Pressureless sintered in situ toughened ZrB2-SiC platelets ceramics

ZrB₂-SiC composite ceramics were densified by pressureless sintering with addition of Si₃N₄ or MoSi₂ at temperatures that induced SiC anisotropic growth from particles to platelets, within a ZrB₂ matrix with rounded grains. Si₃N₄ addition resulted in the formation of large amounts of liquid phase which enhanced mass transfer mechanisms in terms of matrix grain growth and homogeneous distribution of SiC platelets having an aspect ratio of 3. On the contrary, MoSi₂ helped the densification with local formation of liquid phases leading to a finer matrix with finer SiC platelets, though more agglomerated and with a lower aspect ratio (about 2). These different microstructures had very different fracture properties values, namely a toughness of 3.8 MPa m^1/2 and a strength of 300 MPa for the Si₃N₄-doped composite; toughness of 5 MPa m^1/2 and strength of 410 MPa for the MoSi₂-doped one.     

Preparation of TiB2–SiC composites toughened with interlocking microstructure by self-assembled TiB2 plates

The spark plasma sintering (SPS) technique was found to effectively improve the mechanical properties of TiB₂–SiC ceramic by forming a unique interlocking structure. This study investigated the phase transition process of the hexagonal micro-platelets TiB₂ powders with self-assembled structure during the molten-salt-mediated carbothermal reduction and its effect on promoting the mechanical properties of TiB₂-based ceramics. It was found that the SPS approach ensured a highly densified TiB₂–SiC ceramics with enhanced Vickers hardness of 21.0 ± 1.3 GPa and fracture resistance of 7.8 ± 0.3 MPa m^1/2. The performance enhancement of the resultant TiB₂–SiC composite was attributed to the interlocking structure from the original anisotropic TiB₂ powders, which could effectively absorb the energy and facilitate the crack deflection.     

Diffusion bonding of ZrB2–SiC/Nb with in situ synthesized TiB whiskers array

The ZrB₂–20 vol.% SiC (ZS) composites were diffusion bonded to Nb using pure Ti interlayer. Effects of joining temperature on the microstructure and mechanical properties of the joints were investigated. The results show that Ti reacted with Nb and ZS to form a typical three layers in the joint. An in situ synthesized TiB whiskers array which consisted of two types of TiB was produced in the reaction layer. The formation mechanism of TiB was analyzed. Mutual diffusion between Ti and Nb led to a ductile β-(Ti, Nb) layer on Nb side. Joining temperature influenced the thickness of reaction layers and distribution of TiB seriously. The maximum shear strength reached 158 MPa with bonding temperature at 1200 °C for 60 min.     

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.     

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.     

Effects of SiC amount and morphology on the properties of TiB2-based composites sintered by hot-pressing

This investigation intended to assess the influence of SiC morphology on the sinterability and physical-mechanical features of TiB₂-SiC composites. For this aim, different volume percentages of SiC particles and SiC whiskers were introduced to TiB₂ samples hot-pressed at 1950 °C for 2 h under an external pressure of 25 MPa. The characterization of as-sintered specimens was carried out using X-ray diffraction, optical microscopy, and scanning electron microscopy. The relative density studies revealed that SiC_w had a more significant impact on the sinterability of TiB₂-based composites. The XRD investigation confirmed the production of an in-situ TiC phase during the hot-pressing; however, some peaks related to the graphitized carbon also appeared in the patterns of SiC_w-doped ceramics. The addition of 25 vol% SiC_p halved the average grain size of TiB₂ while introducing the same content of SiC_w decreased this value by just around 20%. Finally, the highest Vickers hardness and fracture toughness were obtained for the sample reinforced with 25 vol% SiC_w, standing at 29.3 GPa and 6.1 MPa m^1/2, respectively.     

Microstructure and mechanical properties of in situ synthesized (TiB2 + TiC)/Ti3SiC2 composites

Based on thermodynamic analysis, highly dense (TiB₂ + TiC)/Ti₃SiC₂ composite ceramics with different TiB₂ volume contents were in situ fabricated in situ by hot-pressing at 1500 °C. Laminar Ti₃SiC₂ grains, columnar TiB₂ grains and equiaxed TiC grains were clearly identified from microstructural observation; grain boundaries were clean. The increase of TiB₂ volume content significantly restrains the grain growth of the Ti₃SiC₂ matrix. As the content of TiB₂ increases from 5 vol.% to 20 vol.%, the bending strength and fracture toughness of the composites both increase and then decrease, whereas the Vickers hardness increases linearly from 6.13 GPa to 11.5 GPa. The composite with 10 vol.% TiB₂ shows the optimized microstructure and optimal mechanical properties: 700 MPa for bending strength; 9.55 MPa m^1/2 for fracture toughness. These are attributed to the synergistic action of strengthening and toughening mechanisms such as particulate reinforcement, crack deflection, grain's pull-out and fine-grain toughening, caused by the columnar TiB₂ grains and equiaxed TiC grains.     

Assessing fracture toughness in sintered Al2O3–ZrO2(3Y)–SiC ceramic composites through indentation technique

Al₂O₃–ZrO₂(3Y)–SiC ceramic composites were prepared by spark plasma sintering. The fracture toughness (K_1C) of the material was evaluated by indentation technique using different types of empirical formulas between 29.4 N and 98 N. The calculated K_1C values depend on the crack profile and the applied load. By analyzing the relationship between the indentation radius and the crack length and the crack profile, the crack form of the composite is determined as a Palmqvist crack. Raman spectra result shows that ZrO₂ has a significant martensitic phase transformation when the applied load is 5 kg or higher. Additionally, the K_1C value decreases slightly as the load increases. The equation based on the Palmqvist crack system and the curve fitting equation are more suitable for the calculation of the K_1C value of the material. The composite exhibits a combination of various toughening mechanisms, such as crack deflection and bridging, thereby improving the fracture toughness of the material.     

Effects of in situ synthesized mullite whiskers on flexural strength and fracture toughness of corundum-mullite refractory materials

The method of in situ synthesis of mullite whiskers was introduced to improve the fracture toughness of the corundum-mullite refractory materials. Effects of process parameters (sintering temperature, holding time and addition amount of V₂O₅) on flexural strength and fracture toughness of corundum-mullite during the in situ toughening course were analyzed. The optimum process parameters (the sintering temperature of 1350 °C, the holding time of 2 h, and the V₂O₅ addition amount of 5%) for in situ synthesized mullite whiskers to toughen corundum-mullite were obtained by the response surface method combined with single factor analysis. SEM and EDS analysis results demonstrated that the mullite whiskers had been synthesized in corundum-mullite and they could bridge the cracks during the fracture process. After in situ toughening, the flexural strength versus deflection curves of corundum-mullite showed obvious zigzag or waveform characteristics, indicating in situ toughening effects. At the same time, the flexural strength and corresponding deflection increased remarkably.     

无压烧结碳化硅复合材料的制备与性能研究

以部分碳化钛为增强相投入到碳化硅基体材料中,并投入微量炭黑和碳化硼为烧结活化剂,利用无压固相烧结技术制造了碳化硅基陶瓷复合材料。评测了其力学性能,凭借扫描电镜(SEM)观测了试样的断口形貌与表观形貌,并探讨了其氧化行为。结果表明:在碳化硅中投加部分碳化钛,对复合材料的力学性能有非常大地益处,于9 wt%时达到顶峰,弯曲强度497 MPa,相对密度98.9%,断裂韧性4.79 MPa·m^1/2。复合材料的显微组织构造紧致密实,TiC颗粒在SiC材料中的离散作用而激发的钉扎效果和裂纹偏移转向为其主要的增韧原理。在设定的氧化条件下(1200℃保温2 h),试样表面形成了一层较为致密并可以弱化氧化进程的氧化膜层。     

Deformation and fracture mechanisms of in situ synthesized TiC reinforced TC4 matrix composites produced by selective laser melting

In this study, TiC/TC4 composites were fabricated using selective laser melting (SLM), and the deformation mechanism and fracture characteristics of the composites with nano-sized TiC particles formed in situ were studied. The experimental results showed that the rapid melting and solidification characteristics of SLM and the Marangoni effect of the liquid pool promoted a considerably homogeneous dispersion of the in situ-formed nanoscale-TiC reinforcement in the TiC/TC4 composites. In particular, an enhanced compressive strength of 1490.2 MPa and a considerable fracture elongation of 21.5% were simultaneously achieved for the TiC/TC4 composites, which could be attributed to the load transfer effect and the formation of denser and more uniformly distributed dimples. Combined with the finite element (FE) analysis, the uneven stress distribution in the shear band of the TiC/TC4 composites led to the fracture. Further, the fracture surface analysis showed that the in situ nanoscale TiC reinforcement promoted the fracture of microbubbles from the α/β interface with the concentrated distribution of the V element to the interface between TiC and the Ti matrix because of the load transfer, which promoted the uniform distribution of the V element in the dimple.     

Microstructure and mechanical properties of B4C–TiB2–SiC composites toughened by composite structural toughening phases

B₄C–TiB₂–SiC composites toughened by composite structural toughening phases, which are the units of (TiB₂–SiC) composite, were fabricated through reactive hot pressing with B₄C, TiC, and Si as raw materials. The units of (TiB₂–SiC) composite with the size of 10‐20 μm are composed of interlocking TiB₂ and SiC with the size of 1‐5 μm. The addition of TiC and Si can effectively promote the sintering of B₄C ceramics. The relative densities of all the B₄C composites with different contents of TiB₂ and SiC are close to completely dense (98.9%‐99.4%), thereby resulting in superior hardness (33.1‐36.2 GPa). With the increase in the content of TiB₂ and SiC, the already improved fracture toughness of the B₄C composite continuously increases (5.3‐6.5 MPa·m^1/2), but the flexure strength initially increases and then decreases. When cracks cross the units of the (TiB₂–SiC) composite, the cracks deflect along the interior boundary of TiB₂ and SiC inside the units. As the crack growth path is lengthened, the crack propagation direction is changed, thereby consuming more crack extension energy. The cumulative contributions improve the fracture toughness of the B₄C composite. Therefore, the composite structural toughening units of the (TiB₂–SiC) composite play an important role in reinforcing the fracture toughness of the composites.     

Residual stress and fracture toughness of sintered body of ZrO2-GO composite ceramics material

Zirconia ceramics and carbon-based materials are widely adopted in medical and dental applications due to their excellent biocompatibility and aesthetics. However, fracture toughness of ceramic materials limits their application in clinical dentistry because of the existence of residual stress. In this study, zirconia/graphene oxide (ZrO₂-GO) composite ceramics were fabricated by hot-press sintering. Residual stresses developed on the surface of ZrO₂-GO composite ceramics were evaluated by X-ray residual stress analysis and indentation techniques. The variation of surface residual stress with GO content was evaluated, and found to be consistent with that of fracture toughness. The generation of residual stress was found to be directly related to fracture toughness. Residual stress calculated by theoretical formula of indentation method was consistent with that measured by X-ray diffraction in line with the content of GO. Based on above results, it is concluded that 0.1–0.15 wt% GO composite ceramics possessed better mechanical properties.     

Development and evaluation of TiB2–AlN ceramic composites sintered by spark plasma

Titanium diboride (TiB₂) is a ceramic material with high mechanical resistance, chemical stability, and hardness at high temperatures. Sintering this material requires high temperatures and long sintering times. Non-conventional sintering techniques such as spark plasma sintering (SPS) can densify materials considered difficult to sinter. In this study, TiB₂–AIN (aluminum nitride) composites were sintered by using the SPS technique at different sintering temperatures (1500 °C, 1600 °C, 1700 °C, 1800 °C, and 1900 °C). x-ray diffraction was used to identify the phases in the composites. mechanical properties such as hardness and indentation fracture toughness was obtained using a vickers indenter. Different toughening mechanisms were identified, and good densification results were obtained using shorter times and lower temperatures than those previously reported.     

Pore and microstructure change induced by SiC whiskers and particles in porous TiB2–TiC–Ti3SiC2 composites

TiB₂–TiC–Ti₃SiC₂ porous composites were prepared through a plasma heating reaction using powder mixtures of Ti, B₄C SiC whiskers (SiC_w) and SiC particles (SiC_p). The effects of the SiC_w and SiC_p content on pore structures, phase constituents, microstructure, and crystal morphology of TiC were studied. The results show that TiC, TiB, Ti₃B₄ phases are formed within the 5Ti+B₄C system. With the addition of SiC_w and SiC_p, the TiB and Ti₃B₄ phases are reduced, sometimes even disappeared. Interestingly, the content of TiB₂ and TiC increased, resulting in Ti₃SiC₂ and TiSi₂ being formed. The porosity of composites increases notably with the addition of SiC_w. However, with the increase of SiC_p, the porosity of the composites first decreases, followed by an increase. After adding the specified amount of SiC_w/SiC_p, the compressive strength of composites are improved significantly. Additionally, the pore size of the composites are decreased significantly with the addition of SiC_w/SiC_p. During the plasma heating process, some Si atoms will diffuse into the TiC lattice, which in turn made the cubic TiC grains into hexagonal lamellar TiC or Ti₃SiC₂ grains.     

Relationship between fracture toughness characteristics and morphology of sintered Al2O3 ceramics

The influence of sintering temperature and soaking time on fracture toughness of Al₂O₃ ceramics has been investigated. The samples were prepared by solid state sintering at 1500, 1600 and 1700 °C for different soaking time periods. The fracture toughness of the sintered samples was determined by inducing cracks using Vickers indentation technique. Microstructural investigations on fracture surfaces obtained by three point bend test mode were made and correlated with fracture toughness. Crack deflection in the samples sintered at 1500 and 1600 °C for which ranges of fracture toughness are 5.2–5.4 and 5.0–5.6 MPa m^1/2 respectively, are found. The samples sintered at 1700 °C have lower fracture toughness ranging between 4.6 and 5.0 MPa m^1/2. These samples have larger grains and transgranular fracture mode is predominant. The crack deflection has further been revealed by SEM and AFM observations on fracture surface and fracture surface roughness respectively.     

Matrix cracking of 2D SiC/SiC composite characterized by in situ SEM and nano-CT

Two-dimensional plain-woven silicon carbide (SiC) fiber-reinforced SiC matrix (2D SiC/SiC) composite was prepared by polymer infiltration-pyrolysis (PIP). Matrix cracking mechanisms of the composite were investigated by in situ SEM and nano-CT to grasp tensile damage evolution. Results showed that PIP-SiC matrix possessed low-fracture energy with non-homogeneous distribution, leading to simultaneous initiation of matrix cracking outside transverse fiber bundles and in unreinforced regions. Cracks then got deflected along weak fiber/matrix interface, which accelerated crack proliferation within the composite. With an increase in the stress, cracks subsequently deflected along plain-woven layers and converged to form longitudinal macrocracks. The composite was finally delaminated via sliding.     

Microstructure development,hardness, toughness and creep behaviour of pressureless sintered alumina/SiC micro–nanocomposites obtained by slip-casting

Al₂O₃–SiC micro–nanocomposites are much more resistant materials than monolithic alumina regarding some mechanical properties. In order to study the possibility of obtaining creep resistant alumina/SiC micro–nanocomposites using inexpensive forming methods, alumina 1 and 5 vol% SiC materials were produced by slip-casting and pressureless sintering. Well-densified alumina–SiC pressureless sintered materials were obtained at 1700 °C for 2 h and attained 97–99% of the theoretical density. The microstructure, hardness and toughness were examined and 4-point flexure creep tests were performed at 1200 °C and 100 MPa in air. Compared with pure alumina materials, the creep resistance, toughness and hardness were enhanced drastically in materials containing 5 vol% of SiC.     

Fabrication and Properties of Multilayer Ceramics in the SiC – TiB2 System

The influence of the structure and residual stresses on the strength of multilayer composite ceramic materials in the SiC – MeB₂ system is studied. The composites are produced using slip casting of thin films, stacking and rolling of packets, and hot pressing. The use of β-SiC makes it possible to obtain SiC layers with a porous arch structure reinforced with columnar crystals. The high relaxation capacity of such structures eliminates the formation of cracks in fabrication of the material and provides a high strength. A thermal shock causes progressive local spalling with formation of spit-outs without macroscopic fracture of the material. A pilot process for fabricating multilayer ceramic composites is described.