Microstructures and mechanical properties of high-performance nacre-inspired Al-Si/TiB2 composites prepared by freeze casting and pressure infiltration

The nacre-inspired Al-Si/TiB₂ composites were successfully prepared by freeze casting and pressure infiltration. The microstructures and mechanical properties of nacre-inspired Al-Si/TiB₂ composites were studied by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and mechanical testing. The results show that the high performance of Al-Si/TiB₂ composites can be attributed to the clean interfaces between TiB₂ and Al and several toughening mechanisms, such as crack blunting, crack branching, crack deflection, plastic deformation of Al layer, and bridging of the uncracked fracture process zone. Specifically, the compressive strength, three-point bending strength and K_IC of composites corresponding to LS were 640–710 MPa, 629 MPa, and 16.4 MPa m^1/2, respectively. The fracture behaviors of the Al-Si/TiB₂ composites have been discussed in detail in this work. It was found that single cracks were accompanied by the propagation of multiple micro-cracks in the layered composites. The precipitation of Si particles at the TiB₂/α-Al interface and the Al phases infiltrated in the TiB₂ layers play a great role in the formation of single crack fractures and multiple micro-cracks fractures, respectively, in the nacre-inspired Al-Si/TiB₂ composites.     

Preparation and fracture behavior of bionic layered SiCp/Al composites by tape casting and pressure infiltration

In this study, the bioinspired laminated composites with alternating soft Al layers and hard SiCp/Al were fabricated through the tape casting followed by pressure infiltration. In-situ bending and digital image correlation technology (DIC) analysis were carried out on the laminated composites. The results showed that the uniform layers of SiCp/Al and Al were obtained with the thickness of 30 μm and 10 μm, respectively. The interfaces between layers had an intimated combination. The bending deformation process of the laminated composites could be divided into three stages, i.e., crack initiation, crack stable diffusion and crack propagation instability. During deformation, the laminated structure changed the state of strain and strain distribution, further restricted the development of the crack, and the whole materials presented a stepped fracture. This study provides support for preparation and fracture process analysis of biomimetic layered composites prepared by tape casting.     

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.     

Pressureless ultrafast sintering of near-net-shaped superhard isotropic B4C/rGO composites with Ti-Al additives

Superhard composites of B₄C reinforced with randomly-oriented reduced graphene oxide (rGO) nanoplatelets are manufactured by a near-net-shape fabrication route based on three successive steps. Firstly, aqueous colloidal processing is used for the environmentally-friendly preparation of a semi-concentrated multi-component slurry (B₄C as main component, Ti-Al as sintering additive, and rGO as toughening reinforcement), whose suitability for wet shaping is demonstrated by rheological measurements. Secondly, slip casting is used to produce robust green parts with shapes on demand and microstructures free of macro- and micro-defects. And thirdly, pressureless spark-plasma sintering (PSPS) is used for the ultrafast and energy-efficient densification of the green parts with shape retention. Measurements of shrinkage and hardness, as well as the microstructural observations, are used to identify suitable PSPS temperatures leading to obtaining isotropic B₄C/rGO composites that are superhard and almost twice as tough as the monolithic B₄C ceramics.     

Interface regulation mechanism of Ti doping on B4C/Al composites

The present work adopts a combination of theoretical calculation and experiment. Firstly, the Gibbs free energy enthalpy change of Ti doped B₄C/Al composites is calculated by thermodynamic principle, revealing the principle that Ti will preferentially combine with Al and B₄C to form TiB₂ with excellent performance. Secondly, with the help of spark plasma sintering (SPS) process, pure Al and 4 vol%Ti–Al was used to discuss the degree of interfacial reaction and diffusion between Al–B₄C and Ti/Al–B₄C. It is found that the addition of Ti effectively inhibits the interfacial reaction between Al–B₄C. The kinetic equation of Al diffusion distance and holding time is lnd = 0.66lnt+0.24. Finally, the phase and mechanical properties of two groups of B₄C/Al–Ti and B₄C/Al composites were analyzed. The results showed that the impurity phase of sintering products of Ti doped samples was greatly reduced compared with that of the non doped group, and the mechanical properties were also significantly improved. Ti doping effectively regulates the interfacial reaction of B₄C/Al composites, inhibits the formation of impurity brittle phase in the system, and optimizes the mechanical properties of the composites.     

Gel-cast hierarchical porous B4C/C preform and its role in fabricating reaction bonded boron carbide composites

The resorcinol-formaldehyde (RF) gel-casting system is employed for the first time to fabricate a hierarchical porous B₄C/C preform, which was subsequently used for the fabrication of reaction bonded boron carbide (RBBC) composites via a liquid silicon infiltration process. The effect of the carbon content and carbon structures of this perform on the microstructures and mechanical properties of B₄C/C preform and the resultant RBBC composites is reported. The B₄C/C preform (16 wt% carbon) exhibit a strength of 34±1 MPa. The obtained RBBC composites shown uniform microstructure is consisted of SiC particles bonded boron carbide scaffold and an interpenetrating residual silicon phase. The Vickers hardness, flexural strength and fracture toughness of the RBBC composites (16 wt% carbon) are 24 GPa, 452 MPa and 4.32 MPa m^1/2, respectively.     

Compressive strength and damage mechanisms of 2D-C/SiC composites at high temperatures

Compressive strength of 2D-C/SiC composite was investigated from room temperature(RT) to 1600?°C at present work. Damage evolution was investigated by conducting loading/unloading tests at RT and the damage mechanisms were elucidated by observing the fracture morphology. It is found that compressive strength of 2D-C/SiC was retained until 1200?°C and then decreased with increasing temperature. The variation of compressive strength is closely related to the degradation in matrix modulus. The compressive damage of 2D-C/SiC starts at the buckling of 0° fiber and is followed by opening and closing of original pores, initiation and growth of longitudinal interbundle cracks, separation of 90° fiber bundles by longitudinal cracks, matrix cracking from intrabundle pores, propagation of matrix cracks into 0° fiber bundles, connection of cracks in 0° fiber bundles and longitudinal cracks in 90° fiber bundles.     

Effect of thermal residual stress on the tensile properties and damage process of C/SiC composites at high temperatures

Due to the mismatch of the thermal expansion coefficients between the matrix and yarns, thermal residual stress will appear in C/SiC composites. In this paper, a progressive damage model was used to predict the thermal-mechanical behavior of C/SiC composites and reveal the failure mechanism. Firstly, the properties of the composites under tensile load were tested at three different temperatures in vacuum. Then, the elastic-plastic progressive damage constitutive laws were used and implemented by a user-defined subroutine UMAT in ABAQUS. The thermal residual stress evolution in the cooling and heating processes was characterized. Finally, the stress-strain curves of the composites under tensile load at different temperatures were studied. The effects of thermal residual stress on the tensile properties and progressive damage process of C/SiC composites were revealed sequentially. This work can give design guidance for strengthening of C/SiC composites.     

A novel approach for developing boron carbide (B4C)/cyanate ester (CE) co-continuous Functionally Graded Materials (FGMs) with eliminated abrupt interfaces

Although traditional functionally graded materials (FGMs) have weakened a certain extent abrupt changes along interfaces between layers, eliminating residual abrupt interfaces which results in great inter laminar stresses remains a major challenge. Herein, ceramic scaffolds with novel continuously graded channels have been firstly prepared through combining layer-by-layer casting with gelation-freeze-dry. Followed by infiltrating soft phase, the co-continuous FGMs without delamination and abrupt changes between layers can be successfully fabricated. The wet layering of suspensions and continuous ice crystals across the interface are the main reasons for the eliminated interfaces. More importantly, the performance of FGMs can be optimized to meet the practical requirement attributed to the varied porosity and pore size distribution of freeze-cast ceramic scaffolds. The novel process for co-continuous ceramics/ FGMs without abrupt interfaces can be extended to other polymers or even metals.     

Fabrication and electromagnetic interference shielding effectiveness of Ti3Si(Al)C2 modified Al2O3/SiC composites

A dense alumina fiber reinforced silicon carbide matrix composites (Al₂O₃/SiC) modified with Ti₃Si(Al)C₂ were prepared by a joint process of chemical vapor infiltration, slurry infiltration and reactive melt infiltration. The conductive Ti₃Si(Al)C₂ phase introduced into the matrix modified the microstructure of Al₂O₃/SiC. The refined microstructure was composed of conductive phase, semiconductive phase and insulating phase, which led to admirable electromagnetic shielding properties. Electromagnetic interference shielding effectiveness (EMI SE) of Al₂O₃/SiC and Ti₃Si(Al)C₂ modified Al₂O₃/SiC were investigated over the frequency range of 8.2–12.4 GHz. The EMI SE of Al₂O₃/SiC-Ti₃Si(Al)C₂ exhibited a significant increase from 27.6 to 42.1 dB compared with that of Al₂O₃/SiC. The reflection and absorption shielding effectiveness increased simultaneously with the increase of the electrical conductivity.     

Compressive strength and wear properties of SiC/Al6061 composites reinforced with high contents of SiC fabricated by pressure-assisted infiltration

Pressure-assisted infiltration was used to synthesize SiC/Al 6061 composites containing high weight percentages of SiC. A combination of PEG and glass water was used to fabricate SiC preforms and the effect of the presence of glass water on the microstructure and mechanical properties of the preforms was evaluated by performing compression tests on the preforms. Also, the compressive strength and the hardness of the SiC/Al composites were investigated. The results revealed that the glass water improved the compressive strength of the preforms by about five times. The microstructural characterization of the composites showed that the penetration of the aluminum melt into the preforms was completed and almost no porosity could be seen in the microstructures of the composites. Moreover, the composite containing 75 wt% SiC exhibited the highest compressive strength as well as the maximum hardness. The results of the wear tests showed that increasing the SiC content reduces the wear rate so that the Al-75 wt% SiC composite has a lower wear rate and a lower coefficient of friction than those of Al-67 wt% SiC composite. This indicated higher wear resistance in these composites than the Al alloy due to the formation of a tribological layer on the surface of the composites.     

Fabrication of gradient C/C-SiC-MoSi2 composites with enhanced ablation performance

C/C-SiC-MoSi₂ composites with gradient composition and microstructure were prepared by a novel vacuum filtration infiltration (VFI) process with a later hydrothermal densification. The composition distribution, microstructure, density, porosity, thermal conductivity and ablation properties of the composites were investigated. Results show that the distributions of SiC and MoSi₂ are homogeneous and gradient along the cross-section of the composites, respectively. From the inner part to the outer part of the composites, the increase in density and thermal conductivity is achieved. The outer part of the composites exhibits enhanced ablation performance. After being exposed to the oxyacetylene flame at 2000 °C for 30 s, the linear and mass rates of the as-prepared composites are only 0.0051 mm/s and 0.76 mg/s.     

A new approach for the net-shape fabrication of porous Si3N4 bonded SiC ceramics with high strength

In this study, Si₃N₄ bonded porous SiC ceramics with high strength had been net-shapely fabricated by a new approach. In this approach, we proposed a two-step processing route composed of freeze casting and carbothermal reduction reactions in which carbon aerogels, derived from sol infiltration and pyrolysis, involved. The phase components, microstructures and properties of the prepared ceramics were investigated. The results showed that carbon aerogels with high apparent surface area had been completely reacted and new SiC and Si₃N₄ grains had been produced. The porous ceramics with flexural strength of 164.3 MPa at 33% porosity and 80.5 MPa at 46% porosity were obtained, whose linear shrinkages were only 1.06% and 1.94% during the whole processing respectively.     

Reaction-bonded B4C/SiC composites synthesized by microwave heating

The reaction-bonding technique was used to synthesize boron carbide (B₄C) - silicon carbide (SiC) composites by microwave heating. Preforms of porous B₄C were obtained by compaction followed or not by partial densification. Then, the material was infiltrated by molten silicon under a microwave heating. The influence of the thermal cycles (T: 1400-1500°C, t: 5-120 minutes) is low. The hardness of boron carbide is comparable to that of alumina (15-19 GPa) for a much lower density (≈2.5 g/cm³ for B₄C-based material instead of 3.95 g/cm³ for alumina). These properties make this composite, obtained by microwave heating, a good candidate for ballistic applications.     

Modeling and experimental study on electrical impedance response to damage accumulation in 2D C/SiC composites

The electrical properties of C/SiC composites could be used for online and in-situ damage monitoring. To investigate alternating current (AC) impedance response to damage in the C/SiC composites, monotonic and incremental cyclic tensile tests were performed. Both AC impedance and acoustic emission (AE) techniques were applied to clarify the damage evolution during the tests. The relationship between damage and electrical impedance response was investigated and validated via macroscopic equivalent circuit models. The effects of longitudinal deformation and damage on AC impedance characteristics, including impedance magnitude and phase angle, were obtained from the models. Results showed that the longitudinal deformation increases the impedance magnitude and the phase angle, and the damage causes the impedance magnitude to increase and the phase angle to decrease. The phase angle is significantly sensitive to fiber breakage, which makes the AC-based method more suitable for online damage monitoring and final failure warning.     

Tensile creep properties and damage mechanisms of 2D-SiCf/SiC composites reinforced with low-oxygen high-carbon type SiC fiber

Tensile creep properties of 2D-SiC_f/SiC composites reinforced with low-oxygen high-carbon type SiC fibers were studied in vacuum at 1300°C∼1430°C. The fracture morphology was observed by scanning electron microscopy and the damage of fiber in 2D-SiC_f/SiC composites was characterized by nanoindentation. Moreover, the microstructure of the composite was investigated by high-resolution transmission electron microscopy. The results show that rupture time is much shortened and steady-state creep rate increase three orders of magnitude when creep temperature is higher than 1400°C. There are two different creep damage mechanisms due to the decrease of interfacial bonding strength at high temperature. The amorphous SiO_xC_y phase in the fibers can crystallize into SiC and C and the SiC grain grows in the fiber. The microstructural changes lead to the decrease of fiber strength and degrade the creep properties of the composite above 1400°C.     

Microstructure and properties of B4C-SiC composites prepared by polycarbosilane-coating/B4C powder route

B₄C-SiC composites with fine grains were fabricated with hot-pressing pyrolyzed mixtures of polycarbosilane-coated B₄C powder without or with the addition of Si at 1950 °C for 1 h under the pressure of 30 MPa. SiC derived from PCS promoted the densification of B₄C effectively and enhanced the fracture toughness of the composites. The sinterability and mechanical properties of the composites could be further improved by the addition of Si due to the formation of liquid Si and the elimination of free carbon during sintering. The relative density, Vickers hardness and fracture toughness of the composites prepared with PCS and 8 wt% Si reached 99.1%, 33.5 GPa, and 5.57 MPa m^1/2, respectively. A number of layered structures and dislocations were observed in the B₄C-SiC composites. The complicated microstructure and crack bridging by homogeneously dispersed SiC grains as well as crack deflection by SiC nanoparticles may be responsible for the improvement in toughness.     

Study on ballistic mechanism of B4C/Al gradient armor

In order to improve the anti-penetration performance of gradient armor, the constitutive models of B₄C/Al composites with different compositions were determined according to the bending curves. The anti-bullet simulation of B₄C/Al gradient armor was carried out by ANSYS-DYNA finite element software, and the stress state of B₄C/Al gradient material under 7.62-mm bullet penetration was analyzed. Meanwhile, the propagation law of stress wave in armor was studied by Hopkinson bar simulation and the improved internal stress wave model, which further revealed the ballistic mechanism of B₄C/Al gradient armor. The simulation results showed that, compared with the traditional laminated armor, the toughness of B₄C/Al gradient armor material increased with the change of layer thickness, resulting in the fact that the whole armor could withstand greater stress without breaking, and the anti-penetration time was prolonged. In addition, the performance difference between the layers of the gradient armor was slight, and the spallation phenomenon of the relative double-layer armor decreases, which enhanced the multiple hit performance of the armor and the absorption capacity of the stress wave. The performance of B₄C/Al gradient armor specimens and double-layer specimens were tested by drop hammer impact test. The test results were consistent with the simulation results.     

Evaluation of elastic constants and high temperature tensile behaviour with damage assessment of the SiC seal-coated 2.5D Cf/SiC composites having multilayered interphase and Si-B-C added matrix

Elastic constants and tensile behaviour of chemical vapour infiltration processed 2.5D C_f/SiC composites possessing multilayered (PyC/SiC)_n=4 interphase, Si-B-C containing matrix and SiC seal-coating have been evaluated with microstructural examination and damage assessment. The strength obtained as ～187 ± 2 MPa in tensile tests at 27 °C is increased by ～18% and ～22% at 1000 °C and 1250 °C, respectively due to reduced thermal stress and increased strength of load-sharing C-fibres, which are protected from oxidation till failure by a self-healing borosilicate layer. The damage evolving during tension tests has been quantified by relating it to decrease of stress-strain slope with strain. Higher (6–8 times) elastic constants measured along fibre-axes than that obtained transversely, indicate significant anisotropy. Owing to matrix cracking with fibre-debonding and pull-out, the fibre-oriented elastic constants of tensile-fractured samples are significantly lower than those of as-received composites, and the difference scales with temperature, whereas negligible change is observed perpendicular to the fibre axes.     

Numerical simulation of chemical vapor infiltration of propylene into C/C composites with reduced multi-step kinetic models

A parallel-consecutive reaction model of chemistry and kinetics is proposed to simulate homogeneous gas-phase reactions of propylene pyrolysis in CVI processes. An improved bipore model is also suggested to describe the changes of the pore topology with densification. The competition between the heterogeneous reactions of pyrolytic carbon deposition and the homogeneous reactions is analyzed by a numerical simulation method. Numerical simulation shows that continuous higher density region occurs early in a certain depth of the substrate, which blocks precursor transport into the deeper region. Changing processing parameters can alter when and where the continuous higher density region takes place. Inside-out densification is an inherent characteristic for CVI processes, while premature surface crusting is an apparent phenomenon. According to the concentration ration between C₂H_x and C₆H_y, the textures of pyrolytic carbon are successfully predicted. The present model is validated by comparing predicted with observed densities.