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.     

Comparison of interfaces in Ti composites reinforced with uncoated and TiB2/C-coated SiC fibres

Interfaces play an important role in determining the mechanical properties of composite materials. The interfaces established between a titanium-alloy matrix (Ti-6Al-4V) and uncoated and TiB₂/C-coated SiC fibres are analysed by scanning electron microscopy, transmission electron microscopy and X-ray techniques. Emphasis is placed upon the interfacial morphology and microstructure, identification of reaction products, and the stability of the coating layer. Complex multi-reaction layers are observed frequently in the interfacial zones. Previous, often contradictory, reports about the interlayers are reviewed. Experimental observation demonstrates that the type and distribution of interlayers vary in a given system, due to prolonged treatment of the samples at temperature. The formation and distribution of the interlayers are discussed further, with respect to these and previous findings. Methods of reducing interfacial reactivity are discussed.     

High-resolution electron microscope observation of interface microstructure of a cast Al-Mg-Si-Bi-Pb(6262)/Al2O3p composite

High-resolution electron microscopy was employed to characterize the interface structure of a cast Al-Mg-Si-Bi-Pb aluminium(6262)-based composite reinforced by alpha alumina particles with a trace of beta alumina in order to investigate the behaviour of alloying elements in cast composites. Except for a few primary Mg2Si particles, few reaction products were detected at the interface of Al/alpha-Al2O3 due to the unfavourable reaction kinetics during the squeeze-casting process. The Mg2Si particle has an orientation relationship with alpha-Al2O3 of [011]Mg2Si//[1210]alpha-Al2O3 (111)Mg2Si//(0006)alpha-Al2O3. A significant amount of MgAl2O4 was found on the surface of the beta-Al2O3 particles, which is in contrast to the small degree of reaction found on alpha-Al2O3 particles. MgAl2O4 and beta-Al2O3 particles have the following orientation relationship: [011]MgAl2O4//[1210]beta-Al2O3 (111) MgAl2O4//(0006)beta-Al2O3. The similar crystal structure of beta-Al2O3 to MgAl2O4 favours MgAl2O4 nucleation and growth on the surface of beta-Al2O3. Interfacial energy minimization dominates the atomic structure of the interface with the result that close packed planes and directions in the Al2O3 reinforcement and reaction products are parallel to the interfaces. Bi and Pb were found in the form of metallic nanometre particles between Al2O3 particles, or between the MgAl2O4 and Al2O3 particles, or in the open channels of beta-Al2O3 filled by the Al matrix.     

The microstructure of spray-formed Ti-6Al-4V/SiCf metal-matrix composites

Spray-forming is a possible manufacturing route for the fabrication of Ti alloy fibre-reinforced metal-matrix composites (MMCs) because high rates of alloy-droplet cooling on impact with the fibres prevent excessive fibre-matrix reaction. Ti–6Al–4V matrix MMC monotapes containing TiB₂-coated SiC fibres have been manufactured by electric-arc spray-forming, and the key MMC microstructural characteristics in the as-sprayed monotapes have been investigated by optical and scanning electron microscopy. Fibre infiltration increases with decreasing spraying distance, decreasing atomizing gas pressure and increasing arc current, because of higher temperatures in the Ti alloy spray droplets on impact with the fibres. Too much binder in the fibre preform leads to poor fibre–matrix contact, while removing the binder leads to the fibres becoming misaligned during spraying.     

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.     

Microstructure and creep characteristics of experimental SiCf–YMAS composites

A unidirectional SiC_f –YMAS glass–ceramic composite has been developed by Céramiques-Composites (Bazet) and ONERA (Establishment of Palaiseau) in France. The matrix is totally crystalline and consists essentially of two main phases, cordierite and yttrium disilicate, with some minor phases, mullite, spinel, zirconium and titanium oxides. Image analysis methods have been used to characterize the homogeneity of the composite plates and to obtain granulometric information on the different matrix phases. Different interphase layers formed during the process by reaction between the matrix and the Nicalon NLM 202 fibres have been studied by using HREM and EDX. Their chemical composition has been determined by stepping the probe (8 nm) across the fibre–matrix interface. Two distinct nanoscale sublayers have been imaged. The sublayer on the matrix side has a light contrast in the TEM. The microstructure of this layer (≈ 80 nm) is typical of a turbostratic carbon. The carbon layer also contains Al, O, Mg and Si. The silicon content is low in the carbon layer. The sublayer on the fibre side (≈ 100 nm thick) has a dark contrast in the TEM. Profiles have been taken across this sublayer also. Tensile creep tests in air have been performed to investigate the tensile creep behaviour at 1223 K. They have been conducted in the 50–200 MPa stress range. Tensile creep results indicate that creep rates are of the same order of magnitude as for other glass–ceramic composites. Optical micrographs and SEM observations have revealed the damage in the composite. Changes occurring in the interface region have been studied at a finer scale by TEM and HREM at the surface of the sample and in the core. These observations enable us to explain the mechanical behaviour of the composite observed on a macroscopic scale.     

The microstructure of silicon carbide (Nicalon) fibre reinforced silicon carbide ceramic-matrix composites heat treated in vacuo and in pure oxygen

Silicon carbide (Nicalon) fibre reinforced SiC composites have been heat treated in vacuo and in pure oxygen environments at 1400°C for 100 h. The response of the microstructure and, in particular, of the interface between fibre, carbon interlayer and SiC matrix components has been studied. Microstructural modifications were observed by transmission electron microscopy, using imaging, electron energy-loss spectroscopy and electron diffraction techniques, and fibre stoichiometries were determined using a scanning Auger microprobe. Recrystallization of Nicalon fibres within composites heat treated in vacuo was found to result from decomposition of the metastable silicon oxy-carbide phase found in the fibres. No significant changes to the pyrolytic carbon interlayer were observed. Fibre recrystallization was considered to embrittle the composite. Samples heat treated in oxygen showed no appreciable fibre recrystallization. Study of interlayers in such aged samples often revealed decohesions, holes and narrow silica layers. In the most extreme cases, complete displacement of carbon by SiO₂ was found and such interfaces were identified as silica and α-cristobalite. Interfacial modifications were considered to be responsible for the retention of the small β-SiC grain size in Nicalon fibres and were also considered to be deleterious to the mechanical properties.