Enhancing mechanical properties of fused silica composites by introducing well-dispersed boron nitride nanosheets

Well-dispersed boron nitride nanosheets (BNNSs) reinforced fused silica composites were successfully fabricated by surface modification assisted flocculation method. Surface modification can enhance the performance of flocculation process. BNNSs were homogeneously mixed with fused silica through the electrostatic interaction between hydroxylated BNNSs with negative charge and amino-modified fused silica with positive charge. The BNNSs can act as excellent nanofillers for enhancing the mechanical properties of fused silica composites. Approximately 74% and 48% increases in flexure strength and fracture toughness can be achieved for the 1.5 wt% BNNSs/fused silica composite, respectively. The toughening mechanisms were analyzed by microstructural characterization, especially for pull-out mechanism.     

Microstructure and mechanical properties of boron nitride nanosheets-reinforced fused silica composites

In order to overcome intrinsic brittleness and poor mechanical properties of fused silica (FS), boron nitride nanosheets (BNNSs) as a novel reinforcement were employed for fabrication of BNNSs/fused silica composites. BNNSs with micron lateral size were homogeneously dispersed with FS powder using a surfactant-free flocculation method and then consolidated by hot pressing. The flexural strength and fracture toughness of the composite with the addition of only 0.5 wt.% BNNSs increased by 53% and 32%, respectively, compared with those of pure FS. However, for higher BNNSs contents the improvement in mechanical properties was limited. Microstructural analyzes have shown that the toughening mechanisms are combinations of the pull-out, crack bridging, and crack deflection mechanisms.     

The effect of boron nitride nanosheets on the mechanical and thermal properties of aluminum nitride ceramics

The boron nitride nanosheets (BNNSs)/aluminum nitride (AlN) composites were prepared by hot press sintering at 1600°C. The microstructure, mechanical properties, and thermal conductivity of the samples were measured, and the effect of adding BNNSs to AlN ceramics on the properties was studied. It is found that the addition of BNNSs can effectively improve the mechanical properties of AlN. When the additional amount is 1 wt%, the bending strength of the sample reaches the maximum value of 456.6 MPa, which is 23.1% higher than that of the AlN sample without BNNSs. The fracture toughness of the sample is 4.47 MPa m^1/2, a 68.7% improvement over the sample without BNNSs. The composites obtained in the experiment have brilliant mechanical properties.     

Surface-diffusion mechanism for synthesis of substrate-free and catalyst-free boron nitride nanosheets

This study presents an innovative surface-diffusion mechanism for the growth of substrate-free and catalyst-free boron nitride nanosheets (BNNSs) by annealing an ammonium borate hydroxide hydrate precursor in a NH₃ chemical vapor deposition system. At elevated temperatures, part of NH₄B₅O₈ slowly decomposes and forms B₂O₃, and flowing NH₃ gradually diffuses to the B₂O₃ surface to form vertically aligned BNNSs. The lateral dimension and crystallinity of the BNNSs increase, while their thickness decreases with the continuous surface-diffusion reaction. The residual NH₄B₅O₈ and B₂O₃ absorbs moisture in the air to constitute NH₄B₅O₈·4H₂O and H₃BO₃ substrates. With increasing annealing temperature and soaking time (at 1400 °C for 7 h), all NH₄B₅O₈ decomposes and the surface-diffusion reaction between B₂O₃ and NH₃ completely occurs, forming substrate-free BNNSs with a lateral dimension of 1 μm and a thickness of 10 nm. This reliable approach for synthesizing BNNSs paves the way for future applications in advanced ceramic composites.     

Silicon nitride/boron nitride ceramic composites fabricated by reactive pressureless sintering

Using Si and BN powders as raw materials, silicon nitride/hexagonal boron nitride (Si₃N₄/BN) ceramic composites were fabricated at a relatively low temperature of 1450 °C by using the reaction bonding technology. The density and the nitridation rate, as well as the dimensional changes of the specimens before and after nitridation were discussed based on weight and dimension measurements. Phase analysis by X-ray diffraction (XRD) indicated that BN could promote the nitridation process of silicon powder. Morphologies of the fracture surfaces observed by scanning electron microscopy (SEM) revealed the fracture mode for Si₃N₄/BN ceramic composites to be intergranular. The flexural strength and Young's modulus decreased with the increasing BN content. The reaction-bonded Si₃N₄/BN ceramic composites showed better machinability compared with RBSN ceramics without BN addition.     

Effects of amino groups on dispersibility of silicon nitride powder in aqueous media

Silicon nitride (Si₃N₄) powders were subjected to amination modification by grafting γ-aminopropyltriethoxysilane (APTES) via a direct blending method in solution. Fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS) analyses indicated that the hydroxyl groups present on the surface of Si₃N₄ powder particles interacted with the silanols groups of APTES to combine through covalent bonding. Thermogravimetric analysis (TGA) suggested that the grafting of APTES on Si₃N₄ powder surface was successful with grafting content reaching up to 7%. Compared to native Si₃N₄, the surface hydrophilicity of amino Si₃N₄ powder was enhanced and dispersibility was improved. Overall, these findings indicated the promising aspects of amination modification and future potential use in environmental protection by using water instead of organic solvents during Si₃N₄ ceramic formation process.     

Boron nitride nanosheets reinforced glass matrix composites

The effect of reinforcing boron nitride nanosheets (BNNSs) on the mechanical properties of an amorphous borosilicate glass (BS) matrix was studied. The BNNSs were prepared using liquid exfoliation method and characterised by transmission electron microscopy, scanning electron microscopy and X-ray diffraction (XRD) analysis. The average length was ～0.5?μm, and thickness of the nanosheets was between 4 and 30 layers. These BNNSs were used to prepare BS-BNNS composite with different loading concentrations of 1, 2.5 and 5 mass-% (i.e. 1.395, 3.705 and 7.32 vol.-%). Spark plasma sintering (SPS) was used to densify these composites to avoid structural damages to the BNNSs and/or crystallisation within the composite sample during high temperature processing. The BNNSs were found to be evenly distributed in the composites matrix and were found to be aligned in an orientation perpendicular to the direction of the applied force in SPS. The mechanical properties including fracture toughness, flexural strength and elastic modulus were measured. Both fracture toughness and flexural strength increased linearly with increasing concentration of BNNSs in BS glass. There was an enhancement of ～45% in the fracture toughness (1.10?MPa.m^1/2) as well as flexural strength (118.82?MPa) with the addition of only 5 mass-% loading of BNNSs compared to BS glass (0.76?MPa.m^1/2; 82.16?MPa). The toughening mechanisms developed in the composites because of the reinforcement of BNNSs were thoroughly investigated.     

Surface modification of nano‐sized silicon nitride with BA‐MAA‐AN tercopolymer

In this work, a macromolecular coupling agent (BA‐MAA‐AN tercopolymer) was used for surface modification of native nano‐sized silicon nitride (Si₃N₄) powder. This modification strategy was designed for preparing nano‐Si₃N₄/NBR composites. The structure and surface properties of modified nano‐Si₃N₄ were systematically investigated by FTIR, XPS, TGA, TEM, Size Distributions Analyzer, and Contact Angle Measurement. It was found that, the optimum loading of BA‐MAA‐AN tercopolymer coated on the surface of nano‐sized Si₃N₄ is 10% of nano‐Si₃N₄. According to the spectra of FTIR, XPS and TGA, it can be inferred that this macromolecular coupling agent covalently bonds on the surface of nano‐sized Si₃N₄ particles and an organic coating layer is formed. The contact angle experiments show that the hydrophobic property of nano‐sized Si₃N₄ modified with macromolecular coupling agent is improved obviously. TEM reveals that modified nano‐Si₃N₄ possesses good dispersibility and the average diameter in NBR is less than 100 nm. It has also been found that the oil resistance of NBR based nanocomposites is improved greatly due to the modified nano‐Si₃N₄. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Mechanical,dielectric and thermal properties of porous boron nitride/silicon oxynitride ceramic composites prepared by pressureless sintering

Porous boron nitride/silicon oxynitride (BN/Si₂N₂O) composites were fabricated by pressureless sintering at 1650 °C with Li₂O as sintering aid. The influence of Li₂O and hexagonal boron nitride (h-BN) contents on phase, microstructure, mechanical, dielectric and thermal properties of the resulting porous BN/Si₂N₂O composites was investigated. Increasing Li₂O content facilitated densification and decomposition of Si₂N₂O into Si₃N₄. The apparent porosity of the composites increases with the h-BN content increases and Si₂N₂O grain growth was restrained by the dispersed h-BN particles. The dielectric properties and thermal conductivities (TC) were affected mainly by porosity. Porous BN/Si₂N₂O ceramic composites with 4 mol% Li₂O and 25 mol% BN exhibit both low dielectric constant (3.83) and dielectric loss tangent (0.008) with good mechanical and thermal performance, suggesting possible use as high-temperature structural/functional materials.     

Highly thermal conductivity silicon nitride/carbon fibres/bismaleimide composites

Hybrid fillers of silicon nitride/carbon fibres (Si₃N₄/CFs) are performed to improve the thermal conductivities, mechanical and thermal resistance properties of the bismaleimide (BMI) composites. The thermally conductive coefficient of the Si₃N₄/CFs/BMI composites is improved to 1.68 W/mK with 50 wt% modified Si₃N₄ fillers. The flexural strength and interlaminar shear strength of the composites are optimal with 10 wt% modified Si₃N₄ fillers. The thermal resistance properties of the Si₃N₄/CFs/BMI composites are also improved with the addition of Si₃N₄ fillers. Surface modification of Si₃N₄ fillers exhibits positive effects on the thermal conductivities and mechanical properties of the Si₃N₄/CFs/BMI composites. POLYM. COMPOS., 37:468–471, 2016. © 2014 Society of Plastics Engineers     

Effect of boron nitride nanosheets addition on the mechanical and dielectric properties of magnesium oxide ceramics

Boron nitride nanosheets (BNNSs)/magnesium oxide (MgO) composites were prepared via hot pressing. Mechanical properties of MgO ceramics were improved obviously in virtue of adding BNNSs. The bending strength of the 1 wt% BNNSs/MgO composite increased by about 85% than that of the monolithic MgO. The fracture toughness increased by 34% with the addition of 1.5 wt% BNNSs. Microstructural analyzes have shown that the toughening mechanisms are combinations of the pull-out and bridging of BNNSs, crack deflection, and crack bypassing mechanisms. The addition of a small amount of BNNSs don't destroy the excellent dielectric properties of composites. The dielectric constant of the sample doped with 1 wt% BNNSs was about 9.5 in the whole X-band and the vast majority of P-band, and the loss tangent was less than 5 × 10⁻³ in 10–15.8 GHz.     

Electromagnetic wave-transparent porous silicon nitride ceramic prepared by gel-casting combined with in-situ nitridation reaction

To achieve the balance between mechanical properties and electromagnetic wave-transparent properties of porous silicon nitride (Si₃N₄), the key is to form an interlocking microstructure constituted by columnar β-Si₃N₄ crystals. This structure can be realized by liquid-phase sintering. However, grain boundaries which affect high temperature properties and volume shrinkage during sintering are inevitable. We proposed a strategy to realize this structure by gel-casting of β-Si₃N₄ whisker (Si₃N_4w) and Si powder followed by in-situ nitridation of Si. To achieve chemically-stable slurry containing micro-sized Si with low viscosity, a novel formulation was developed. Two key structural parameters of the interlocking Si₃N_4w network, i.e., density of the Si₃N_4w skeleton and inter-whisker bonding mode, were adjusted by composition of raw materials and nitridation temperature. The flexural strength, dielectric constant and loss of the porous ceramics are 44.9 MPa, 2.7 and 2 × 10⁻³, when the volume fraction of Si₃N_4w/Si is 5 and the nitriding temperature is 1400 °C.     

Effects of heat treatment on mechanical properties of 3D Si3N4f/BN/Si3N4 composites by PIP

The fabrication of three-dimensional silicon nitride (Si₃N₄) fiber-reinforced silicon nitride matrix (3D Si₃N_4f/BN/Si₃N₄) composites with a boron nitride (BN) interphase through precursor infiltration and pyrolysis (PIP) process was reported. Heat treatment at 1000–1200 °C was used to analyze the thermal stability of the Si₃N_4f/BN/Si₃N₄ composites. It was found after heat treatment the flexural strength and fracture toughness change with a pattern that decrease first and then increase, which are 191 ± 13 MPa and 5.8 ± 0.5 MPa·m^1/2 respectively for as-fabricated composites, and reach the minimum values of 138 ± 6 MPa and 3.9 ± 0.4 MPa·m^1/2 respectively for composites annealed at 1100 °C. The influence mechanisms of the heat treatment on the Si₃N_4f/BN/Si₃N₄ composites include: (Ⅰ) matrix shrinkage by further ceramization that causes defects such as pores and cracks in composites, and (Ⅱ) prestress relaxation, thermal residual stress (TRS) redistribution and a better wetting at the fiber/matrix (F/M) surface that increase the interfacial bonding strength (IBS). Thus, heat treatment affects the mechanical properties of composites by changing the properties of the matrix and IBS, where the load transfer efficiency onto the fibers is fluctuating by the microstructural evolution of matrix and gradually increasing IBS.     

Fabrication and mechanical properties of boron nitride nanotube reinforced silicon nitride ceramics

In this study, silicon nitride (Si₃N₄) ceramics added with and without boron nitride nanotubes (BNNTs) were fabricated by hot-pressing method. The influence of sintering temperature and BNNTs content on the microstructures and mechanical properties of Si₃N₄ ceramics were investigated. It was found that both flexural strength and fracture toughness of Si₃N₄ were improved when sintering temperature increases. Moreover, α-Si₃N₄ phase could transform into β-Si₃N₄ phase completely when sintering temperature rises to 1800 °C and above. BNNTs can enhance the fracture toughness of Si₃N₄ dramatically, which increases from 7.2 MPa m^1/2 (no BNNTs) to 10.4 MPa m^1/2 (0.8 wt% BNNTs). However, excessive addition of BNNTs would reduce the fracture toughness of Si₃N₄. Meanwhile, the flexural strength and relative density of Si₃N₄ decreased slightly when BNNTs were added. The related toughening mechanism was also discussed.     

Preparation and properties of silicon nitride/glass fiber/epoxy composites

Silicon nitride/glass fiber (Si₃N₄/GF) hybrid fillers are performed to prepare the Si₃N₄/GF/epoxy composites. Results showed the thermal conductivities of the Si₃N₄/GF/epoxy composites that are improved with the addition of Si₃N₄, and the thermal conductive coefficient λ is 1.412 W/mK with 38 vol% modified Si₃N₄/GF hybrid fillers (30 vol% Si₃N₄ + 8 vol% GF), seven times higher than that of pure epoxy resin. The flexural strength and impact strength of the composites are optimal with 13 vol% modified Si₃N₄/GF hybrid fillers (5 vol% Si₃N₄ + 8 vol% GF). The dielectric constant and dielectric loss of the composites are increased with the increasing addition of Si₃N₄. For a given Si₃N₄/GF hybrid fillers loading, the surface modification can further improve the thermal conductivities of the Si₃N₄/GF/epoxy composites. POLYM. COMPOS., 35:1338–1342, 2014. © 2013 Society of Plastics Engineers     

Microstructure control and mechanical properties of porous silicon nitride ceramics

Porous silicon nitride ceramics with a fibrous interlocking microstructure were synthesized by carbothermal nitridation of silicon dioxide. The influences of different starting powders on microstructure and mechanical properties of the samples were studied. The results showed that the microstructure and mechanical properties of porous silicon nitride ceramics depended mostly on the size of starting powders. The formation of single-phase β-Si₃N₄ and the microstructure of the samples were demonstrated by XRD and SEM, respectively. The resultant porous Si₃N₄ ceramics with a porosity of 71% showed a relative higher flexural strength of 24 MPa.     

Self-coiling silicon nitride nanobelts into microrings

In the present work, we reported the growth of silicon nitride (Si₃N₄) microrings formed by self-coiling of nanobelts with a typical saw-like structure on one side, which were synthesized via catalyst-assisted pyrolysis of organic precursors. The as-grown microrings were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The pyrolysis temperature played a crucial role in the self-coiling of Si₃N₄ microrings, enabling the tailored growth of Si₃N₄ microrings. The mechanism for the growth of Si₃N₄ microrings was discussed, which mainly involved the growth of Si₃N₄ nanobelts via a vapor-solid (VS) process, followed by bending into a ring-like shape driven by the surface stress.     

A facile strategy for fabricating self-sealing dense coating grown in-situ on porous silicon nitride ceramics

This present work explores initially the feasibility of producing in-situ surface oxidized coating on porous silicon nitride (Si₃N₄) ceramics. Theoretical prediction identifies the applied conditions of self-sealing strategy and oxidation time required to form dense coating. Experimentally, the porous Si₃N₄ ceramics with different pore structures were selected to fabricate in-situ oxidized coatings. The phase compositions, microstructures and mechanical properties of the porous Si₃N₄ ceramics were investigated before and after oxidation. The results show that flat and dense coatings are prevailed in all samples, which consist of amorphous SiO₂ and its precipitates besides dominant Si₃N₄ phase. The strengthened substrate and strengthening effect of coating are the essential mechanisms associated with the improved mechanical properties. Self-sealing method seems to offer an inexpensive and efficient route to prepare coating on porous Si₃N₄ ceramics.     

Microstructure and mechanical properties of Si3N4f/Si3N4 composites with different coatings

The Si₃N₄ coating and Si₃N₄ coating with Si₃N₄ whiskers as reinforcement (Si₃N_4w-Si₃N₄) were prepared by chemical vapor deposition (CVD) on two-dimensional silicon nitride fiber reinforced silicon nitride ceramic matrix composites (2D Si₃N_4f/Si₃N₄ composites). The effects of process parameters of as-prepared coating including the preparation temperature and volume fraction of Si₃N_4w on the microstructure and mechanical properties of the composites were investigated. Compared with Si₃N₄ coating, Si₃N_4w-Si₃N₄ coating shows more significant effect on the strength and toughness of the composites, and both strengthening and toughening mechanism were analyzed.     

Effects of heat treatment on mechanical and dielectric properties of 3D Si3N4f/BN/Si3N4 composites by CVI

In this study, three-dimensional silicon nitride fiber-reinforced silicon nitride matrix (3D Si₃N_4f/BN/Si₃N₄) composites with a boron nitride (BN) interphase were fabricated through chemical vapor infiltration. Through comparing the changes of microstructure, thermal residual stress, interface bonding state, and interface microstructure evolution of composites before and after heat treatment, the evolution of mechanical and dielectric properties of Si₃N_4f/BN/Si₃N₄ composites was analyzed. Flexural strength and fracture toughness of composites acquired the maximum values of 96 ± 5 MPa and 3.8 ± 0.1 MPa·m^1/2, respectively, after heat treatment at 800 °C; however, these values were maintained at 83 ± 6 MPa and 3.1 ± 0.2 MPa·m^1/2 after heat treatment at 1200 °C, respectively. The relatively low mechanical properties are mainly attributed to the strong interface bonding caused by interfacial diffusion of oxygen and subsequent interfacial reaction and generation of turbostratic BN interphase with relatively high fracture energy. Moreover, the Si₃N_4f/BN/Si₃N₄ composites also displayed moderate dielectric constant and dielectric loss fluctuating irregularly around 5.0 and 0.04 before and after heat treatment, respectively. They were mainly determined based on the intrinsic properties of materials system and complex microstructure of composites.