TEM characterization of some crude or air heat-treated SiC Nicalon fibres

Commercial Nicalon fibres were prepared by thin transverse sectioning and studied by transmission electron microscopy. A progressive tilting of the incident beam allows us to explore the selected-area diffraction (SAD) pattern along two orthogonal directions, increasing the tilting angle (dark-field (DF) imaging). The lattice fringes technique was also used. The samples were Nicalon 001, 101 and 201 fibres, the latter also being studied after heat treatment in air at 1300° C for 48 h. The SAD pattern of the 001 fibre only shows the SiC, 1 1 intense halo whereas the other samples show all the SiC (1 1 1, 2 2 0 and 31 1) strongly scattered beams, indicating a microcrystalline state. Correspondingly, DF imaging does not indicate any localized measurable scattering domain for 001. Only bright dots can be seen, less than 1 nm in size. The other fibres show SiC microcrystals respectively 2 nm (1 01 ), 3 nm (201 ) and up to 7 nm (heat-treated 201) in extent. Free aromatic carbon, shaped in small units less than 1 nm in size fills up the interstices between SiC. These units tend to lie flat on SiC. In heat-treated fibres, they form incomplete layers around the edges. In addition, the heat-treated 2 01 fibre show a 1m thick layer of cristobalite at the fibre surface. These crystals are polytypes.     

Tensile properties of jute fibres

Abstract

One hundred tensile tests were undertaken at each of five distinct fibre lengths (6, 10, 20, 30 and 50 mm) on a single batch of jute fibres from South Asia. The Young's moduli were found to be independent of length. The ultimate stress (fracture strength) and fracture strains were found to decrease with increasing fibre length. The variation in mechanical properties at each fibre length was characterised using Weibull statistics based on a maximum likelihood estimate; referred to as point estimates. Two empirical based models (a linear and a natural logarithmic interpolation model) have been developed to estimate the fracture properties at any length between 6 and 50 mm. These two interpolation models were also developed based on maximum likelihood estimates. The point estimates were used to benchmark the performance of the two models. The natural logarithmic model was found to be superior to the linear model.     

Improvements in refractoriness and properties of Nicalon fibres by high-temperature heat-treatment

Nicalon SiC fibres were heat-treated in various atmospheres and at various pressures. Initially CO, nitrogen and air were used as the heat-treatment environment at one atmosphere pressure. Microstructural changes and any related strength degradation or improvement were measured for the heat-treated fibres. After heat-treatment in the temperature range 1000°C–1600°C, each sample showed different weight changes. Thus, in air, a weight gain was observed with increasing temperature, whereas in CO and N₂, weight losses were observed but with a smaller weight loss observed for CO. Moreover, carbon monoxide had a significant effect on the strength retention of the fibres. Since the lowest weight loss was observed after heat-treatment in CO at one atmosphere, high pressure CO gas was used to heat-treat Nicalon fibres between 1000°C and 1700°C and the resulting fibres were analysed by single-filament strength testing, scanning electron microscopy, and X-ray diffraction. The results were completely different compared with those in one atmosphere of CO. As the temperature increased, weight and strength increased whereas at one atmosphere pressure, both weight and strength had decreased. The weight increase was because of surface reaction between the CO atmosphere and the SiC fibre and/or because of deposition of carbon from the pressurised CO gas, giving the fibre a surface carbon coating. Carbon coating of a fibre is a beneficial property for CMCs since it provides a weak interface which facilitates pull-out during fracture.     

Electron probe microanalysis of Nicalon fibres

Electron probe microanalysis of a sample of Nicalon fibre showed it to consist of 54.9 wt% Si, 32.1 wt% C and 11.6 wt% O. Studies of the fine structure of the X-ray emission bands suggested these elements were combined as 46 vol% silicon carbide, 34 vol% silicon oxycarbide and 20 vol% free carbon, with the oxycarbide in the outermost regions of the fibre being significantly richer in oxygen. The silicon carbide was composed of microcrystallites several micrometres in diameter and the remaining material formed an amorphous network of material surrounding the microcrystallites.     

Effects of HF treatments on tensile strength of Hi-Nicalon fibres

Tensile strengths of as-received Hi-Nicalon fibres and those having a dual BN–SiC surface coating, deposited by chemical vapour deposition, have been measured at room temperature. These fibres were also treated with HF for 24 h followed by tensile strength measurements. Strengths of uncoated and BN–SiC coated Hi-Nicalon fibres extracted from celsian matrix composites, by dissolving away the matrix in HF for 24 h, were also determined. The average tensile strength of uncoated Hi-Nicalon was 3.19±0.73 GPa with a Weibull modulus of 5.41. The Hi-Nicalon–BN–SiC fibres showed an average strength of 3.04±0.53 GPa and Weibull modulus of 6.66. After HF treatment, the average strengths of the uncoated and BN–SiC coated Hi-Nicalon fibres were 2.69±0.67 and 2.80±0.53 GPa and the Weibull moduli were 4.93 and 5.96, respectively. The BN–SiC coated fibres extracted from the celsian matrix composite exhibited a strength of 2.38±0.40 GPa and a Weibull modulus of 7.15. The strength of the uncoated Hi-Nicalon fibres in the composite was so severely degraded that they disintegrated into small fragments during extraction with HF. The uncoated fibres probably undergo mechanical surface damage during hot pressing of the composites. Also, the BN layer on the coated fibres acts as a compliant layer, which protects the fibres from mechanical damage during composite processing. The elemental composition and thickness of the fibre coatings were determined using scanning Auger analysis. Microstructural analyses of the fibres and the coatings were done by scanning electron microscopy and transmission electron microscopy. Stengths of fibres calculated using average and measured fibre diameters were in good agreement. Thus, the strengths of fibres can be evaluated using an average fibre diameter instead of the measured diameter of each filament. © 1998 Kluwer Academic Publishers     

Weibull analysis of strength-length relationships in single Nicalon SiC fibres

Nicalon SiC fibre is naturally brittle and offers high-temperature application in fibrous composites. Due to the randomly distributed flaws along the fibre, the statistical variability in single-fibre strength is obvious. In this paper, the effect of heat-cleaning procedures on Nicalon fibres has been investigated, and the statistical strength and variability of single Nicalon fibres have been characterized in tension and compared. Experimental results show that the strengths of single Nicalon fibres among the three types of heat-cleaning procedures are less than that of as-received unsized fibres by 22–30%. In addition, both the failure load and the failure stress of the fibres, for a given gauge length (50 mm) and yarn cross-section, can be well fitted to a two-parameter Weibull distribution. The effect of gauge length over the range from 10–175 mm, holding the strain rate constant, was also studied. The logarithmic strength-length plots show that the strength of single Nicalon fibres follows the weakest-link rule.     

Tensile and compressive properties of flax fibres for natural fibre reinforced composites

Mechanical properties of standard decorticated and hand isolated flax bast fibres were determined in tension as well as in compression. The tensile strength of technical fibre bundles was found to depend strongly on the clamping length. The tensile strength of elementary flax fibres was found to range between 1500 MPa and 1800 MPa, depending on the isolation procedure. The compressive strength of elementary flax fibres as measured with a loop test lies around 1200 MPa. However, the compressive strength can be lowered severely by the decortication process. The standard decortication process induces kink bands in the fibres. These kink bands are found to contain cracks bridged by microfibrils. The failure behaviour of elementary flax fibres under compression can be described as similar to the failure behaviour of a stranded wire.     

Effect of heat treatment in air on the structure and properties of barium osumilite reinforced with Nicalon fibres

Microstructural studies have been carried out on glass-ceramic matrix composites, consisting of barium osumilite reinforced with Nicalon fibres, which have been subjected to heat treatment in air in the range 600–1100 °C. Parallel studies have involved the measurement of the friction stress between fibre and matrix and the flexural strength of the composite. The matrix was shown to consist of barium osumilite, hexacelsian, mullite and a silica-rich glass, the thermal mismatch of these different phases leading to the development of appreciable strains. Whilst high-temperature treatments caused the formation of voids due to flow of the glassy phase, the major factor controlling the mechanical properties of the composite was the fibre/matrix interface. A change in microstructure, from a weak carbon-rich interface to one where the fibre and matrix were strongly bonded together by a silica layer, was thus reflected in an increase in the interfacial friction stress and a change in fracture behaviour from one showing fibre pull-out and delamination to one with brittle characteristics.     

Tensile properties of chemically treated hemp fibres as reinforcement for composites

Natural fibres, unlike synthetic fibres fabricated in-house, grow naturally. Their geometrical and physical properties are highly affected by environmental issues such as climate change. For instance, inconsistent cross-sectional areas and shapes along the length of a natural fibre can result from environmental changes. These irregularities in natural fibres affect the ultimate load that can be carried by these fibres in structural engineering applications. In this study, the tensile properties of single hemp fibres were measured by taking into account, the variations in fibre diameters. Alkali, acetyl and silane treatments of fibres were carried out to obtain a better surface finish. The treatment effects on the fibres with respect to tensile properties were discussed. The relationship between tensile properties of treated fibres and the variation of their diameters was also studied. It was found that the tensile strength of chemically-treated fibres was lower than that of untreated fibres.     

Creep behaviour and structural characterization at high temperatures of Nicalon SiC fibres

Two types of Nicalon SiC fibres having different structures have been examined. Their mechanical properties and their microstructures have been studied up to 1300° C. The fall in strength above 1000° C has been shown to be due to the microcrystallization of the fibre structure. Under low loads this change in structure led to a shrinkage of the fibre. The fibres were found to creep at temperatures above 1000° C when loads greater than a threshold level were applied. The creep of the fibres has been shown to be controlled by the changes which occur to the fibre structure. Degradation of the fibres on heating in air or argon has been shown to depend on SiO₂ and free carbon, which have been shown to exist in the fibre.     

The oxidation behaviour of low-temperature heat-treated carbon fibres

The oxidation behaviour of partially carbonized polyacrylonitrile fibres was studied primarily by both dynamic and isothermal thermogravimetric analysis. These fibres, referred to as quasi-carbon fibres (QCFs), were obtained by pyrolysis of a polyacrylonitrile precursor at a heat-treatment temperature (HTT) ranging from 400–950°C. Results indicated that QC fibres exhibited increased thermal stability with increasing HTT. The oxidation behaviour was strongly related to the microstructure of QC fibres. An empirical model was developed to simulate the real oxidation process. Two different oxidation mechanisms were operational in QC fibres; one with a more moderate oxidation rate and the other with an auto-acceleration effect. Only the QC fibres that were heat treated above 650°C to develop an extended two-dimensional graphite-like structure, exhibited an auto-acceleration effect. This revised version was published online in November 2006 with corrections to the Cover Date.     

Electron-probe microanalysis of oxygen in heat-treated Orlon fibres

A method of using electron probe microanalysis to measure oxygen contents of heat treated Orlon fibres is described. The method utilizes specimens in the form of thin sections (～ 1 μm thick) which are coated with a thin layer of gold prior to analysis. It is shown that by comparing oxygen X-ray spectra obtained from inner and outer regions of certain heat-treated fibres the presence of oxygen gradients may be established. The findings are discussed in relation to rate controlling processes occurring during oxidation.     

Tensile behaviour of as deposited and heat-treated electroless Ni-P deposits

Electroless Ni-P coatings were deposited on mild steel substrates and the effect of heat-treatment on their structure and tensile behaviour was studied, with the following conclusions. The as-deposited electroless Ni-P coating is amorphous and it remains amorphous up to 300 °C. At 400 °C the coating becomes crystalline and consists of a Ni₃P matrix containing areas of metallic nickel. For the selected coating/substrate thickness ratio, the contribution of the coating in the tensile properties of the coating-substrate system is negligible as expressed by the values of yield strength, ultimate tensile strength and fracture strain in mild steel substrates and coated as-deposited and heat-treated specimens. Extensive cracking of the coating accompanied by spalling was occurred during the tensile tests. The density of cracks was found to increase close to the fracture surface of the tensile specimen and with increasing heat-treatment temperature. The cracks observed on the surface of the coatings are believed to form due to the inability of the brittle coating to accommodate the strain generated in the ductile substrate. Their orientation to the tensile axis is in close relation to the structure of the coating and the failure mechanism that is dictated by this structure. The first cracks on the surface of the coatings were found to form after the yield strength of the tensile specimen has been reached and plastic deformation of the substrate takes place. Their density increases with the accumulation of strain up to fracture.     

Microstructure property relationship in Pyrex glass composites reinforced with Nicalon fibres

Detailed microstructural studies have been carried out on a series of composites consisting of Pyrex glass reinforced with Nicalon fibres. A variety of techniques has been employed, including X-ray and electron diffraction, electron-probe microanalysis and thin foil analytical electron microscopy. In parallel, mechanical tests have been performed on the composites and measurements have been made of the fibre-matrix bond.Substantial amounts of cristobalite have been identified in the matrix, up to 48% by volume in some cases. At such levels, microcracking is a common occurrence due to the high differential contraction between the matrix constituents upon cooling, which leads to matrix disintegration upon mechanical testing. A second microstructural feature which affects the mechanical behaviour of the composite concerns the fibre-matrix interface and, in particular, the chemistry of the outermost (200 nm) surface regions of the fibre. The amount of graphite here is shown to affect directly the strength of the fibre-matrix bond and, in turn, the degree of fibre pull out and the mechanical properties of the composite.     

Tensile fatigue behaviour of PBO fibres

Poly(p-phenylene benzobisoxazole) (PBO) fibres are finding increasing applications on account of their exceptional stiffness and strength. This article presents results from tests on single PBO filaments, to characterize their intrinsic behaviour under quasi-static and cyclic tensile loading. Scanning electron microscopy is used to show the fibrillation mechanism leading to failure. Results are compared to data for polyester, aramid and high modulus polyethylene fibres. PBO fibres show shorter fatigue lifetimes than the other fibres when maximum stress is expressed as a percentage of quasi-static break load, but the absolute stress values applied are much higher for an equivalent lifetime.     

Characterization of Nicalon fibres with varying diameters: Part I Strength and fracture studies

Experimental studies have been conducted to examine the strength and fracture behaviour of monofilament Nicalon SiC fibres with diameters ranging from 8 to 22 m. The effects of varying fibre diameter, flaw location and flaw population on the mechanical response of individual fibres were investigated by recourse to extensive fractographic analysis performed on fibres fractured under tensile loading. Results indicate that variations in fibre diameter influence the apparent fibre fracture toughness (K1c), with higher K1c values observed for decreasing fibre diameters. Observations also suggest that the location of the critical flaw may play a role in the fracture of Nicalon fibres. Tensile strength values are shown to increase as the normalized distance of the critical flaw from the fibre centre increases, while critical flaw population appears to be strongly dependent on location. The ratio of K1c to geometry factor (Y) is observed to remain constant with varying flaw location. In addition to surface flaws, three distinct internal flaw populations are seen to cause fracture in Nicalon fibres. Based on these experimental findings, a statistical characterization of the strength of Nicalon fibres with varying diameters is presented in Part II of this paper. © 1998 Chapman & Hall     

Tensile static and fatigue behaviour of sisal fibres

The work describes the quasistatic tensile and fatigue behaviour of as-received sisal fibres. Natural-based reinforced composites are gaining significant interest within the structural community, due to their interesting mechanical properties, recyclability and environmentally-sustainable production and use. Natural fibres such as sisal constitute an excellent reinforcement material, due to the low extraction costs from plants, and high level of recycling involved in their manufacturing process. In this work the diameter, Young’s modulus, strength and strain to failure over 15 different samples are measured and compared against data from open literature. Tensile cyclic fatigue loading at eight loading levels (from 0.6 to 0.95) has been carried out. The maximum forces involved (between 9 N and 22 N) are considerably higher than the ones used previously in open literature, and lead to significant dependence of the hysteresis loops, energy dissipation and S–N behaviour of the sisal fibres versus the cycle and loading ratio levels. The results obtained from this work can be used to predict from a fatigue and structural integrity point of view the behaviour of sisal-based reinforced composites with high load bearing capability, and extend the design envelope of this class of natural-reinforced materials.     

Characterization of Nicalon fibres with varying diameters: Part II Modified Weibull distribution

Diameters vary significantly in a tow of commercial NicalonTM fibres, which is one of the most attractive ceramic reinforcements for structural composites. It was found that the strength distribution of Nicalon fibres could not be adequately characterized using either single- or bi-modal Weibull distribution. A recently proposed modified Weibull distribution can account for the effect of varying diameter in the characterization of fibre strength. To verify the validity of the modified Weibull distribution, comprehensive mechanical testing and fractographic studies have been conducted on Nicalon SiC fibres with diameters varying from 8 to 22 m. The experimental results have been reported in Part I. Part II of this paper further modifies the derivation of the modified Weibull distribution to yield a relationship which is similar in form, but soundly based on experimental findings. Factors considered in the modified Weibull distribution include the dependence of fracture toughness and flaw density on fibre diameter, both of which may vary with fibre diameter, as reported in Part I. Comparison with experimental data shows that the current modified Weibull distribution works very well, while both single-modal and bi-modal Weibull distributions are inadequate for describing Nicalon fibres with varying diameters. © 1998 Chapman & Hall     

Tensile strength and crack nucleation in boron fibres

Boron fibres of about 100m diameter have been tested to fracture in a micro-tensile testing machine. The fracture surfaces have been investigated using a scanning electron microscope and classified according to the fracture nucleation type. Comparison with the measured fracture stresses proved a significant correlation with the type of crack nucleation. Transverse cracks, nucleated at the edge of radial cracks along the fibre axis direction, are the most critical weakening feature. Also crack nucleation at the external fibre surface implies a low tensile strength, and is discussed in terms of a notch effect of the well-known nodular surface topography.