The effect of cure cycle heating rate on the fibre/matrix interface

Development of civil aerospace composites is key to future “greener” aircraft. Aircraft manufacturers must improve efficiency of their product and manufacturing processes to remain viable. The aerospace industry is undergoing a materials revolution in the design and manufacture of composite airframes. The Airbus A350 and Boeing 787 (both due to enter service in the latter part of this decade) will push utilisation levels of  composite materials beyond 50% of the total airframe by weight. This  change requires massive investment in materials technology, manufacturing capability and skills development. The Quickstep process provides the ability to rapidly cure aerospace standard composite materials whilst providing enhanced mechanical properties. Utilising fluid to transfer heat to the   composite component during the curing process allows far higher heat rates than with conventional cure techniques. The rapid heat-up rates reduce the viscosity of the resin system greatly to provide a longer processing window introducing greater flexibility and removing the need for high pressure during cure. Interlaminar fracture toughness (Mode I) and Interfacial Shear Strength of aerospace standard materials cured using Quickstep have been    compared to autoclave cured laminates. Results suggest an improvement in fibre-matrix adhesion.

Study on thermoplastic-modified multifunctional epoxies : influence of heating rate on cure behaviour and phase separation

The effect of heating rate on the cure behaviour and phase separation of thermoplastic-modified epoxy systems was investigated. Polyethersulphone (PES) modified multifunctional epoxies, triglycidyl-aminophenol (TGAP) and tetraglycidyldiaminodiphenylmethane (TGDDM), as well T300/914 prepreg were used. It was shown that heating rate had a significant influence on the cure kinetics and phase structures of investigated systems. Greater heating rate causes higher epoxy conversion. The domain size of the macrophases formed from phase separation increases with the increase of heating rate. A more complete phase separation is achieved by fast heated thermoplastic-modified epoxy blends.

The effect of a rapid heating rate, mechanical vibration and surfactant chemistry on the structure-property relationships of epoxy/clay nanocomposites

The role of processing conditions and intercalant chemistry in montmorillonite clays on the dispersion, morphology and mechanical properties of two epoxy/clay nanocomposite systems was investigated in this paper. This work highlights the importance of employing complementary techniques (X-ray diffraction, small angle X-ray scattering, optical microscopy and transmission electron microscopy) to correlate nanomorphology to macroscale properties. Materials were prepared using an out of autoclave manufacturing process equipped to generate rapid heating rates and mechanical vibration. The results suggested that the quaternary ammonium surfactant on C30B clay reacted with the epoxy during cure, while the primary ammonium surfactant (I.30E) catalysed the polymerisation reaction. These effects led to important differences in nanocomposite clay morphologies. The use of mechanical vibration at 4 Hz prior to matrix gelation was found to facilitate clay dispersion and to reduce the area fraction of I.30E clay agglomerates in addition to increasing flexural strength by over 40%.

Poly (vinyl alcohol) / silica nanocomposites: morphology and thermal degradation kinetics

The morphology of self-assembled poly(vinyl alcohol)/silica (PVA/SiO₂) nanocomposites is investigated with atomic force microscopy (AFM) and transmission electron microscopy (TEM). It is found that the SiO₂ nanoparticles are homogenously distributed throughout the PVA matrix in a form of spherical nano-cluster. The average size of the SiO₂ clusters is below 50 nm at the low contents (SiO₂ ≤ 5 wt%), while particle aggregations are clearly observed and their average size markedly increases to 110 nm when 10 wt% SiO₂ is loaded. The thermogravimetric analysis (TGA) shows that the nanocomposite significantly outperforms the pure PVA in the thermal resistance. By using a multi-heating-rate method, the thermal degradation kinetics of the nanocomposite with a SiO₂ content of 5 wt% is compared to the PVA host. The reaction activation energy (E) of the nanocomposite, similar to the pure PVA, is divided into two main stages corresponding to two degradation steps. However, at a given degradation temperature, the nanocomposite presents much lower reaction velocity constants (k), while its E is 20 kJ/mol higher than that of the PVA host.

One-dimensional growth of TiO2 nanorods from ilmenite sands

Growth mechanisms of TiO₂ nanorods synthesized from mineral ilmenite using ball milling and annealing method have been systematically investigated. Two annealing processes are needed to grow the nanorods. The heating rate and gaseous environment in the first annealing step are critical to the formation of intermediate phases; these and the annealing atmosphere in the second heating play very important roles in nanorod growth. One-dimensional growth of the nanorods induced by low-temperature annealing in nitrogen plus hydrogen is possibly driven by atom vacancy diffusion in addition to surface diffusion.

The effect of alternate heating rates during cure on the structure-property relationships of epoxy/MMT clay nanocomposites

This paper investigates the effect of both the mixing technique and heating rate during cure on the dispersion of montmorillonite (MMT) clay in an epoxy resin. The combination of sonication and using a 10. °C/min heating rate during cure was found to facilitate the dispersion of nanoclay in epoxy resin. These processing conditions provided a synergistic effect, making it possible for polymer chains to penetrate in-between clay galleries and detach platelets from their agglomerates. As the degree of dispersion was enhanced, the flexural modulus and strength properties were found to decrease by 15% and 40%, respectively. This is thought to be due to individual platelets fracturing in the nanocomposite. Complementary techniques including X-ray diffraction (XRD), small angle X-ray scattering (SAXS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX), transmission electron microscopy (TEM) and optical microscopy were essential to fully characterise localised and spatial regions of the clay morphologies.

Recrystallization of 304SS during and after high strain rate deformation

During the hot working of austenitic stainless steels the shape of the flow curve is strongly influenced by the strain rate. Low strain rate deformation results in flow curves typical of dynamic recrystallization (DRX) but as the strain rate increases the shape changes to a ‘flat-top’ curve. This has traditionally been thought to indicate no DRX is taking place and that dynamic recovery (DRV) is the only operating softening mechanism. Examining the work-hardening behaviour and corresponding deformation microstructures showed this is not the case for austenitic stainless steel, as clear evidence of dynamic recrystallization process can be seen. The post-deformation recrystallization kinetics can be modelled using a standard Avrami equation with an Avrami exponent, n, of 1.15. With an increasing value of the Zener-Hollomon parameter it was found that the kinetics of recrystallization become less strain rate sensitive until at the highest values (highest strain rates/lowest temperatures) the recrystallization kinetics become strain rate insensitive.

The influence of processing techniques on the matrix distribution and filtration of clay in a fibre reinforced nanocomposite

A nano-modified matrix based on an epoxy resin and montmorillonite (MMT) layered silicates, was successfully infiltrated through 10 ply of carbon fibre preform. A combined fabrication process of a vacuum assisted resin infusion method (VARIM) followed by a rapid heating rate and mechanical vibration during cure, facilitated the infiltration of the nano-modified matrix through the preform. This was achieved by dispersing the MMT clay in the resin and ensuring that the viscosity of the nano-modified matrix remained low during fabrication. SEM-EDX (energy dispersive X-ray spectroscopy) spectra showed that chemical constituents within MMT clay including silicon, aluminium and magnesium elements had permeated through the fibre preform and were detected throughout the laminate. A homogeneous resin/particle distribution was achieved with the size of clay particles ranging from 100 nm to 1 μm.