Reactive hot pressing of zirconium diboride

The reaction of zirconium and boron was investigated as a potential route to form dense monolithic zirconium diboride (ZrB₂) ceramics. Attrition milling of the precursors produced nanosized (less than 100 nm) zirconium metal particles that reacted with boron to form ZrB₂ with an average particle size of less than 100 nm at temperatures as low as 600 °C. Scanning electron microscopy of ZrB₂ compacts heated to 1450 °C and 1650 °C showed average particle sizes of 0.6 μm and 1.0 μm, respectively, suggesting that the fine particle size was maintained during densification. Ceramics with a relative density of 99% were produced by hot pressing at 2100 °C. Dense ZrB₂ produced by the reactive hot pressing process had mechanical properties that were comparable to ceramics produced by conventional processes. The four-point flexure strength of ZrB₂ produced in this study was 434 MPa.     

Synthesis,microstructure and mechanical properties of Cr2AlC/Al2O3 in situ composites by reactive hot pressing

Al₂O₃ particle-reinforced Cr₂AlC in situ composites were successfully fabricated from powder mixtures of Cr₃C₂, Cr, Al, and Cr₂O₃ by a reactive hot-pressing method at 1400 °C. A possible synthesis mechanism was proposed to explain the formation of the composites in which Al₂O₃ was formed by the aluminothermic reaction between Al and Cr₂O₃, meanwhile, Cr₃C₂, Al, together with Cr reacted to form Cr₂AlC in a shortened reaction route. The effect of Al₂O₃ addition on the microstructure and mechanical properties of Cr₂AlC/Al₂O₃ composites was investigated. The results indicated that the as-sintered products consisted of Cr₂AlC matrix and Al₂O₃ reinforcement, and the in situ formed fine Al₂O₃ particles dispersed at the matrix grain boundaries. The flexural strength and Vickers hardness of the composites increased gradually with increasing Al₂O₃ content. But the fracture toughness peaked at 6.0 MPa m^1/2 when the Al₂O₃ content reached 11 vol.%. The strengthening and toughening mechanism was also discussed.     

Reactive hot pressing of TiC0.5 ceramic at low applied pressure with 1 wt% Ni additive

Densification in non-stoichiometric TiC_0.5 ceramic has been studied by reactive hot pressing (RHP) of Ti:0.5C composition at 4–40 MPa, 1200°C for 60 min. Incomplete reaction and 94% relative density (RD) at a pressure of 4 MPa changed to 99% RD and a negligible amount of residual Ti at 40 MPa. In contrast, the addition of 1 wt% Ni in the starting Ti-0.5C powder mixture resulted in full density at a lower pressure of 4 MPa, leading to comparable hardness. It is argued that both, reaction as well as densification, were improved by the formation of transient Ti-Ni liquid phase. The enhanced RD and residual metallic phase in the nickel-containing non-stoichiometric TiC_0.5 showed high flexural strength (537 ± 79 MPa), which is comparable to values obtained from materials processed at high temperature and pressure.     

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.     

Microstructure and anisotropic mechanical properties of B6.5C-TiB2-SiC-BN composites fabricated by reactive hot pressing

B_6.5C-TiB₂-SiC-BN composite ceramics were prepared by a novel solid-state reaction using TiCN, B, and Si as raw materials. The final products obtained by hot pressing at 1950 °C possessed a fine microstructure, homogeneous distribution, and excellent mechanical properties. The obtained bulk B_6.5C-TiB₂-SiC-BN composite ceramic shows a high relative density (98.8 %). The mechanical properties of the composites are anisotropic because of the orientation growth and structural characteristics of TiB₂ and h-BN grains. The values of hardness, bending strength, and fracture toughness measured along the hot-pressing direction were 19.6 GPa, 801 MPa, and 4.30 MPa m^1/2, respectively, which were higher than those measured perpendicular to the hot-pressing direction. The formation of twin structures in B_6.5C and SiC grains and the crack deflections induced by h-BN and TiB₂ grains are beneficial for improving the mechanical properties of these composites.     

Fabrication and mechanisms of densification of ZrB2-based ultra high temperature ceramics by reactive hot pressing

Dense ZrB₂–SiC (25–30 vol%) composites have been produced by reactive hot pressing using stoichiometric Zr, B₄C, C and Si powder mixtures with and without Ni addition at 40 MPa, 1600 °C for 60 min. Nickel, a common additive to promote densification, is shown not to be essential; the presence of an ultra-fine microstructure containing a transient plastic ZrC phase is suggested to play a key role at low temperatures, while a transient liquid phase may be responsible at temperatures above 1350 °C. Hot Pressing of non-stoichiometric mixture of Zr, B₄C and Si at 40 MPa, 1600 °C for 30 min resulted in ZrB₂–ZrC_x–SiC (15 vol%) composites of 98% RD.     

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.     

Reactive hot pressing of ZrB2-based composites with changes in ZrO2/SiC ratio and sintering conditions. Part I: Densification behavior

ZrB₂–SiC–ZrO₂ composites were hot pressed in order to investigate the effects of adding nano-sized ZrO₂ particles as well as the hot pressing parameters on the densification behavior of ZrB₂–SiC composites. An L9 orthogonal array of the Taguchi method was employed to study the significance of each parameter such as the sintering temperature, time, the applied external pressure, and ZrO₂/SiC volume ratio on the densification process. The statistical analyses revealed that among the mentioned parameters, the hot pressing temperature had a great influence over the densification. By being hot pressed at 1850 °C for 90 min under 16 MPa, fully dense ZrB₂-based composites were obtained. The relative density of the composites decreased at first and then enhanced as a function of ZrO₂/SiC ratio. Microstructural investigation of the fracture surfaces of the composites, which was carried out using the SEM analysis, showed the formation of new phases on the surfaces of SiC grains. The EDS and XRD analyses identified the ZrC as the newly formed interfacial phase due to the reaction between nano-ZrO₂ and SiC. The ZrC acted as an adhesive interphase between the ZrB₂/SiC grains, which could assist the sintering process.     

Microstructures and mechanical properties of B4C-TiB2-SiC composites fabricated by ball milling and hot pressing

B₄C-TiB₂-SiC composites were fabricated via hot pressing using ball milled B₄C, TiB₂, and SiC powder mixtures as the starting materials. The impact of ball milling on the densification behaviors, mechanical properties, and microstructures of the ceramic composites were investigated. The results showed that the refinement of the powder mixtures and the removal of the oxide impurities played an important role in the improvement of densification and properties. Moreover, the formation of the liquid phases during the sintering was deemed beneficial for densification. The typical values of relative density, hardness, bending strength, and fracture toughness of the composites reached 99.20%, 32.84?GPa, 858?MPa and 8.21?MPa?m^1/2, respectively. Crack deflection, crack bridging, crack branching, and microcracking were considered to be the potential toughening mechanisms in the composites. Furthermore, numerous nano-sized intergranular/intragranular phases and twin structures were observed in the B₄C-TiB₂-SiC composite.     

In situ synthesis,mechanical properties,and microstructure of reactively hot pressed WB4 ceramic with Ni as a sintering additive

In this study, tungsten tetraboride (WB₄) ceramics were synthesized in situ from powder mixtures of W and amorphous B with Ni as a sintering aid by reactive hot pressing method. The as-synthesized ceramics exhibited porosity as low as 0.375% and ultra-high Vickers hardness (H_v), as much as 49.808?±?1.683?GPa (for the low load of 0.49?N). It was seen that the addition of Ni greatly improved the sinterability of WB₄ ceramic. Besides, the flexural strength and fracture toughness of WB₄ ceramic were measured for the first time to be 332.857?±?36.763?MPa and 4.136?±?0.259?MPa?m^1/2, respectively, suggesting that the ceramic has good mechanical properties. The effects of sintering temperature and holding time on the densification, Vickers hardness, and mechanical properties of WB₄ ceramics were also investigated systematically as part of our study. The results indicated that increasing the sintering temperature can obviously improve the densification and mechanical properties of the ceramics. The bulk density and Vickers hardness of WB₄ ceramic sintered at 1650?°C for 60?min under 30?MPa revealed the highest values of 6.366?g?cm^?3 and 27.948?±?0.686?GPa (for the high load of 9.8?N), respectively. The flexural strength increased to the highest value of 332.857?±?36.763?MPa for sintering temperature up to 1550?°C, but decreased slightly as the sintering temperature further increased to 1650?°C. On the other hand, the fracture toughness increased gradually with increasing temperature. It was also found that Vickers hardness showed a similar trend as the densification of the samples with increasing temperature and holding time. Besides, no obvious improvements in the densification, mechanical properties, and Vickers hardness of the samples with sintering time were observed in this study. The microstructure and fracture behaviours of the as-synthesized WB₄ ceramic were also revealed, and the toughening mechanism has been discussed.     

Influence of B4C nanoparticles on mechanical behaviour of Silicon brass nanocomposite through mechanical alloying and hot pressing

This research article has concentrated to develop a novel silicon brass of [82Cu4Si14Zn]_100-x – x wt.% B₄C (x = 0, 3, 6, 9, and 12) nanocomposites which were synthesized by mechanical alloying followed by vacuum hot pressing for consolidation of powders into bulk samples. Single vial planetary ball mill was used to synthesize the nanocomposite powders in which the ball-to-powder ratio of 10:1 with the milling time of 20 h was used. The milled powders were compacted and sintered simultaneously using vacuum hot pressing equipment for 1 h at 900 °C. The structural, mechanical and tribological properties were characterized and investigated by x-ray line profile analysis (XRD), scanning electron microscopy (SEM), electron backscattered diffraction images (EBSD), energy dispersive x-ray spectroscopy (EDS), Vickers microhardness, compression test, and dry sliding wear behaviour analysis. It has been found that B₄C nanoparticles had homogeneously distributed and embedded in the nanocrystallite matrix. As a result, the fabricated nanocomposites were exhibited superior properties than the conventional alloy. Here, 12 wt% B₄C reinforced silicon brass of bulk nanocomposite was produced higher hardness and compressive strength than the unreinforcement matrix. Further, the worn morphologies were evidenced the mild wear occurred at higher reinforced nanocomposites owing to decohesion and lower wear rate with considerable wear resistance.     

Effects of Ta2O5 on mechanical properties and elements diffusion of Ti/Al2O3 composites prepared via hot pressing sintering

Homogeneous Ti/Al₂O₃ composites with different volume percentages of Ta₂O₅ addition were prepared at different temperatures via hot pressing sintering. Laminated Ti/Al₂O₃ composites with different volume percentages of Ta₂O₅ added were prepared. The effects of Ta₂O₅ on the composition, microstructure, mechanical properties and elements diffusion of the composites were characterized and investigated. Ta₂O₅ inhibited the production of TiAl and Ti₃Al by forming solid solution with Ti or new reaction product of Al. This solid solution melted and filled the void of Al₂O₃ phase to increase the density of Ti/Al₂O₃ composites at high temperature. Mechanical properties had also been improved by this phenomenon. Because Al element couldn’t diffuse in Ta or react with it, Al couldn’t diffuse through the Ta-enriched area at the interface of Ti and Al₂O₃.     

Mechanical and tribological properties of alumina-MWCNTs composites sintered by rapid hot-pressing

Alumina – MWCNTs composites were prepared using a novel approach. This process comprises functionalization of MWCNTs and stabilization of alumina-MWCNTs dispersion with subsequent freezing, which resulted in formation of granulated powders with homogeneous distribution of MWCNTs. The granulated powders were sintered by rapid hot pressing (RHP) at 1550 °C. Relative densities, microstructural analysis, tribological properties, fracture toughness and bending strength of prepared composites were investigated to reveal the effect of MWCNTs. Compared to pure alumina, bending strength and fracture toughness of dense alumina-5 vol.% MWCNTs composites decreased about 37% and 18%, respectively. At higher MWCNT contents, strength remained almost constant and fracture toughness slightly increased. Thus, the positive effect of CNTs on fracture toughness was demonstrated despite their counteracting effect on the refinement of the microstructure.     

The microstructure and mechanical properties of Ni/Al2O3 composites by in-situ generated CaAl12O19 and ZrO2 via hot pressing sintering

Ni/Al₂O₃ composites with a varying mass fraction of CaZrO₃ (0–12 wt%) were prepared by vacuum hot pressing sintering at 1650 °C under a pressure of 30 MPa for 30 min to investigate how CaZrO₃ affect the mechanical properties and morphology of the composites. The results show that CaZrO₃ can react with Al₂O₃ and form new strengthening and reinforcing phases of CaAl₁₂O₁₉ and ZrO₂, which can promote complete densification and solve the problem of uneven distribution due to the poor wettability between Al₂O₃ and Ni. Additionally, composites showed satisfactory mechanical properties when 6.0–9.0 wt% CaZrO3 was added and the major toughening mechanism involved the typical fracture of delamination and the transgranular mode.     

Study on mechanical properties of hot pressing sintered mullite-ZrO2 composites with finite element method

In this study, mullite–zirconia (ZrO₂) composites were fabricated by hot pressing sintering method. The effects of sintering temperature and holding time on the microstructures, phase compositions and mechanical properties of the composites were investigated. The results indicated that the size of t-ZrO₂ grain varies with sintering temperature and holding time, and the maximum flexural strength of 674.05?MPa and fracture toughness of 12.08?MPam^1/2 are obtained when the sintering temperature is 1500?°C with holding times of 20 and 60?min, respectively. Finite element method was employed to analyze the relationship between grain size and mechanical properties of mullite–ZrO₂ composites for the first time. The results showed that the maximum stress on mullite–ZrO₂ interface increases with the growth of t-ZrO₂ grain size, which enhances the generation and propagation of cracks on grain boundaries significantly and degrades the flexural strength and fracture toughness of the mullite–ZrO₂ composite ceramics.     

Fabrication of ZrB2 ceramics by reactive hot pressing of ZrB and B

Zirconium diboride (ZrB₂) ceramics were prepared by reactive hot pressing of ZrB+B powder mixture. Formation of a transient liquid due to eutectic reaction of ZrB₂+Zr→L_eu(ZrB2+Zr) at 1661°C following peritectic decomposition of 2ZrB=ZrB₂+Zr at 1250°C during heating up of the ZrB+B mixture facilitated densification. The liquid phase was subsequently eliminated via reaction of B with Zr in the eutectic liquid L_eu(ZrB2+Zr) to result in a dense ZrB₂ ceramic. Full density was reached after reactive hot pressing at 1900°C under 30 MPa for 1 h. The ZrB₂ ceramic had a refined microstructure consisting of grains of <1.5 μm in size and relatively good Vickers hardness (21 ± 2 GPa) and flexural strength (595 ± 63 MPa).     

Preparation and mechanical properties of SiCw-Al2O3-YAG ceramic composite by hot oscillatory pressing

SiC_w-Al₂O₃-YAG ceramic composites were prepared by hot oscillatory pressing (HOP) and traditional hot pressing (HP). The results showed that compared with static pressure, the oscillatory pressure could effectively promote densi?cation and mechanical properties of the composites. The sample prepared by HOP exhibited higher hardness (15.72 ± 0.20 GPa) and fracture toughness (7.13 ± 0.19 MPa m^1/2). The current work suggests that HOP could be an effective technique for the preparation of whisker reinforced ceramic composites.     

Microstructure and mechanical properties of Cf/ZrC composites fabricated by reactive melt infiltration at relatively low temperature

Carbon fiber-reinforced zirconium carbide matrix composites (C_f/ZrC) were prepared by vacuum infiltrating porous carbon/carbon preforms with molten Zr₂Cu alloy at 1200 °C. X-ray diffraction, scanning electron microcopy and transmission electron microscopy analysis were used to characterize the composition and microstructure of the final composites. It was found that the matrix of the composites were composed of the Cu–Zr–C amorphous phase dispersed with either single- or polycrystalline ZrC. Based on the microstructural analysis, the formation mechanism of the matrix was proposed to be a solution-precipitation and grain coalescence process. The influence of the heat treatment at 1800 °C was also investigated. Results indicated that at very high temperature the volatilization of residual metal somewhat deteriorated the flexural strength and the elastic modulus, but the fracture toughness of the composites was improved due to the sintering of ZrC grains.     

Effect of Ge on microstructure and mechanical properties of Ti3SiC2/Al2O3 composites

Owing to the good physicochemical compatibility and complementary mechanical properties of Ti₃SiC₂ and Al₂O₃, Ti₃SiC₂/Al₂O₃ composites are considered as ideal structural materials. However, TiC and TiSi₂ typically coexist during the synthesis of Ti₃SiC₂/Al₂O₃ composites through an in-situ reaction, which adversely affects the mechanical properties of the resulting composites. In this study, Ti₃SiC₂/Al₂O₃ composites were prepared via in-situ hot pressing sintering at 1450 °C. Ge, which was used as a sintering aid, improved the purity and mechanical properties of the Ti₃SiC₂/Al₂O₃ composites. This is because Ge replaced some of the Si atoms to compensate the evaporation loss of Si to form Ti₃(Si_1-xGe_x)C₂, which showed a crystal structure similar to that of Ti₃SiC₂. Furthermore, the molten Ge accelerated the diffusion reaction of the raw materials, increasing the overall density of the Ti₃SiC₂/Al₂O₃ composites. The optimum Ge amount for improving the mechanical properties of the composites was found to be 0.3 mol. The flexural strength, fracture toughness, and microhardness of the composite with the optimum Ge amount were 640.2 MPa, 6.57 MPa m^1/2, and 16.21 GPa, respectively. The formation of Ti₃(Si_1-xGe_x)C₂ was confirmed by carrying out X-ray diffraction, energy dispersive spectroscopy, and transmission electron microscopy analyses. A model crystal structure of Ti₃(Si_1-xGe_x)C₂ doped with 0.3 mol Ge was established by calculating the solid solubility of Ge.     

Microtopography and mechanical properties of vacuum hot pressing Al/B4C composites

Al/B₄C composites with various volume contents of B₄C (5%, 10%, 15%, 20%, and 25%) reinforcing the Al matrix, have been fabricated by vacuum hot press sintering at 680 °C, with a soaking time of 90 min and external pressure of 30 MPa. Mechanical properties, phase composition, and microstructure of the Al/B₄C composites are discussed to reveal the physical properties of the composites. Field emission transmission electron microscopy and selected area electron diffraction have been employed to verify the interior structure and crystal growth direction, respectively. The Vickers hardness, fracture strength, tensile strength, and maximum force attained the optimal values of 108.45 ± 4.02 HV, 585.70 ± 23.26 MPa, 196.18 ± 2.48 MPa, and 4.44 ± 0.17 kN, respectively, for 25 vol% B₄C/Al composites. The static compression strength increased before the 15 vol% B₄C addition and then decreased, acquiring the highest value of 292.15 ± 2.09 MPa for 15 vol% B₄C/Al composites. In general, the relative density and ductility of these composites consistently increased, with an increase in the volume content of Al, achieving a maximum of 99.22% and 54.63 ± 7.34%, respectively, for 5 vol% B₄C/Al composites.