughness laminated Si3N4 ceramics based on hollow oriented one-dimensional microstructure

A laminated silicon nitride (Si₃N₄) ceramic material with a hollow, oriented, one-dimensional microstructure was successfully prepared based on the tape casting and sacrificial template method. The results show that hollow, oriented, one-dimensional microstructures can effectively induce crack deflection. Different arrangements of the structural design layer and dense layer will have different effects on the material. In particular, bulks with a single-layer orthogonal arrangement of the structural design layer possess high toughness and obvious crack deflection during the fracture process. A kind of multiscale crack deflection mode was realized. Compared with the fracture toughness of the monolithic Si₃N₄ ceramic bulk (5.55 MPa m^1/2), the fracture toughness can reach 8.73 MPa m^1/2, and the flexural strength can still reach 391.47 MPa with only a slight decrease.     

B4C–TiB2 composites fabricated by hot pressing TiC–B mixtures: The effect of B excess

Previous research have reported that B₄C–TiB₂ composites could be prepared by the reactive sintering of TiC–B powder mixtures. However, due to spontaneous oxidation of raw powders, using TiC–B powder mixtures with a B/TiC molar ratio of 6: 1 introduced an intermediate phase of C during the sintering process, which deteriorated the hardness of the composites. In this report, the effects of B excess on the phase composition, microstructure, and mechanical properties of B₄C–TiB₂ composites fabricated by reactive hot pressing TiC–B powder mixtures were investigated. XRD and Raman spectra confirmed that lattice expansion occurred in B-rich boron carbide and B_xC–TiB₂ (x > 4) composites were obtained. The increasing B content improved the hardness and fracture toughness but decreased the flexural strength of B_xC–TiB₂ (x > 4) composites. When the molar ratio of B/TiC increased from 6.6:1 to 7.8:1, the Vickers hardness and the fracture toughness of the composites were enhanced from 26.7 GPa and 4.53 MPa m^1/2 to 30.4 GPa and 5.78 MPa m^1/2, respectively. The improved hardness was attributed to the microstructural improvement, while the toughening mechanism was crack deflection, crack bridging and crack branching.     

Fabrication and characterization of SiC-ZTA ceramic composites by hot pressing

Al₂O₃/ZrO₂/SiC ceramic composites with different SiC contens have been prepared by hot pressuring. The effect of SiC content on the microstructure and mechanical properties of composites have been studied. The results show that SiC has obvious grain refinement effect on ZTA ceramics and change the fracture mode of the matrix from intergranular fracture to transgranular fracture. Simultaneously, it has been found that the mechanical properties of the material are significantly enhanced in comparison with ZTA matrix. The highest strength is acquired at 10% SiC content, the flexural strength and toughness are obtained when the SiC content is 15 vol%, and the values are 18.86 GPa, 1262 MPa and 6.13 MPa m^1/2, respectively. The mechanisms of hardening, strengthening and toughening have been discussed.     

Developing high toughness and strength Al/TiC composites using ice-templating and pressure infiltration

We prepared Al/TiC composites with different ceramic volume fractions (15, 25 and 35 vol%) using ice-templating and pressure infiltration. The thickness of the lamellar layer and the porosity in the ceramic layer of the TiC scaffolds were controlled by varying the slurry concentration. The Al/15 vol%TiC composite had a thick metal layer and a low-density ceramic layer, which effectively dissipated the stress at the crack tip and fractured in a multiple-crack-propagation mode, giving bending strength of 355±3 MPa and fracture toughness of 81±2 MPa m^1/2. However, the Al/25 vol%TiC and Al/35 vol%TiC composites had much higher bending strength (417−500 MPa) but lower fracture toughness (46−33 MPa m^1/2) as compared to the Al/15 vol%TiC composite, and they fractured in a single-crack-propagation mode. In addition, an increase in the brittle TiAl₃ phase with increasing ceramic volume at the fracture surface greatly deteriorated the toughness of the Al/TiC composites. Finally, the relationship between cracking mode and structure features in the laminated composites was discussed to account for the toughening mechanism.     

Role of carbon nanotubes on mechanical properties of SiC-B4C-Ni hybrid composites fabricated by reactive spark plasma sintering

The present study was conducted to investigate the microstructural and mechanical properties of SiC-45 vol%B₄C-10 vol%Ni and SiC-45 vol% B₄C-10 vol%Ni-5vol% CNT in-situ composites fabricated through reactive spark plasma sintering (SPS) method at 1650 °C for 5 min. The phase and microstructural characterization of the composites were evaluated utilizing x-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Ultimately, microhardness, flexural strength, and fracture toughness of the composites were measured. Densification behavior of the samples revealed that the initial shrinkage of the composites took place at about 750 °C, which is related to the reaction between Ni and SiC phases. XRD results confirmed the formation of Ni₂Si phase. The relative density of 98.3 ± 0.32% was achieved for the SiC-B₄C-10Ni sample; this value was 97.8 ± 0.62% for the SiC-B₄C-10Ni-5CNT sample. The flexural strength of 362 ± 23 MPa was achieved for the SiC-B₄C-10Ni sample; this value was 369 ± 15 MPa for the SiC-B₄C-10Ni-5CNT sample. The comparison between the fabricated composites concerning the fracture toughness indicated further fracture toughness of the SiC-B₄C-10Ni-5CNT sample (5.82 ± 0.32 MPa m^1/2) than that of the SiC-B₄C-10Ni sample (3.35 ± 0.56 MPa m^1/2). Formation of micro-cracks, crack path deflection, and CNT bridging was the main toughening mechanisms in the SiC-B₄C-10Ni-5CNT sample.     

Microstructures and mechanical properties of B4C–SiC and B4C–SiC–TiB2 ceramic composites fabricated by hot pressing

Boron carbide (B₄C) ceramic composites with excellent mechanical properties were fabricated by hot-pressing using B₄C, silicon carbide (SiC), titanium boride (TiB₂), and magnesium aluminum silicate (MAS) as raw materials. The influences of SiC and TiB₂ content on the microstructural evolution and mechanical properties of the composites were systematically investigated. The mechanism by which MAS promotes the sintering process of composites was also investigated. MAS exists in composites in the form of amorphous phase. It can effectively remove the oxide layer from the surface of ceramic particles during the high temperature sintering process. The typical values of relative density, hardness, bending strength, and fracture toughness of B₄C–SiC–TiB₂ composites are 99.6%, 32.61 GPa, 434 MPa, and 6.20 MPa m^1/2, respectively. Based on the microstructure observations and finite element modeling, the operative toughening mechanism is mainly attributed to the crack deflection along the grain boundary, which results from the residual stress field generated by the thermal expansion mismatch between B₄C and TiB₂ phase.     

Nanoindentation and TEM investigation of spark plasma sintered TiB2–SiC composite

The impact of adding 20 vol% SiC on the properties of TiB₂ was studied in this research. The spark plasma sintering (SPS) process was used as the preparation technique at 1850 °C, the resulted composite was characterized using X-ray diffraction (XRD), field emission electron probe micro analyzer, transmission electron microscopy (TEM), field emission scanning electron microscopy, energy dispersive X-ray analysis, and nanoindentation. The prepared composite presented a relative density of ～98.5%. XRD and TEM results confirmed the in-situ formation of graphite; no in-situ TiC could be detected in the final microstructure of the composite. Forming a low melting point compound between SiO₂ and B₂O₃ oxides lead to the creation of wet interfaces between the ingredients. In terms of mechanical properties, the composite possessed Vickers hardness of 21.6 ± 2.2 GPa, flexural strength of 616 ± 28 MPa, fracture toughness of 5.3 ± 1.2 MPa m^1/2, and elastic modulus of 498 ± 12 GPa. According to the microstructural images, crack deflection, crack branching, crack arresting, crack bridging, and grain breaking events were found to be the main toughening mechanisms in this ceramic. In addition, the nanoindentation investigation indicated the role of SiC addition in improving the elastic modulus, hardness, and wear resistance of the prepared composite.     

Toughness mechanism and plastic insensitivity of submicron second phase Ta in a novel Ta–Hf6Ta2O17 composite ceramic

The introduction of metal-second phase can improve the fracture toughness of metal-ceramic composite (MCC) material, but usually degrades the strength and hardness. The pace of exploring the process and materials to both improve the toughness and hardness has never stopped. In this study, a novel Ta–Hf₆Ta₂O₁₇ composite ceramic is successfully prepared by spark plasma sintering. The effects of Ta content on microstructure and mechanical properties of the as-sintered ceramic are investigated. The fracture toughness of Ta–Hf₆Ta₂O₁₇ composite ceramic first increases and then decreased slightly with the increase in Ta content, reaching the maximum value of 4.21 ± 0.09 MPa m^1/2 at 20 vol% Ta. The improvement of the fracture toughness does not affect the hardness, whose value is stable between 16.74 GPa and 18.43 GPa. Based on the results of Selsing’s model, Raman spectra and TEM, it is confirmed that the toughness mechanism of Ta–Hf₆Ta₂O₁₇ composite ceramics originates from good inherent interface strength and crack deflection caused by the second phase. The maintenance of hardness comes from the plastic insensitivity of submicron Ta caused by the interfacial tensile stress, which provides a potential mechanism for the design of metal-ceramic composite with excellent strength and toughness.     

Novel (Zr,Ti)B2-(Zr,Ti)C-SiC ceramics via reactive hot pressing

Fully dense (Zr, Ti)B₂-(Zr, Ti)C-SiC ceramics were prepared by reactive hot-pressing using ZrB₂, TiC, and SiC as the initial materials for the first time. Effects of SiC addition on the microstructure evolution and mechanical properties were reported. The in-situ reaction between ZrB₂ and TiC as well as the SiC addition leads to the grain refinement. Besides, elongated (Zr, Ti)B₂ plate-like grains are obtained due to the occurrence of a transient liquid phase, which leads to the crack deflection in the matrix effectively. Mechanical properties are improved significantly due to grain-refinement and solid solution strengthening, and plate-like grains toughening effects. The ZrB₂-10 mol%TiC composite with 10 mol% SiC additional exhibits good comprehensive mechanical properties of the hardness of 20.2 GPa, the flexural strength of 803 MPa, and the fracture toughness of 5.7 MPa m^1/2.     

High hardness and high fracture toughness B4C-diamond ceramics obtained by high-pressure sintering

The B₄C-diamond composite with high hardness and toughness was first prepared by high-pressure sintering of B₄C and diamond powders at 5 GPa and 1600 °C. The effect of the diamond fraction on the densification, microstructure and mechanical properties of B₄C-diamond composite were investigated. The results indicated that the hardness of the as-prepared composite ceramics increased gradually with the increase in diamond content. The composite having 40 vol% diamond exhibited excellent comprehensive mechanical properties with a relative density of 98.3%, a density of 2.86 g/cm³, Vickers hardness of 39.8 GPa and fracture toughness of 8.1 MPa·m^1/2. The use of superhard diamond enhanced the fracture toughness of the B₄C while maintaining its lightweight and high hardness. The main toughening mechanisms were crack bridging, crack deflection and pull-out of homogeneously dispersed diamond grains. Superhard second phase dispersion high-pressure sintering provides a new technical route to improve the properties of advanced composites.     

The role of TiO2 incorporation in the preparation of B4C/Al laminated composites with high strength and toughness

We prepared B₄C/Al laminated composites via ice-templating and gas-aided pressure infiltration and investigated the effects of TiO₂ addition on the microstructures and mechanical properties of the composites. The incorporation of TiO₂ led to the formation of TiB₂ after sintering, reduced the formation of harmful phases and increased the strength of ceramic architectures. However, its excessive addition resulted in the cracking of ceramic layers and the formation of metal strips after Al infiltration. The bending strength, fracture toughness and work of fracture of the composites first increased and then decreased with increasing initial TiO₂ content, reaching maxima of 420?±?20?MPa, 44?±?2?MPa?m^1/2 and 5002?±?175?J?m^?2, respectively. The specific strength and toughness are comparable to those of titanium alloys. Furthermore, fracture modes and toughening mechanisms were thoroughly addressed by analyzing crack propagation paths and fracture surface morphologies. Crack deflection and metal bridging are two primary extrinsic toughening mechanisms.     

Spark plasma sintering of boron nitride micron tubes reinforced boron carbide ceramics with excellent mechanical property

In this paper, the novel boron nitride micron tubes (BNMTs) were used to reinforce commercial boron carbide (B₄C) ceramics prepared via spark plasma sintering technology. The effects of the sintering parameters, sintering temperature, the holding time, and the BNMTs content on the microstructure and mechanical properties of B₄C/BNMTs composite ceramics were studied. The results indicated that adding a proper amount of BNMTs could inhibit the grain growth of B₄C and improve the fracture toughness of the B₄C/BNMTs composite ceramics. The prepared composite ceramic sample with 5 wt% BNMTs at 1850°C, 8 min and 30 MPa displayed the best mechanical properties. The relative density, hardness, fracture toughness, and bending strength of the samples were 99.7% ± .1%, 35.62 ± .43 GPa, 6.23 ± .2 MPa m^1/2, and 517 ± 7.8 MPa, respectively. Therein, the corresponding value of hardness, fracture toughness, and bending strength was increased by 10.3%, 43.59%, and 61.5%, respectively, than that of the B₄C/BNMTs composite ceramic without BNMTs. It was proved that the high interface binding energy and bridging effect between boron carbide and BNMTs were the toughening principle of BNMTs.     

Effects of residual stress and intragranular particles on mechanical properties of hot-pressed Al2O3/SiC ceramic composites

Al₂O₃/SiC ceramic composites with different SiC contents have been prepared by powder metallurgy at 1600 °C for 120 min at 30 MPa pressure. The effect of second phase particles on the microstructure and mechanical properties of composites have been studied. The results show that SiC particle has a significant impact on the matrix subjected to residual stress, and on the microstructure of the composites as well. The average grain size of alumina matrix decreases as the SiC particle content increases. Simultaneously, it has been found that the mechanical properties of the material are significantly enhanced in comparison with monolithic Al₂O₃. The highest strength and toughness are obtained when the SiC content is 15 vol%, and the values are 1237 MPa and 5.68 MPa m^1/2, respectively. The mechanisms of strengthening and toughening have been discussed.     

Microstructure and mechanical properties of reaction-hot-pressed zirconium diboride based ceramics

ZrB₂ ceramics were prepared by in-situ reaction hot pressing of ZrH₂ and B. Additions of carbon and excess boron were used to react with and remove the residual oxygen present in the starting powders. Additions of tungsten were utilized to make a ZrB₂-4 mol%W ceramic, while a change in the B/C ratio was used to produce a ZrB₂-10 vol% ZrC ceramic. All three compositions reached near full density. The baseline ZrB₂ and ZrB₂–ZrC composition contained a residual oxide phase and ZrC inclusions, while the W-doped composition contained residual carbon and a phase that contained tungsten and boron. All three compositions exhibited similar values for flexure strength (~520 MPa), Vickers hardness (~15 GPa), and elastic modulus (~500 to 540 GPa). Fracture toughness was about 2.6 MPa m^1/2 for the W-doped ZrB₂ compared to about 3.8 MPa m^½ for the ZrB₂ and ZrB₂–ZrC ceramics. This decrease in fracture toughness was accompanied by an observed absence of crack deflection in the W-doped ZrB₂ compared with the other compositions. The study demonstrated that reaction-hot-pressing can be used to fabricate ZrB₂ based ceramics containing solid solution additives or second phases with comparable mechanical properties.     

Influence of graphite nano-flakes on densification and mechanical properties of hot-pressed ZrB2–SiC composite

Hot pressed monolithic ZrB₂ ceramic (Z), ZrB₂–20 vol% SiC composite (ZS₂₀) and ZrB₂–20 vol% SiC–10 vol% nano-graphite composite (ZS₂₀G_n10) were investigated to determine the influence of graphite nano-flakes on the sintering process, microstructure, and mechanical properties (Vickers hardness and fracture toughness) of ZrB₂–SiC composites. Hot pressing at 1850 °C for 60 min under 20 MPa resulted in a fully dense ZS₂₀G_n10 composite (relative density: 99.6%). The results disclosed that the grain growth of ZrB₂ matrix was efficiently hindered by SiC particles as well as graphite nano-flakes. The fracture toughness of ZS₂₀G_n10 composite (7.1 MPa m^1/2) was essentially improved by incorporating the reinforcements into the ZrB₂ matrix, which was greater than that of Z ceramic (1.8 MPa m^1/2) and ZS₂₀ composite (3.8 MPa m^1/2). The fractographical observations revealed that some graphite nano-flakes were kept in the ZS₂₀G_n10 microstructure, besides SiC grains, which led to toughening of the composite through graphite nano-flakes pull out. Other toughening mechanisms such as crack deflection and branching as well as crack bridging, due to the thermal residual stresses in the interfaces, were also observed in the polished surface.     

Transition metal diboride-silicon carbide-boron carbide ceramics with super-high hardness and strength

Three phase boride and carbide ceramics were found to have remarkably high hardness values. Six different compositions were produced by hot pressing ternary mixtures of Group IVB transition metal diborides, SiC, and B₄C. Vickers’ hardness at 9.8 N was ~31 GPa for a ceramic containing 70 vol% TiB₂, 15 vol% SiC, and 15 vol% B₄C, increasing to ~33 GPa for a ceramic containing equal volume fractions of the three constituents. Hardness values for the ceramics containing ZrB₂ and HfB₂ were ~30% and 20% lower than the corresponding TiB₂ containing ceramics, respectively. Hardness values also increased as indentation load decreased due to the indentation size effect. At an indentation load of 0.49 N, the hardness of the previously reported ceramic containing equal volume fractions of TiB₂, SiC and B₄C was ~54 GPa, the highest of the ceramics in the present study and higher than the hardness values reported for so-called “superhard” ceramics at comparable indentation loads. The previously reported ceramic containing 70 vol% TiB₂, 15 vol% SiC, and 15 vol% B₄C also displayed the highest flexural strength of ~1.3 GPa and fracture toughness of 5.7 MPa·m^1/2, decreasing to ~0.9 GPa and 4.5 MPa·m^1/2 for a ceramic containing equal volume fractions of the constituents.