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.     

B4C-based hard and tough ceramics densified via spark plasma sintering using a novel Mg2Si sintering aid

Full-dense B₄C-based ceramics with excellent mechanical properties were fabricated using spark plasma sintering with Mg₂Si as a sintering aid at a low temperature of 1675 °C while applying a uniaxial pressure of 50 MPa. The effect of Mg₂Si addition on the densification behaviours, mechanical properties and microstructure of as-sintered ceramics were investigated. Not only did the formation of ultra-fine grained SiC using the in-situ reaction effectively inhibit the growth of B₄C grains, but it also contributed to the strength and toughness of the resultant ceramics. Additionally, microalloying Mg imparted more metal bonding characteristics to the B₄C matrix, thereby improving their ductility. The results indicate that the composite containing 7 wt% Mg₂Si had excellent mechanical properties, including a light weight of 2.54 g/cm³, Vickers hardness of 34.3 GPa, fracture toughness of 5.09 MPa m^1/2 and flexural strength of 574 MPa.     

Microstructure and mechanical properties of hot-pressed B4C/TiC/Mo ceramic composites

Boron carbide (B₄C)/TiC/Mo ceramic composites with different content of TiC were produced by hot pressing. The effect of TiC content on the microstructure and mechanical properties of the composites has been studied. Results showed that chemical reaction took place for this system during hot pressing sintering, and resulted in a B₄C/TiB₂/Mo composite with high density and improved mechanical properties compared to monolithic B₄C ceramic. Densification rates of the B₄C/TiC/Mo composites were found to be affected by additions of TiC. Increasing TiC content led to increase in the densification rates of the composites. The sintering temperature was lowered from 2150 °C for monolithic B₄C to 1950 °C for the B₄C/TiC/Mo composites. The fracture toughness, flexural strength, and hardness of the composites increased with increasing TiC content up to 10 wt.%. The maximum values of fracture toughness, flexural strength, and hardness are 4.3 MPa m^1/2, 695 MPa, and 25.0 GPa, respectively.     

Investigation the effect of FeNiCoCrMo HEA addition on properties of B4C ceramic prepared by spark plasma sintering

In this study, monolithic B₄C and B₄C-based ceramics incorporating FeNiCoCrMo dual-phase (FCC and BCC) high entropy alloys (HEAs) were produced by spark plasma sintering (SPS). The effect of additives on the densification behavior, mechanical properties, microstructures, and phase evaluation of the samples were investigated. X-ray analysis confirmed the existence of FCC structured HEA and depletion of BCC structured HEA, after high-temperature reaction between B₄C-HEAs. The addition of HEAs enhanced the densification behavior by liquid phase sintering. Furthermore, hardness and fracture toughness values of the samples increased with increasing HEAs content. Fracture toughness and hardness values for all composites were higher than the monolithic B₄C. A combination of the highest density (∼99.22 %) and the best mechanical properties (32.3 GPa hardness and 4.53 MPa m^1/2 fracture toughness) was achieved with 2.00 vol.% HEA addition.     

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.     

Microstructure and mechanical properties of B4C matrix composites prepared via hot-pressing sintering with Pr6O11 as additive

High-performance B₄C-PrB₆ composites were prepared via hot-pressing sintering with matrix phase B₄C and with 2–5 wt% Pr₆O₁₁ as additive. The effects of different sintering processes and Pr₆O₁₁ content on the microstructure and mechanical properties of the composites were studied in detail. It is found that increasing sintering temperature and pressure will contribute to the densification of B₄C-PrB₆ composites. Coarse grains are formed in B₄C without additives at high temperature conditions, resulting in the decrease of the densification. Pr₆O₁₁ can effectively hinder the formation of coarse grains and finally promote the densification of the composites. The main toughening mechanisms of composites was crack deflection. The composites with 4 wt% Pr₆O₁₁ prepared at 2050 °C and 25 MPa had the best comprehensive mechanical properties. The relative density, hardness, flexural strength and fracture toughness reached to 98.9%, 37.6 GPa, 339 MPa and 4.4 MP am^1/2, respectively.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

Rapid synthesis of Ti3AlC2/TiB2 composites by the spark plasma sintering (SPS) technique

Dense Ti₃AlC₂/TiB₂ composites were successfully fabricated from B₄C/TiC/Ti/Al powders by spark plasma sintering (SPS). The microstructure, flexural strength and fracture toughness of the composites were investigated. The experimental results indicate that the Vickers hardness increased with the increase in TiB₂ content. The maximum flexural strength (700 ± 10 MPa) and fracture toughness (7.0 ± 0.2 MPa m^1/2) were achieved through addition of 10 vol.% TiB₂, however, a slight decrease in the other mechanical properties was observed with TiB₂ addition higher than 10 vol.%, which is believed to be due to TiB₂ agglomeration.     

High-performance B4C matrix composites fabricated from the B4C–Si–CeO2 system via reactive hot pressing

Boron carbide (B₄C) matrix composites had the advantages of high hardness, high melting point and low density. However, due to the low relative density and poor fracture toughness of B₄C, its comprehensive properties were limited in engineering applications. In this work, in order to improve the comprehensive properties of B₄C composites, B₄C–SiC–SiB₆–CeB₆ composites were designed and fabricated via reactive hot pressing at 2050 °C and 20 MPa with B₄C matrix and novel additives (Double doping of Si and CeO₂) as raw materials. The effects of additive CeO₂ content on the microstructures and mechanical properties of composite were investigated, and reaction mechanisms of B₄C, Si and CeO₂ at different temperatures were studied in detail. The work showed that liquid phase Si and SiB₆ greatly improved the densification of composites. CeB₆ played an indispensable role in the formation of SiC–SiB₆ agglomerate structure, increasing strength and supplementing toughness. When the content of CeO₂ was 6 wt%, the relative density, hardness, flexural strength and fracture toughness reached to 99.7%, 34.9 GPa, 461.46 MPa and 5.57 MPa m^1/2, respectively. Our strategy benefited from the formation of two liquid phases and SiC–SiB₆ agglomerate structure, showing great potential in promoting sintering and improving fracture toughness.     

High-strength TiB2-B4C composite ceramics sintered by spark plasma sintering

Spark plasma sintering (SPS) is an advanced sintering technique because of its fast sintering speed and short dwelling time. In this study, TiB₂, Y₂O₃, Al₂O₃, and different contents of B₄C were used as the raw materials to synthesize TiB₂-B₄C composites ceramics at 1850°C under a uniaxial loading of 48 MPa for 10 min via SPS in vacuum. The influence of different B₄C content on the microstructure and mechanical properties of TiB₂-B₄C composites ceramics are explored. The experimental results show that TiB₂-B₄C composite ceramic achieves relatively good comprehensive properties and exceptionally excellent flexural strength when the addition amount of B₄C reaches 10 wt.%. Its relative density, Vickers hardness, fracture toughness, and flexural strength reach to 99.20%, 24.65 ± .66 GPa, 3.16 MPa·m^1/2, 730.65 ± 74.11 MPa, respectively.     

Performance of B4C/CeB6 composites fabricated via hot pressing under different processes

In this work, CeO₂ sintering additive reinforced B₄C ceramic composites were prepared by hot-pressing reaction sintering under different processes of low temperature–long holding time (1980°C, 30 MPa, 3 h, 4 wt% CeO₂) and high temperature–short holding time (2050°C, 30 MPa, .5 h, 4 wt% and 6 wt% CeO₂). The effect of sintering process and CeO₂ content on the microstructure and mechanical properties of B₄C-CeB₆ composites were investigated. The existed impurities in the obtained composites were also analyzed. Results show that CeO₂ is an active sintering additive. CeB₆ is formed by the reaction between CeO₂, B₄C and C in sintering process. The densification of B₄C ceramics is enhanced, and the grains can be refined by the formed CeB₆, which promotes the strength. The thermal expansion coefficient mismatch, crack deflection, and fracture mode change caused by the in situ formed CeB₆ improve the toughness. The process of low temperature–long holding time is more suitable for playing the role of CeO₂ additive in sintering of B₄C, under which condition the relative density, flexural strength, fracture toughness, and hardness reach 99%, 417 MPa, 5.32 MPa·m^1/2, and 30.66 GPa, respectively. The impurities in the composites are the kinds of Ti-contained, C-O-Mg-Ca-contained, C-O-Ca-S-contained, and Si-contained impurities.     

Preparation and characterization of reduced graphene oxide-reinforced boron carbide ceramics by self-assembly polymerization and spark plasma sintering

A self-assembly polymerization process was used to prepare graphene oxide/boron carbide (GO/B₄C) composite powders, spark plasma sintering (SPS) was used to fabricate reduced graphene oxide/boron carbide (rGO/B₄C) composites at 1800 °C and 30 MPa with a soaking time of 5 min. The effects of rGO addition on mechanical properties of the composites, such as Vickers hardness, flexural strength and fracture toughness, were investigated. The results showed that GO/B₄C composite powders were successfully self-assembled and a network structure was formed at high GO contents. The flexural strength and fracture toughness of rGO/B₄C composites were 643.64 MPa and 5.56 MPa m^1/2, respectively, at 1 and 2.5 wt.% rGO content, corresponding to an increase of 99.11% and 71.6% when compared to B₄C ceramics. Uniformly dispersed rGO in rGO/B₄C composites played an important role in improving their strength and toughness. The toughening mechanisms of rGO/B₄C composites were explained by graphene pull-out, crack deflection and bridging.     

Preceramic paper-derived Ti3Al(Si)C2-based composites obtained by spark plasma sintering

The paper describes the structure and properties of preceramic paper-derived Ti₃Al(Si)C₂-based composites fabricated by spark plasma sintering. The effect of sintering temperature and pressure on microstructure and mechanical properties of the composites was studied. The microstructure and phase composition were analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. It was found that at 1150 °C the sintering of materials with the MAX-phase content above 84 vol% leads to nearly dense composites. The partial decomposition of the Ti₃Al(Si)C₂ phase becomes stronger with the temperature increase from 1150 to 1350 °C. In this case, composite materials with more than 20 vol% of TiC were obtained. The paper-derived Ti₃Al(Si)C₂-based composites with the flexural strength > 900 MPa and fracture toughness of >5 MPa m^1/2 were sintered at 1150 °C. The high values of flexural strength were attributed to fine microstructure and strengthening effect by secondary TiC and Al₂O₃ phases. The flexural strength and fracture toughness decrease with increase of the sintering temperature that is caused by phase composition and porosity of the composites. The hardness of composites increases from ~9.7 GPa (at 1150 °C) to ~11.2 GPa (at 1350 °C) due to higher content of TiC and Al₂O₃ phases.     

Microstructure and mechanical behaviour of transient liquid phase spark plasma sintered B4C–SiC–TiB2 composites from a B4C–TiSi2 system

Almost fully-dense B₄C–SiC–TiB₂ composites with a high combination of strength and toughness were prepared through in situ reactive spark plasma sintering using B₄C and TiSi₂ as raw materials. The densification, microstructure, mechanical properties, reaction, and toughening mechanisms were explored. TiSi₂ was confirmed as a reactive sintering additive to promote densification via transient liquid-phase sintering. Specifically, Si formed via the reaction between B₄C and TiSi₂ that served as a transient component contributed to densification when it melted and then reacted with C to yield more SiC. Toughening mechanisms, including crack deflection, branching and bridging, could be observed due to the residual stresses induced by the thermoelastic mismatches. Particularly, the introduced SiC–TiB₂ agglomerates composed of interlocked SiC and TiB₂ played a critical role in improving toughness. Accordingly, the B₄C–SiC–TiB₂ composite created with B₄C-16 wt% TiSi₂ achieved excellent mechanical performance, containing a Vickers hardness of 33.5 GPa, a flexural strength of 608.7 MPa and a fracture toughness of 6.43 MPa m^1/2.     

High-performance B4C-YB4 composites fabricated with Y2O3 additive via hot-pressing sintering

The B₄C-YB₄ composites with good comprehensive properties were prepared by in-situ hot pressing sintering under the conditions of sintering temperature 1950–2050 °C, pressure 20 MPa and holding time 15 min using B₄C and Y₂O₃ as the raw materials. The phase composition, microstructure, mechanical properties of the composites fabricated with different contents of Y₂O₃ and different temperatures were studied, and the reaction mechanism, toughening and strengthing mechanism were explored. Y₂O₃ can react with B₄C to form YB₄, and 15B₄C+7Y₂O₃ = 14YB₄+2B₂O₃+15CO is the total reaction. With the increase of temperature, the mechanical properties of B₄C-YB₄ composites improve obviously, and the B₄C-YB₄ composites prepared with 3 wt% Y₂O₃ have the best performance. The relative density, hardness, flexural strength and fracture toughness of the B₄C-YB₄ composites fabricated at 2050 °C with 3 wt% Y₂O₃ are 97.00%, 34.84 GPa, 422.67 MPa and 4.92 MPa m^1/2 respectively. The good comprehensive properties are attributed to the uniform distribution and small size of the second phase YB₄, and the lower porosity. The coexistence of transgranular and intergranular fracture, and the phenomena such as crack bridging, deflection and microcracks contribute to the improvement of the toughness.     

Structure and mechanical properties of hot-pressed B4C-NdB6 composites

High-performance B₄C-NdB₆ composites were fabricated by hot-pressing sintering at the temperature of 2050 °C for 20 min holding time and 20 MPa pressure with Nd₂O₃ (1～4 wt%) as the aiditive. The effects of Nd₂O₃ on the sintering process of the B₄C were studied. The reaction mechanisms of B₄C and Nd₂O₃ at different temperature were investigated. Based on the results of TG-DSC and thermodynamic calculation,. NdB₆ was formed via Nd₂O₃ react with B₄C in the sintering process, which greatly enhanced the densification of B₄C and promoted the sintering process. The flexural strength, fracture toughness and hardness of the B₄C-NdB₆ composites rose to 366.42 MPa, 5.27 MPa m^1/2 and 38 GPa by adding 3 wt% Nd₂O₃, respectively. The coexistence of transgranular and intergranular fracture is the major fracture mode. The phenomenon of pull-out contributed to improvement of the fracture toughness.     

Preparation of B4C composites toughened by MoB2/Mo2B5-SiC interlocking structure via reactive hot pressing

B₄C composites toughened by MoB₂/Mo₂B₅-SiC interlocking structure were prepared via reactive hot pressing with B₄C and MoSi₂ as raw materials. The phase composition, microstructure, and mechanical properties of the fabricated B₄C composites were studied. The crack propagation and fracture surface were observed, and the toughening mechanism was analyzed. The results indicate that the interlocking structure of MoB₂/Mo₂B₅-SiC is formed in the obtained B₄C composites. The relative density, flexural strength, and fracture toughness of the B₄C composites reach 99.3%, 480 MPa, and 5.2 MPa·m^1/2, respectively, when the MoSi₂ content is 30 wt%. The hardness is 33 GPa when the MoSi₂ content is 20 wt%. The special laminar fracture of the interlocking structure of MoB₂/Mo₂B₅-SiC elongates the crack extending path and thus consumes more energy of crack extension. The phenomena of crack bridging and branching and the special laminar fracture of the interlocking structure have a synergistic effect on promoting the overall fracture toughness.     

Densification and mechanical properties of mullite/TiO2-coated B4C composites

Mullite/TiO₂-coated B₄C composites with up to 40 wt.% B₄C were fabricated by coating B₄C powders with Ti-chelate compounds via a sol-gel method prior to the hot-pressing of mullite/B₄C mixtures at 1600 °C for 1 h. The effects of TiO₂-coated B₄C on the densification and the mechanical properties of mullite/B₄C composites were investigated. TiO₂ reacts with B₄C at high temperatures to produce B₂O₃ and TiB₂, both seems to be favorable for the densification of mullite/B₄C composites. The formation of TiB₂, besides, may lead to the generation of thermal residual stresses, which is deemed to be beneficial to the fracture toughness but detrimental to the flexural strength. The mechanical properties of mullite/B₄C composites such as hardness, flexural strength and fracture toughness, are enhanced remarkably with the increasing addition of B₄C. However, with a B₄C addition more than 20 wt.%, the flexural strength tends to decrease gradually, probably due to the increasing residual stresses originated from the thermal mismatch of TiB₂ with mullite and B₄C matrix. B₄C contents above 30 wt.% easily cause the aggregation of B₄C particles in mullite matrix, which will lower the degree of improvement in fracture toughness.     

Correlation between phase content and mechanical properties of SiCw- ZTA composites sintered by SPS

The zirconia toughened alumina (ZTA) composites have been widely used as an engineering material in many application areas due to their remarkable mechanical properties. However, the fracture toughness of ZTA does not generally meet the requirements of aerospace, machinery and other fields. In this study, the SiC whiskers (SiC_w) have been incorporated in the ZTA composites to improve the fracture toughness. The SiC_w employed in this study mainly consist of the β phase, with a small fraction of the α phase. The effect of the SiC_w content and sintering temperature on the microstructure and mechanical properties of the SiC_w-ZTA (ZAS_w) composites has been systematically studied. The incorporation of SiC_w is noted to reduce the density of the ZAS_w composites. On enhancing the SiC_w content, the Vickers hardness and fracture toughness of the composites initially decrease, followed by an increase. However, the flexural strength of the composites increases with the SiC_w content. At a SiC_w content of 10.0 vol %, the strength, hardness and toughness are observed to reach the maximum values. On enhancing the sintering temperature, the strength and hardness of the composites are observed to remain nearly constant, while the toughness of the composites is increased.     

Microstructure and properties of bilayered B4C-based ceramics

Bilayered B₄C-based ceramics were obtained by hot-pressing. Microstructure, mechanical and ballistic properties of the bilayered ceramics were investigated. One layer was obtained upon addition of Ti and C to the hard B₄C matrix, the newly formed TiB₂ phase uniformly distributed in the matrix. The other layer included variable amounts of Ti₃SiC₂, equal to 10, 20, 30, 40 wt%, and the B₄C-SiC matrix in a fixed weight ratio of 7:3. The amount of TiB₂ and SiC phases, deriving from Ti₃SiC₂ decomposition upon sintering, increased with increasing the Ti₃SiC₂ content. The flexural strength and fracture toughness of bilayered ceramics both increased with increasing the Ti₃SiC₂ content from 10 to 40 wt%. Ballistic testing showed that the B₄C-based ceramic target containing 30 wt% Ti₃SiC₂ broken into pieces upon being impacted by a 12.7 mm armor-piercing incendiary (API) projectile, and effectively consumed the bullet energy and protected the backing plate from serious damage.