Preparation of carbon fibre reinforced aluminium via ultrasonic liquid infiltration technique

Abstract

An ultrasonic liquid infiltration technique has been developed for the fabrication of carbon fibre reinforced aluminium (CF/Al) precursor wires. The principal effect of ultrasound on aluminium infiltration into carbon fibres is considered to be caused by cavitation. The acoustic power required to produce cavitation in the present experimental system has been approximately calculated to be about 150 W, which is much greater than the requirement, several tens of watts, for overcoming the capillary pressure among carbon fibres. The observations on the morphology of the CF/Al precursor wires show that there are generally four states of infiltration: totally non-infiltrated, non-infiltrated in the centre and in some local regions of the wires, and completely infiltrated. It is found that carbon fibres can be sufficiently impregnated by molten aluminium given the appropriate application of ultrasound. Furthermore, a single fibre tensile test shows that there is no strength degradation of carbon fibres after aluminium infiltration. The CF/Al precursor wires obtained have an average fibre volume fraction of 26%. The maximum longitudinal tensile strength of the CF/Al wires is 605 MN m^?2, which implies a fibre strength transfer efficiency of 0·76.

MST/1715     

Mechanical properties of T300/Al composites. Embrittlement effects due to a B4C coating

During the preheating treatment preceding the processing of C/Al composites, a decrease in the mechanical properties of the carbon fibres is generally observed, owing to the oxidation of the fibres. Thus, it implies the use of a surface coating likely to resist the oxidation of the fibres. In this work, we chose to protect the carbon fibres by a B₄C coating, using a RCVD process. This coating leads to an effective protection against oxidation, as was shown by the mechanical properties obtained by single fibre tests on the coated fibres before and after preheating. However, although this coating also protects the fibres against the reaction with liquid aluminium during processing, the tensile properties of the composite were very weak. An analysis of these results based both on the use of loose bundle tests and on a microstructural characterization of the reinforcement and of the composite by transmission electron microscopy (TEM) observations and by electron spectroscopy for chemical analysis (ESCA) led us to the conclusion that the local overthicknesses of the B₄C coating have an embrittling effect, leading to a premature failure of the composite.     

Compatibility between alumina fibres and aluminium

An investigation is carried out on the interfacial wetting behaviour and reactions between aluminium and alumina fibres (85mass% Al₂O₃ and 15mass% SiO₂). Aluminium is coated onto alumina fibres by a vacuum evaporation technique and the surface of the fully coated fibres and the edge of the partially coated fibres are examined by scanning electron microscope after heat treatments at various temperatures. Within a temperature regime between 943 and 1273 K, occurrence of such interfacial reactions as 4Al(I) + Al₂O₃(s) 3Al₂O₃(g) and 4Al(I) + 3SiO₂(s) 2Al₂O₃(s) + 3Si(s) are detected. It is found that molten aluminium can cover the alumina fibre surface but it peels off near the edge of the coating film on a partially coated fibre, showing the very weak interface cohesion. This is ascribed to the lack of a stable compound formation at the interface. Results of tensile test show that the strength of the coated fibres is degraded after heat-treating at above the melting point of aluminium. The culprits for the tensile failure of alumina fibres are evaluated by the Weibull distribution theory.     

Characteristics of several carbon fibrereinforced aluminium composites prepared by a hybridization method

The properties and microstructures of several high-strength and high-modulus carbon fibrereinforced aluminium or aluminium alloy matrix composites (abbreviated as HSCF/Al and HMCF/Al, respectively, for the two types of fibre) have been characterized. The composites evaluated were fabricated by pressure casting based on a hybridization method. It was found that the strength degradation of high-modulus carbon fibres after infiltration of aluminium matrices was not marked and depended upon the type of aluminium matrix. However, the strength of high-strength carbon fibres was greatly degraded by aluminium infiltration and the degradation seemed to be independent of the type of aluminium matrix. The longitudinal tensile strength (LTS) of CF/Al composites was very different between HMCF/Al and HSCF/Al composites. The HMCF/Al composites had LTS values above 800 MPa, but the HSCF/Al composites had only about 400 MPa. In contrast, the transverse tensile strength of the HSCF/Al composites, above 60 MPa, was much higher than that of the HMCF/Al composites, about 16 MPa. Chemical reactions were evident to the interface of high-strength carbon fibres and aluminium matrices. There was no evidence of chemical products arising between high-modulus carbon fibres and Al-Si alloy and 6061 alloy matrices. However, it was considered that some interfacial reactions took place in pure aluminium matrix composites. Fracture morphology observation indicated that the good LTS of CF/Al composites corresponded to an intermediate fibre pull-out, whereas a planar fracture pattern related to a very poor LTS and fibre strength transfer. The results obtained suggested that interfacial bonding between carbon fibres and aluminium matrices had an important bearing on the mechanical properties of CF/Al composites. An intermediate interfacial bonding is expected to achieve good longitudinal and transverse tensile strengths of CF/Al composites.     

Behaviour of coatings on reinforcements in some metal matrix composites

Coating on reinforcements affects the interface bonding of a composite, and is therefore usually used for improving the composite's properties. The behaviour of SiC coating on carbon fibre in reinforced aluminium metal castings, Fe on carbon fibre-reinforced copper and alumina coating on K₂O · 6TiO₂ whisker-reinforced aluminium composites were investigated, respectively, by modern techniques such as TEM, SEM etc. with the goal of controlling the interfacial interaction and wettability of reinforcement with the matrices. SiC coating produced by a polycarbosilane solution process effectively improved the strength because it successfully controlled oxidation of the carbon fibres themselves and the harmful reaction between the carbon fibres and molten aluminium during the fabrication process and heating process of the composites. The metal coating, Fe, made by electrical plating, strengthened the bonding of carbon fibres with copper by changing the bonding state of the interface from a mechanical one to a partly chemical one. Therefore the strengths of the resulting composites were improved. The alumina coating on K₂O · 6TiO₂ also controlled the diffusion of the K element from the whiskers into the aluminium matrix and altered the reaction with aluminium, and led to the optimization of interfacial bonding between the whiskers and a superior composite.     

Surface oxidation of carbon fibre on tribological properties of PEEK composites

Abstract

In this work, ozone modification method and air oxidation were used for the surface treatment of polyacrylonitrile (PAN) based carbon fibre. The surface characteristics of carbon fibres were characterised by X-ray photoelectron spectroscopy. The interfacial properties of carbon fibre reinforced PEEK (CF/PEEK) composites were investigated by means of the single fibre pull-out tests. As a result, it was found that IFSS values of the composites with ozone treated carbon fibre are increased by 60% compared with that without treatment. X-ray photoelectron spectroscopy results show that ozone treatment increases the amount of carboxyl groups on carbon fibre surface, thus the interfacial adhesion between carbon fibre and PEEK matrix is effectively promoted. The effect of surface treatment of carbon fibres on the tribological properties of CF/PEEK composites was comparatively investigated. Experimental results revealed that surface treatment can effectively improve the interfacial adhesion between carbon fibre and PEEK matrix. Thus the wear resistance was significantly improved.     

Effect of alumina coating and extrusion deformation on microstructures and thermal properties of short carbon fibre–Al composites

Short carbon fibres were coated with alumina by sol–gel process. Uncoated and alumina-coated short carbon fibre–Al composites were fabricated by gas pressure infiltration process. The effects of alumina coating and extrusion deformation on microstructures and thermal properties of the composites were studied. The results show that alumina coating is effective to improve the quality of the short carbon fibre preform as well as act as diffusion barrier to impede interfacial harmful chemical reactions between aluminium and short carbon fibres, which would increase the thermal properties of the composites. Extrusion deformation can orient the carbon fibres to the extrusion direction to improve their degree of orientation, meanwhile decreasing their aspect ratio. Extrusion deformation has a beneficial effect on the thermal conductivity of the composites. However, its effect on coefficient of thermal expansion of the composites is small because the effects of the improvement in degree of orientation and the decrease of aspect ratio tend to cancel each other somewhat.     

Mechanical damping and dynamic modulus measurements in alumina and tungsten fibre-reinforced aluminium composites

Simultaneous measurements of mechanical damping, or internal friction (Q ^–1 ), and dynamic Young's modulus (E) were made near 80 kHz and at strain amplitudes () in the range 10^–8 to 10^–4 on small specimens of continuous or chopped fibre-reinforced metal matrix composites (MMCs): 6061 aluminium reinforced with alumina (Al/Al₂O₃) and 6061 aluminium reinforced with tungsten (Al/W). Baseline experiments were also done on 99.999% aluminium (pure Al). The strain amplitude dependence of damping and the temperature dependence of dynamic modulus were of particular interest in this study. The temperature (T) dependence of the modulus from room temperature up to 475° C was determined for the Al/Al₂O₃ and pure Al specimens and a highly linear decrease in modulus with increasing temperature was observed. The rate of modulus loss (dE/dT –80 M Pa° C^–1 ) was the same for both materials and the reduction in modulus of the Al/Al₂O₃ was attributed to the reduction in modulus of the alu minium matrix, not the alumina fibres. The size, type, and amount of fibre reinforcement were found to have a significant effect on the strain amplitude dependence of the damping in both MMCs. Unreinforced aluminium exhibited classical dislocation damping trends with a region of strain amplitude independent damping at low strains (less than 10^–5) followed by a non linear, strain amplitude dependent region at higher strains. The addition of alumina fibres (chopped or continuous), while increasing stiffness, resulted in a significant reduction in damping capacity for the MMC relative to that for aluminium and near complete suppression of the amplitude dependent response. The damping levels increased as the volume fraction of fibre, and therefore, the amount of fibre/matrix (FM) interface decreased, indicating that the matrix, not factors such as increased dislocation densities at the FM interface, was the dominant influence on the damping. Analysis of the Al/Al₂O₃ results by Granato-Lücke (GL) theory indicated that dislocation densities were increased relative to those in aluminium, but the dis locations were well pinned and unable to increase damping levels effectively. Analysis of the Al/W results by GL theory also revealed high dislocation densities, but, unlike the Al/Al₂O₃ specimens, the Al/W specimens (continuous fibres) exhibited strong amplitude dependent damping (starting near strain levels of 2 × 10^–6) with damping levels approximately twice those of pure aluminium. Trends showed increased damping with increased fibre diameter, not with increased FM interface area. There was some evidence that it was the tungsten fibre itself that dominated the damping behaviour in Al/W composites, not the aluminium matrix or the FM interface.     

Influence of fibre surface oxidation treatment on mechanical interfacial properties of carbon fibre/ polyarylacetylene composites

Abstract

In the present work, the mechanical interfacial properties of carbon fibre (CF) reinforced polyarylacetylene (PAA) resin composites were modified through the surface oxidation treatment of carbon fibres by ozone. Both X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) spectroscopy showed that oxidation treatment could increase the amount of elemental oxygen on the fibre surface markedly by introducing more oxygen groups. Atomic force microscopy (AFM) images indicated that weak surface regions of fibres had been etched and removed, and the degree of fibre surface roughness was increased. The interlaminar shear strength (ILSS) and the interfacial shear strength (IFSS) of CF/PAA composites were both improved notably (no less than 50%). It could be concluded that an improvement of fibre surface chemical activity, better wettability of resin on the carbon fibre surface, and stronger mechanical joining between fibres and resin all resulted in the modification of interfacial properties of carbon fibre reinforced PAA composites. The influences of temperature, ozone concentration, and treatment time on the oxidation results were studied, and optimal treatment parameters determined.     

Improvement of the temperature resistance of aluminium-matrix composites using an acid phosphate binder

The use of phosphate binders instead of the widely used silica binder resulted in improved temperature resistance, increased tensile strength and decreased coefficient of thermal expansion. The effects were largest for the phosphate binder which contained the largest amount of phosphoric acid (P/Al atom ratio = 24 in the liquid binder). These effects were probably due to the protection of the SiC whiskers by the binder phases (aluminium metaphosphate or aluminium orthophosphate), the binder-SiC reaction product (SiP₂O₇) and the binder-aluminium reaction product (AIP) from further reaction between the SiC and aluminium. The tensile strength of the composite containing the SiC whisker preform made with the phosphate binder (P/Al atom ratio = 6 or 24 in the liquid binder) was increased after heating at up to 600 °C for 240 h. The silicon phosphate (SiP₂O₇) acted as an in situ binder and was primarily responsible for increasing the compressive strength of the preform and increasing the temperature resistance of the composite. The carbon fibre composite containing the preform made by using the phosphate binder (P/Al atom ratio = 24 in the liquid binder) with either water or acetone as the liquid carrier during wet forming of the preform had a higher tensile strength than the carbon fibre composite made by using the silica binder. After composite heat exposure to 600 °C for 14 h, the carbon fibre composite made by using this phosphate binder with acetone as the liquid carrier during wet forming of the preform showed the best temperature resistance, while the carbon fibre composites made by using this phosphate binder with water as the carrier showed the second best temperature resistance, and that made by using silica binder was the worst. The reason for the better effect of the phosphate binder than the silica binder is probably due to the ability of the phosphate binder and the binder-aluminium reaction product (AIP) to protect the carbon fibres from the undesirable reaction between the carbon fibres and aluminium. The lack of a binder-fibre reaction contributed to making the carbon fibre composites less temperature resistant than the SiC whisker composites. The use of a higher binder concentration is attractive for increasing the temperature resistance of the composites. The binder concentration in the preform can be increased by increasing the binder concentration in the slurry used in the wet forming of the preform.     

Secondary ion mass spectrometry and multireflection infrared analyses of conversion coatings on Fe–Cr–Al stainless steels for catalysis: study of thermal stability

Abstract

The thermal stability of three stainless steel conversion coatings for high temperature applications (e.g. photothermal conversion catalysis) are investigated. The thermal oxidation in air up to 1000°C of Fe–17Cr, Fe–18Cr–1·3Al, and Fe–22Cr–5Al coatings (all wt-%) are compared. This study has revealed a critical temperature below which the coating thickness is preserved; the critical temperature increases and the thermal oxidation of the conversion coating decreases with higher chromium and aluminium content. This is attributed to the difference in the substitution ratio of γ lacunar phase (additionally oxidised substituted magnetite), which is the main component of the conversion coatings. The thermal stability of this phase is higher when it is richer in chromium or aluminium. Higher contents of these elements raise the temperature of formation of chromite (FeCr₂O₄) and alumina, the occurrence of which causes thickening of the coating during thermal treatment.

MST/1891     

Effect of aluminium in thermal oxidation of Fe–Cr–Al conversion coating for catalysis

Abstract

The use of coatings having special properties for photothermal conversion or catalysis is often complicated by problems of high temperature stability. This study deals with the effect of aluminium, as an additional element inferritic stainless steel, on the behaviour of Fe–Cr–Al conversion coatings during their thermal oxidation in air up to 1000°C. X-ray diffraction and infrared spectrometry show that the main component of the coating is a chromium, aluminium substituted magnetite and that the presence of aluminium slows down the oxidation rate of the coating-substrate system mainly owing to the formation of mixed iron oxides containing aluminium and of alumina.

MST/1400     

Interface analysis in Al and Al alloys/Ni/carbon composites

Nature of fibre/matrix interfaces existing in Al/C composites were investigated depending on the presence of a nickel interlayer deposited on carbon fibres and on the composition of the aluminium matrix. Auger and electron microprobe analyses were used. The role of the nickel layer on the chemical evolution of the system after a 96 h heat treatment at 600°C is discussed. The presence of this nickel layer limits the diffusion of carbon into aluminium, and thereby, eliminates the formation of a carbide interphase, Al₃C₄, which is known to lower the mechanical properties of Al/C composites. The mechanisms differ according to the composition of the matrix. In the case of pure aluminium, an Al-Ni intermetallic is formed after thermal annealing. It does not react with the carbon fibre and so inhibits the growth of Al₃C₄. In the case of the alloyed matrix (AS7G0.6), the dissolution of the Ni sacrificial layer, after annealing, does not lead to the same Al-Ni intermetallic but a thin nickel layer remain in contact with the carbon fibre avoiding formation and growth of Al₃C₄ carbide. This difference of behaviour is tentatively ascribed to the presence of silicon that segregates at the fibre/matrix interface.     

A TEM study of the interfaces and matrices of SiC-coated carbon fibre/aluminium composites made by the K2ZrF6 process

Carbon fibre-reinforced aluminium composites were pressurelessly cast by using K₂ZrF₆ as the wetting promotion agent. Transmission electron microscopy (TEM) and energy dispersed analysis of X-rays, (EDAX) were used. The results showed that interfacial reactions were very active after K₂ZrF₆ treatment. This was caused by the diffusion and reaction of zirconium in the surface of carbon fibres or in the SiC coating. Silicon alloying of aluminium could suppress the interfacial reactions by decreasing the activity of zirconium and changing intermetallic Al₃Zr to Zr₃Al₄Si₅, and building up the phase equilibrium between SiC, aluminium and silicon. The requested silicon content was higher than the equilibrium content of Al-Si-SiC system to suppress the SiC/Al interfacial reaction. A perfect interface was achieved in SiC-coated carbon fibre Al-12 wt% Si composite.     

Studies on nickel coated carbon fibres and their composites

Uniform and continuous coating of nickel was given to the carbon fibres by cementation, electroless or electroplating techniques. The coating thickness was ranged between 0.2 and 0.6 m for all the three methods used. Coating thickness less than 0.2 m showed discontinuous coating of nickel over the fibre surface. Beyond 0.6 m thickness, nickel deposited in den-drite form over the continuous coating. For continuously coated fibres, the ultimate tensile properties of electroless coated fibres were near to uncoated carbon fibres suggesting adherent and defect free coating; while fibres coated by electrolytic and cementation process exhibited lower ultimate tensile strength (UTS) properties. The tensile fracture of the cementation coated fibres suggested degradation of the fibres. In composites, prepared by dispersing the coated fibres in pure aluminium matrix, no appreciable fibre-metal interaction was observed. NiAl₃ intermetallics were observed around and adjacent to the carbon fibres. Sometimes carbon fibres were found embedded in massive NiAl₃ intermetallics suggesting that fibre surface can also act as nucleating centre for these precipitates.     

溶胶-凝胶法TiO2涂层碳纤维增强铝基复合材料的研制

以钛酸丁酯为原料,醋酸为螯合剂,通过水解缩合制得TiO2溶胶.研究了溶胶-凝胶法在碳纤维上涂覆TiO2氧化物陶瓷的连续工艺,采用了IR、TG-DTA、XRD、SEM等分析表征手段.结果表明,溶胶液的粘度是决定涂层质量的关键因素,涂层有效的覆盖了碳纤维表面的裂纹和缺陷;与原纤维相比,锐钛矿型TiO2涂层碳纤维的抗氧化性和耐高温性能均有提高.涂层后碳纤维与熔融铝的润湿性和相容性明显改善,涂层有效的阻止了碳/铝界面反应,使预制丝强度明显提高.     

Influence of fibre surface oxidation–reduction followed by silsesquioxane coating treatment on interfacial mechanical properties of carbon fibre/polyarylacetylene composites

Carbon fibre was treated with oxidation–reduction followed by silsesquioxane coating method to improve the interfacial properties of carbon fibre/polyarylacetylene (CF/PAA) composites. The treatment method was divided into three phases, i.e., oxidation with oxygen plasma, reduction with LiAlH₄, and coating treatment with vinyl silsesquioxane (VMS–SSO). The fibre surface composition and functional group were analyzed using X-ray photoelectron spectroscopy (XPS). The polar functional groups, especially C–OH which could react with Si–OH on silsesquioxanes, were increased after redox reaction. VMS–SSO coating treatment imported vinyl groups which could react with PAA resin during PAA cure process. The surface morphology of carbon fibre was observed by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The mechanical interfacial properties of the CF/PAA composites were characterized by short-beam bending testing method. Interlaminar shear strength (ILSS) of the CF/PAA composites in different treatment phases were increased by 31.7%, 28.8%, and 59.3%, respectively. The conclusion that oxidation–reduction followed by silsesquioxane coating treatment is an effective method to improve the interfacial properties of the CF/PAA composites can be drawn. This method can be used in other resin systems if the functional groups on silsesquioxane are changed according to those in resins.     

Anorganische Fasern. Herstellung,Eigenschaften und Verwendung

Inorganic Fibres – Fabrication, Properties and Application Glass- and carbon fibres are preferred reinforcement materials for composites with polymer matrix. Basing on an analysis of their properties it is shown that other inorganic fibres can combine the advantages of both, and avoid their disadvantages. Boron-, siliconcarbide- and alumina-fibres are discussed in detail. The boron fibre has a YOUNG's modulus up to 45 MN/m² and a strength of 3000–4000 MN/m² as well as high compressive and shear strength. Therefore the boron fibres are superior to the carbon fibres as high modulus reinforcement material. The disadvantages of the boron fibres are their complicated fabrication process (chemical vapour deposition on a tungsten monofilament), and their only availability in form of monofilaments with diameters of at least 60 μm. The boron fibre recristallizes at 6000 °C and reacts also with the tungsten substrat. Thus, its application at elevated temperatures is limited. The SiC-fibre shows the same mechanical properties as the boron fibre but it can be fabricated by chemical vapour deposition also on a carbon monofilament. The advantages are the chemical compatibility with carbon substrat and the resistance against oxidation. The disadvantage is the higher density compared with that of boron (3,5 against 2,6 · 10³ kg/m³) Carbon yarns (with 10 000 monofilaments of 10 μm diameter) with SiC coatings of 0,5 μm can be seen as an alternative to the relatively thick SiC-monofilaments with 60 μm diameter. The advantage of such coated carbon yarn is a better applicability in fibre reinforced composite materials. There exists a further alternative preparation process for SiC-yarn, namely the spinning of polycarbosilanes with subsequent formation of SiC by pyrolysis treatment. Al₂O₃-fibres are chemically inert against most oxidic and metallic matrix materials, and promises to be candidate reinforcement materials for aluminium. They can be prepared by melt-spinning process as well as by a hydrolysis-process starting from aluminium organic compounds with subsequent heat treatment for thermal decomposition. The properties of all these fibre materials are compared with those of glass-, polyamid- and carbon-fibres as well as with metal wires.     

Control of interfaces in Al-C fibre composites

The interface of Al-C fibre composite was modified by coating a silver layer on the surface of carbon fibres prior to making composites, in an attempt to improve the wettability between molten aluminium and carbon fibres during infiltration. An electroless plating technique was adopted and perfected to provide a homogeneous silver coating on the carbon fibre surface. Al-C fibre composites were prepared using a liquid infiltration technique in a vacuum. It was found that silver coating promoted the wetting between aluminium and carbon fibres, particularly with polyacrylonitrile-base carbon fibres. However, due to rapid dissolution of silver in molten aluminium, it was believed that the improved infiltration was not due to the wetting behaviour between molten aluminium and silver. The cleaning of the fibre surface and the preservation of the cleaned carbon surface with silver coating was considered to be the prime reason for the improved wettability. Interfacial reactions between aluminium and carbon fibres were observed. Amorphous carbon was found to react more with aluminium than graphitic carbon. This is believed to be because of the inertness of the graphitic basal planes.     

Assessment of diffusion barriers for Ti–SiC composites

Abstract

The application of chemical vapour deposition and physical vapour deposition coatings, either singly or in combination, onto SiC fibres is discussed in terms of their ability to enhance the high temperature stability of Ti–SiC composites. The thermal stability and success of potential barrier layers was assessed by studying the fibre-matrix interdiffusion and measurement of the mechanical properties of individual fibres following coating and thermal exposure. Measurements of the level of strength retention have proved to be a reliable method of assessing the effectiveness of potential diffusion barriers. Failures may result from one of three sources. For high strength fibres failures are SiC–core reaction zone initiated, for intermediate strength fibres failures are surface defect (SiC) initiated and for low strength fibres, failures are fibre–matrix reaction zone or coating initiated. To ensure high strength (i.e. core failures) it is essential that a carbon layer is retained at the SiC surface. The most successful barriers have been shown to be TiB₂ and PtAl₂ coatings preventing outward diffusion of carbon and minimising the interaction with the titanium matrix. From these results a life prediction model has been developed based on the fibre–coating interaction, which will predict fibre strength as a function of time at a given temperature.

MST/3001