Characterization of the fibre–matrix interfacial structure in carbon fibre-reinforced polycarbosilane-derived SiC matrix composites using STEM/EELS

This paper presents a characterization study of the microstructural evolution of various carbon fibre-reinforced polycarbosilane (PCS)-derived SiC matrix composites during high temperature heat treatment. Both surface-treated and untreated carbon fibre reinforcements were investigated. The STEM/EELS technique was found to be a particularly useful characterization tool. The results of quantitative EELS linescans have been interpreted in terms of the migration of gaseous SiO and CO, produced by the reaction between the small amount of SiO₂ and excess carbon within the PCS-derived SiC matrix, from the central matrix region towards the fibre–matrix interfaces. Generally, the migration of gaseous SiO and CO results in an enrichment of SiO₂ at the region adjacent to the fibre–matrix interface. However, differing final composite microstructures are formed depending on the strength of the fibre–matrix bonding. In the case of strong fibre-matrix interfacial bonding where few escape channels are present, a distinct Si–C–O layer was identified within the matrix adjacent to the fibre–matrix interface; both crystalline β-SiC and the segregated Si–O–C phase coexist in this microstructure up to at least 1450 °C. In the case of weak fibre–matrix bonding this oxygen segregated interfacial layer is eventually removed at high enough temperatures. The final interfacial microstructure has important consequences for the mechanical properties of the composite material.     

The compatibility of TiB2 protective coatings with SiC fibre and Ti-6Al-4V

TiB₂ coatings have been studied as prospective protective layers to inhibit the interfacial reaction between SiC fibres and Ti-alloy matrices. This protective coating has been deposited onto SiC monofilament fibres using a chemical vapour deposition (CVD) technique. The fibre-matrix compatibility of these TiB₂-coated SiC fibres in Ti-6Al-4V composites was evaluated by incorporating the coated fibres into Ti-6Al-4V using a diffusion bonding technique. The interfaces of this composite were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron probe microanalysis, to evaluate the interfacial microstructures, chemical stability and the efficiency of TiB₂ as a protective coating for SiC fibres in Ti-alloy matrices, and to study the effects of deposition temperature on the interface of the coated fibre. Results show that stoichiometric TiB₂ coatings are stable chemically to both SiC fibres and Ti-6Al-4V and hinder the deleterious fibre-matrix reactions effectively. Boron-rich TiB₂ coatings should be avoided, as they lead to the formation of a needle-like TiB phase at the fibre–matrix interface. These findings provide promising evidence for the value of further exploration of the use of stoichiometric TiB₂ as a protective coating for SiC fibre in Ti-based composites.     

The response of SiC fibres to vacuum plasma spraying and vacuum hot pressing during the fabrication of titanium matrix composites

Vacuum plasma spraying (VPS) and vacuum hot pressing (VHP) have been used to fabricate Ti-6Al-4V matrix composite material reinforced longitudinally with DERA Sigma C coated SiC 1140+ fibres. VPS of Ti-6Al-4V onto Sigma 1140+ SiC fibres caused no fibre/matrix interfacial reaction. During VHP a fibre/matrix reaction occurred, producing a mixture of fine (< 50 nm) TiC_x (x ≤ 1) adjacent to the fibre coating and coarse-grained (0.3–0.5 μm) equiaxed TiC_x adjacent to the Ti matrix. A decrease in C concentration with increasing distance from the C coating is proposed, and is consistent with the evidence presented. A similar thickness and morphology of reaction product arose from conventional foil–fibre foil processing, but the matrix coated fibre/hot isostatic pressing process led to a slightly thicker reaction layer. The TiC_x reaction product acted as a diffusion barrier, inhibiting further reaction more effectively than in experiments on earlier SiC fibres having a C coating. Surface damage was shown to be a factor in lowering 1140+ SiC fibre failure stress. Surface damage to 1140+ fibres resulted from both VPS and VHP, the former causing a slight reduction in mean ultimate tensile strength (UTS), and a large reduction in the bend strain to failure Weibull modulus. This damage was caused by both fibre winding and by deposition of metal during VPS, giving rise to coating flaws, and is not in itself considered to be a major problem. Surface damage increased after VHP, reducing the mean UTS and tensile Weibull modulus, and the mean bend strain to failure. This damage arose from bending and flattening of the rough monotapes, and from the fibre/matrix reaction caused by thermal exposure. The level of damage to 1140+ SiC fibre from VHP was reduced by modification of the process path. Increasing the VHP temperature and lowering the pressure ramp rate reduced fibre damage sufficiently to enable a macroscopic composite UTS of 95% of the theoretical maximum to be achieved.     

Environmental ageing effects in a silicon carbide fibre-reinforced glass-ceramic matrix composite

A silicon carbide fibre-reinforced glass-ceramic composite, based upon a BaO–MgO–Al₂O₃–SiO₂ (BMAS) matrix, has been used for a study of microstructural stability (specifically interface stability) after environmental exposure at elevated temperature. Characterization of the as-received material demonstrated the presence of a thin ‘carbon-rich’ interfacial layer between fibre and matrix, as typically observed in glass-ceramic/silicon carbide fibre composite systems. Samples have been subjected to heat-treatments in an oxidizing atmosphere at temperatures between 723 and 1473 K, for up to 500 h. Intermediate-temperature ageing, between 873 and 1073 K, results in strong fibre/matrix bonding, with consequent degradation of strength and composite ‘ductility’. This is due to oxidative removal of the carbon interfacial layer and subsequent oxidation of the fibre surface, forming a silica bridge. Carbon is retained at higher ageing temperatures due to the formation of a protective surface oxide scale at exposed fibre ends. Attempts to pretreat the BMAS composite at high temperature (1273–1473 K), designed to inhibit intermediate-temperature degradation via the formation of silica plugs at exposed fibre ends, has given mixed results due to the high residual porosity content in these materials, allowing paths of ‘easy’ oxygen ingress to be retained.     

Interface compatibility in Nicalon-fibre reinforced metal and ceramic composites

Microstructural characteristics of the fibre–matrix interface of two composite systems which utilize Nicalon fibre reinforcement are analysed and discussed. An Al-based composite produced by liquid-metal infiltration was found to contain crystals of aluminium carbide and alumina at the fibre–matrix interface, which produced a strong interfacial bond, restricted fibre pullout, and resulted in an essentially brittle composite. A ceramic-matrix composite based upon calcium aluminosilicate and produced by hot pressing exhibited substantial fibre pullout during testing; microstructural analysis of the interface showed the presence of a C-rich layer. Treatment of the composite in air over a range of temperatures (600–1200°C) progressively oxidized the carbon and formed silica ‘bridges' between fibre and matrix, which resulted in increased brittleness. Electron-probe microanalysis combined with electron microscopy of the Nicalon fibre showed that approximately half the material consisted of microcrystalline β-SiC and the remainder was free carbon and silicon oxycarbide. Thus the carbon constituent was largely responsible for carbide formation in the Al-based material, which restricted fibre pullout, whilst free carbon, plus the additional free carbon formed by chemical reaction between silicon carbide in the fibre and the calcium aluminosilicate matrix, provided the interfacial carbon layer which gave enhanced fibre pullout in the ceramic-based composite; the decreased fibre pullout and increased brittleness of the latter after heat treatment in air could thus be explained by the removal of the carbon layer and the development of silica bridges between fibre and matrix.     

Evaluation of interface bonding strength of aluminum/silicon carbide

The quality of interface bonding between matrix and reinforcement is important in composite strengthening. Interface bonding strength of particulate reinforced metal matrix composites were investigated by joining process. The aluminum/silicon carbide specimens were prepared by different processing temperature with constant holding time. The structural morphologies have been evaluated by using scanning electron microscope and interfacial products were identified by using energy dispersive spectroscopy. The interface strength has been evaluated by tensile test and microhardness test.     

Effect of reinforcement coatings on the dry sliding wear behaviour of aluminium/SiC particles/carbon fibres hybrid composites

Dry sliding wear of an AA 6061 alloy reinforced with both modified SiC particles and metal coated carbon fibres has been studied. SiC particles were used to increase the hardness of the composite while short carbon fibres are supposed to act as a solid lubricant. SiC particles were coated with a silica layer deposited through a sol–gel procedure to increase the processability of the composite and to enhance the particle–matrix interfacial resistance. The metallic coatings on carbon fibres were made of copper or nickel phosphorus which was deposited through an electroless process. The metallic coatings favoured the wetting of the fibres during processing and then dissolved in the aluminium matrix forming intermetallic compounds that increased its hardness. Wear behaviour of AA 6061–20%SiC and AA 6061–20%SiC–2%C was compared with that of the composites with the same reinforcement content but using coated particles and fibres. The influence that the modification of the matrix because of the incorporation of coatings on the reinforcements had on the mild wear behaviour was investigated. The wear resistance of the composites increased when carbon fibres were added as secondary reinforcement and when coated reinforcements were used.     

SOLIDIFICATION PROCESSING AND FRACTURE MORPHOLOGY OF SiCp/ZL108 COMPOSITE

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Heterogeneous fibre microstructures and their influence on failure

A detailed microscopic, experimental and micromechanical evaluation of fibre damage initiation in a unidirectional aluminium matrix-silicon carbide fibre (SCS-8^TM) composite has been performed for a monotonic load sequence. The salient fibre features include a 33-μm-diameter monofilament turbostratic carbon (C) core, a ∼ 1·5-μm pyrolytic C layer, an interior sheath of β-phase silicon carbide (SiC) crystallites imbedded in an amorphous C matrix, and an exterior sheath of radially orientated β-SiC. Quantitative microscopy shows that the interior sheath's surplus C varies smoothly from ∼ 35% by volume near the core to zero at the mid-radius. The multi-phase structure of the fibre produces an internal mechanical stiffness that increases with distance from the core, and thus peak stresses result in the exterior sheath. X-ray tomographic microscopy (XTM) reveals that cores fracture randomly, without failure of the surrounding SiC, at stress levels above half the ultimate strength of the composite. Three-dimensional XTM reconstructions show planar, non-planar and spiral cracks in the failed fibre, suggesting multiple and competing initiation mechanisms. Qualitative fracture assessments suggest that flaws near the C core grow outward in a curved manner through the SiC–C and planar beyond the mid-radius, whereas cracks originating near the fibre–matrix interface favour planar trajectories inward across the whole fibre.     

喷射沉积SiC_p/Al-20Si复合材料高周疲劳行为研究

采用喷射沉积法制备15%(体积分数)4.5 m SiCp/Al-20Si复合材料及其基体合金,研究该组材料的微观组织、力学性能、高周疲劳性能以及疲劳断口形貌。结果表明:SiC颗粒的加入有利于提高材料的力学性能;复合材料及其基体的高调疲劳寿命随应力幅值的减小而增加,在相同应力幅值下,复合材料的疲劳寿命远远高于基体合金。疲劳裂纹从大颗粒的初晶Si的断裂以及Si相脱离处形核,并开始扩展。对于复合材料而言,SiC颗粒尺寸较小,不容易发生断裂,在形核过程中,当裂纹遇到SiC颗粒时,裂纹或者避开增强体,或者受阻于SiC颗粒,只能在基体合金中扩展,从而扩大了疲劳形核区的面积,提高了材料的疲劳寿命。Si颗粒的脱离、Si相的断裂以及SiC颗粒与基体界面的脱粘是复合材料疲劳断裂失效的主要机制。     

Moisture and gamma‐ray irradiation effects on the mechanical properties of carbon fibre–reinforced plastics

The effects of γ‐irradiation and moisture absorption on the mechanical properties of carbon fibres–epoxy resin composites were studied. The properties dominated by the matrix and fibre–matrix interface (interlaminar and in‐plane shear strength) were measured at room temperature using standard tests. These tests were carried out before and after exposures to gamma irradiation and before and after immersion in water at 80°C during 21 days. The dosage of gamma irradiation was up to 11.7 MGy. The micrographs of surfaces fractured in performed tests were observed on a scanning electron microscope. They were analyzed with consulting the stated effects on mechanical properties and the measured values of the glass transition temperature of tested coupons before and after irradiation and immersion in water. The obtained results show that moisture and irradiation, if they act one after the other, have a significant influence on the degradation of matrix‐dominated mechanical properties of the tested carbon–epoxy composite.     

Scanning ion microprobe analysis of composite materials

Applications of scanning ion imaging with high lateral resolution in the microchemical investigation of metal – and ceramic-matrix composites are described. The technique, which combines a scanning ion microprobe with secondary ion mass spectrometry (SIMS), is ideally suited to the study of complex, multicomponent composite structures. Most elements can be detected with good sensitivity, enabling the determination of spatial distributions for major and minor elements. Analytical images obtained with this technique reveal unprecedented chemical information about interfacial segregation and interdiffusion phenomena. As examples, the characterization of both ceramic–matrix (Al borate–SiC) and metal–matrix (Ni alloy–Al₂O₃) composite materials is described.     

Producing of AZ91/SiC composite by friction stir processing (FSP)

Friction stir processing (FSP) was used to fabricate SiC/AZ91 composite layer. Effect of process parameters such as rotational and traverse speeds, tool penetration depth and tilt angle on the formation of defects such as cracks, tunnelling cavity and also on sticking of matrix material to the tool was investigated. Also, effect of these parameters was studied on the mechanical properties and microstructures of specimens. Microstructure studies were carried out by optical and SEM. Results showed that FSP is an effective process to fabricate SiC/AZ91 composite layer with uniform distribution of SiC particles, good interfacial integrity and significant grain refinement. Increasing the rotational speed leads to a decrease in the grain size and an increase in the traverse speed leads to a decrease in the grain size. There are upper and lower limitations for these speeds which were determined. PD is a more effective parameter to produce sound surface layer. PD value was affected by traverse and rotational speeds and the tilt angle values. This study shows that by using 5 μm SiC particles, the stir zone grain size reduces from 150 to 7.17 μm and stir zone hardness increases from 63 to 96 Hv.     

Study of carbon fibres and carbon–carbon composites by scanning thermal microscopy

Scanning thermal microscopy (SThM) is a relatively new technique based on atomic force microscopy in which the tip is replaced by an ultra‐miniature temperature probe. This paper reports on a preliminary investigation of the application of SThM in the characterization of the thermal properties of carbon fibres and carbon–carbon (CC) composites. The technique enabled a comparative study to be made of discrete fibre and matrix thermal properties in a series of model unidirectional composites. The thermal images revealed a marked increase in thermal conductivity of the matrix with increasing temperature of treatment and hence confirmed the development of a highly ordered carbon matrix. The results were in qualitative agreement with previously determined values of thermal conductivity from which the separate values of fibre and matrix thermal conductivity had been derived. The technique was also applied to the characterization of samples of unknown processing history, enabling an estimation to be made of the heat treatment and type of the fibres and matrix present in the composite. It was concluded that SThM promises to be a powerful technique for the study of the thermal properties of CC composites and carbon fibres, as it uniquely enables variations in local thermal conductivity to be detected and resolved. Absolute quantification of the technique remains the key to its future widespread acceptance in materials characterization.     

Transmission electron microscopy of interfaces in structural ceramic composites

Ceramic composites based either on a particulate, fibre or a lamellar architecture are potentially useful as damage-tolerant high-temperature engineering materials. The ability of the interfaces in such systems to deflect cracks is vital to the damage tolerance of these materials. Transmission electron microscopy techniques enable the chemical and physical characterization of these interfaces, providing information on interlayer thicknesses, chemical species, local bonding and the microstructural features which give rise to the interfacial properties, thereby enabling a full understanding not only of composites after processing, but also after exposure to aggressive environments such as air at high temperature. Examples of the application of transmission electron microscopy to all three composite architectures are described.     

Friction and Wear of Epoxy Composites Containing Surface Modified SiC Nanoparticles

The authors of the present paper evaluated the sliding wear behaviors of epoxy and its composites filled with untreated and treated SiC nanoparticles. The experimental results indicate that the nanoparticles pretreated by graft polymerization of polyacrylamide effectively improved the overall performance of the matrix epoxy. In comparison with the untreated SiC nanoparticles, the grafted SiC nanoparticles led to more significant reduction in frictional coefficient and wear rate of epoxy. Even under high contact pressure, the composites with grafted SiC nanoparticles possessed the highest wear resistance. The strong interfacial bonding between the grafted SiC nanoparticles and the matrix should account for the properties enhancement. Accordingly, a feasible way of efficiently applying SiC nanoparticles to the preparation of wear resisting nanocomposites has been developed.     

Fabrication and AE characteristics of TINI/A16061 shape memory alloy composite

TiNi/A16061 shape memory alloy (SMA) composite was fabricated by hot press method to investigate the microstructure and mechanical properties. Interface bonding between TiNi reinforcement and A1 matrix was observed by using SEM and EDS. Pre-strain was imposed to generate compressive residual stress inside composite. A tensile test for specimen, which underwent pre-strain, was performed at high temperature to evaluate the variation of strength and the effect of pre-strain. It was shown that interfacial reactions occurred at the bonding between matrix and fiber, creating two inter-metallic layers. And yield stress increased with the amount of pre-strain. Acoustic Emission technique was also used to nondestructively clarify the microscopic damage behavior at high temperature and the effect of pre-strain of TiNi/A16061 SMA composite.     

真空热压烧结SiC_p/Al复合材料的界面元素扩散及增强断裂机理

采用真空热压粉末冶金烧结工艺制备了含SiC颗粒体积分数分别为 5 %、15 %和 2 5 %的SiC颗粒增强铝基复合材料 ,结合其力学性能、扫描电镜和界面微区能谱分析结果 ,分析了SiC/Al复合材料的真空烧结过程中的界面现象 ,以及材料增强和断裂机理。结果表明 ,真空烧结过程中出现了界面反应 ,改善了界面结合强度 ,断裂破坏主要在基体上进行。随着SiC粒子体积分数的增加 ,SiCp/Al复合材料的抗拉强度增加 ,弹性模量显著增加 ,延伸率降低 ,材料脆性增加。     

Tribological Behavior of Cu Matrix Composites Containing Graphite and Tungsten Disulfide

Copper matrix composites containing graphite and tungsten disulfide were prepared and tested under the loads of 1–5 N to investigate their friction and wear behaviors. The microstructure, worn surfaces, and cross section of worn subsurfaces were observed, and the lubricating films formed on the worn surfaces were analyzed. It is found that the Cu–24 vol% WS₂ composite presents a higher mechanical performance and lower wear rate compared to the Cu–24 vol% graphite composite with same volume fraction of solid lubricant. This could be attributed to the high-strength chemical bonding of the interface between WS₂ and the copper matrix. The high-strength interfacial bonding also helps prevent plastic deformation and the formation of cracks at the worn subsurfaces of the composites. The amount of lubricant on the outmost worn surfaces is significantly higher than that in the composite. The lubricating film of WS₂ with relatively high thickness provides a low friction coefficient to the composites.     

A method for estimating the fibre length in fibre‐PLA composites

Wood pulp fibres are an important component of environmentally sound and renewable fibre‐reinforced composite materials. The high aspect ratio of pulp fibres is an essential property with respect to the mechanical properties a given composite material can achieve. The length of pulp fibres is affected by composite processing operations. This thus emphasizes the importance of assessing the pulp fibre length and how this may be affected by a given process for manufacturing composites. In this work a new method for measuring the length distribution of fibres and fibre fragments has been developed. The method is based on; (i) dissolving the composites, (ii) preparing the fibres for image acquisition and (iii) image analysis of the resulting fibre structures. The image analysis part is relatively simple to implement and is based on images acquired with a desktop scanner and a new ImageJ plugin. The quantification of fibre length has demonstrated the fibre shortening effect because of an extrusion process and subsequent injection moulding. Fibres with original lengths of >1 mm where shortened to fibre fragments with length of <200 μm. The shortening seems to be affected by the number of times the fibres have passed through the extruder, the amount of chain extender and the fraction of fibres in the polymer matrix.