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.

Manufacturing process effects on the mode I interlaminar fracture toughness and nanocreep properties of CFRP

Quickstep ™ is a fluid filled floating mould technology which was recently developed by an Australian company of the same name. The Quickstep and conventional autoclave manufacture of composites were compared by investigating the mode I interlaminar fracture toughness and nanocreep propeties of HexPly914 carbon epoxy composites. It was found that composites cured using the Quickstep technology had significantly higher fracture toughness (1.8 times) than the composites cured via autoclave for this system. DMTA (dynamic mechanical thermal analysis) results showed a higher Tg (glass transition temperature) for the material manufactured by the Quickstep than that cured by the autoclave. FTIR (Fourier transform infrared spectroscopy) spectra did not indicate any difference in cure chemistry between the two processes. Nanocreep experiments were performed to explore the viscoelastic properties of the epoxy matrix of composites. The KelvinVoigt three-element model was applied to analyse the indentation creep behaviour of both composites.

Inspection of drop-weight impact damage in woven CFRP laminates fabricated by different processes

The influence of manufacturing process on the drop-weight impact damage in woven carbon/epoxy laminates was inspected by visual observation, dyepenetrant X-ray technique, and optical microscopy observation. The MTM56/ CF0300 woven quasi-isotropic laminates were fabricated by two processes: the autoclave and the Quickstep processes. Quickstep^TM is a novel composite manufacturing process, which was designed for the out-of-autoclave production of high-quality composite parts at lower cost. It utilizes higher heat conduction of fluid other than gas to transfer heat to components, which results in much shorter cure cycles. The laminates cured by this fast heating process showed different impact failure modes from those cured by the conventional autoclave process. The residual indentation in the top side of the Quickstep-cured laminates had a bigger diameter, but a smaller depth at the same impact energy level. Dye-penetrant X-ray revealed more intense and connected impact damage regions in the autoclave-cured laminates. Optical micrography as a supplementary method showed less severe matrix damage in the quickstep-cured laminates indicating a more ductile property of the resin matrix cured at a faster heating rate.

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.

Composite crashworthy structures

This study presents an innovative finite element delamination model which successfully reproduced the experimental failure behaviour observed in axial crush testing. Tests were conducted on tubes manufactured by a novel composite curing process, resulting in the ability to cure tubular profiles in 7 minutes - 95% quicker than traditional autoclave curing.

Fracture behaviour of a rapidly cured polyethersulfone toughened carbon fibre/epoxy composite

An out-of-autoclave rapid heating/low pressure technique has been used to cure polyethersulfone (PES) toughened HexPly 8552. Mode I and mode II tests were conducted to evaluate the fracture toughness of the composites and the effectiveness of cure was determined through thermal analysis. When compared to the autoclave process, the out-of-autoclave process resulted in a 52% reduction in processing time, without any sacrifice to the matrix intrinsic properties. Thermal analysis indicated an 8 °C improvement in glass transition temperature (T_g) as a result of an increased degree of cure. The out-of-autoclave process did lack in the ability to facilitate the removal of porosity which affected the fracture toughness results. The porosity is believed to have increased the mode I propagation fracture toughness. However its effect on mode II was quite deleterious, shown by scanning electron microscopy (SEM). This study managed to identify a number of key parameters associated with the out-of-autoclave process essential for further optimisation.

Stability of oxide films formed on mild steel in turbulent flow conditions of alkaline solutions at elevated temperatures

In the industries involving alkaline solutions in different process streams, the nature and stability of oxide films formed on the metallic surfaces determine the rates of erosion–corrosion of the equipment. In the present study the characteristics of the oxide films formed on AISI 1020 steel in a 2.75 M sodium hydroxide solution at temperatures up to 175°C, have been investigated by employing electrochemical techniques of cyclic voltammetry and chronoamperometry. The experiments were carried out in an autoclave system based upon a ‘rotating cylinder electrode’ geometry to determine the effects of turbulence on the stability of the films. The results suggest that little protection is afforded in the active region (at about −0.8 V_SHE). In the passive region at low potentials (−0.6 V to −0.4 V_SHE), it appears the films are compact and more stable, and therefore provide good protection. At higher potentials (>−0.4 V_SHE) in the passive region, the results suggest that film formation and dissolution occur simultaneously and the increase in temperature and turbulence causes a breakdown of the passive film resulting in a situation similar to nonprotective magnetite growth.

Effect of manufacturing method and aging environment on painted automotive carbon fibre composite surfaces

In this paper, the effect of various aging environments on the painted surface finish of unidirectional carbon fibre composite laminates, manufactured by autoclave and a novel out-of-autoclave technique was investigated. Laminates were exposed to water immersion, 95 % relative humidity and cyclic environments for 552 h and the surface finish was evaluated using visual and wave-scan distinctness of image (DOI) techniques. It was found that the laminate surface finish was dependent on the amount of moisture in the aging test. Minor surface waviness occurred on the laminates exposed to the cyclic test, whereas, surface waviness, print through and DOI values were all significantly higher as the laminates absorbed larger quantities of moisture from the hygrothermal and hydrothermal tests. The water immersion test, which was the most detrimental to the surface finish of the painted laminates, produced dense blistering on the autoclave manufactured laminate surface whereas the out-of-autoclave laminate surface produced only a few. It was found that the out-of-autoclave laminate had high substrate surface roughness which resulted in improved paint adhesion and, therefore, prevented the formation of surface blistering with aging. © 2012 Springer Science+Business Media Dordrecht.

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%.

Energy absorption behaviour of rapidly manufactured carbon/epoxy and glass/polypropylene structures

In this thesis the crashworthiness of composite tubular structures was investigated along with the property structure relationships of a glass/polypropylene material. The energy absorption capacity of tubular structures in a number of different testing configurations was made. Two materials; carbon/epoxy pre-preg and a glass/polypropylene dry pre-preg were investigated.

Carbon nexus: a strategic overview and research highlights

Carbon Nexus (www.carbonnexus.com.au) is a globally significant research facility at Deakin University focused on the manufacture and use of carbon fibre. Carbon Nexus represents a partnership between Deakin University and the Victorian Centre for Advanced Materials Manufacturing (VCAMM) and houses two production lines capable of manufacturing industrially relevant quantities of aerospace grade carbon fibre. The facility enables scientists to conduct research into the chemical, mechanical and nano-scale characteristics of new carbon fibre materials produced on site. There is a strong focus on evaluating these new carbon fibre products in composite materials, particularly composites cured using out-of-autoclave techniques. This paper will present an overview of the vision for Carbon Nexus as well as the technical capabilities of both the laboratory scale single tow line and the larger pilot line capable of producing up to 50 tons of carbon fibre per year. Both lines are fully operational and able to convert a range of polymer precursors into carbon fibre. They are representative of world's best practice for carbon fibre manufacturing methods and well suited to conducting energy efficiency studies. Highlights from recent research projects will focus on the effect of the surface treatment and sizing of carbon fibre on fibre-matrix adhesion in composite materials. In addition to this, results from studies of the effect of varying processing parameters on the structure and properties of oxidised polyacrylonitrile and carbon fibre will also be presented.

Estabilização pozolânica de cinzas volante e pesada com cal dolomítica hidratada e areia, curadas pelos processos de autoclavagem e câmara a temperatura constante

Este trabalho tem como objetivo verificar o comportamento mecânico e físico de pozolanas artifíciais estabilizadas química e granulometricamente, curadas por dois processos de cura denominados de : autoclave(ATC), que utiliza temperaturas na faixa de 149 a 188°C e câmara à temperatura constante(CTC) que utiliza uma temperatura de ± 21°C. Também fez-se análises estatísticas com a finalidade de se determinar o efeito da energia de moldagem, temperatura e tempo de cura sobre os resultados dos ensaios, para cada processo de cura, além de se determinar modelos matemáticos para previsão de resultados de resistência através de regressões múltiplas e simples. As pozolanas artificiais empregadas foram as cinzas volante e pesada da Usina de Candiota, as quais foram estabilizadas com cal dolomítica hidratada e areia do Rio Guaíba. Os ensaios de resistência à compressão simples , absorção e perda de massa basearam-se nas normas da ABNT e DNER e para os estudos de análise estatística, fez-se anteriormente aos ensaios, dois planejamentos experimentais denominados de Split-Splot e Quadrado Latino, que foram utilizados nos processos de autoclavagem e câmara à temperatura constante, representativamente. Os Corpos-de-Prova curados na câmara à temperatura constante, até os 28 dias de cura, apresentaram resultados de resistências inferiores aqueles curados pelo processo de autoclave. Aos 60 dias de cura suas resistências ficaram na faixa dos valores de Corpos-de-Provas curados pela autoclave nas temperaturas de 149 a 188°C, excessão feita na mistura utilizando areia, onde em todos os períodos de cura estudados,os valores de resistência dos Corpos-de-Prova curados pelo câmara à temperatura constante foram inferiores. A proporção da quantidade de cal e cinza na mistura, bem como o valor da superfície específica da cinza influenciam nos resultados de ensaios, independentemente da variação dos fatores principais. Em termos de análise estatística verificou-se que a energia de moldagem e o tempo de cura são os fatores que apresentam os maiores efeitos sobre os resultados da resistência, para os processos de cura ATC e CTC, respectivamente.

Atividade de proteases e disponibilidade de nitrogênio para laranjeira cultivada em Latossolo Vermelho distrófico

O conhecimento do potencial da mineralização dos compostos orgânicos nitrogenados do solo é fundamental para o uso eficiente do N em sistemas de produção agrícola. Com o objetivo de avaliar a atividade de proteases e suas relações com os teores de diferentes formas de N em Latossolo Vermelho distrófico cultivado com laranjeira, foram coletadas amostras de solo em duas profundidades (0-10 e 10-20 cm), na linha de projeção da copa e nas entrelinhas, nos meses de novembro e dezembro/98, fevereiro e março/99. em março/99, época recomendada para a diagnose foliar, também foram coletadas amostras de folhas. As amostras de solo foram avaliadas com relação à atividade de proteases e aos teores de N-amoniacal, N-nitrato, N-total, N-amoniacal obtido após incubação anaeróbia (N-pot) e N-amoniacal extraído por solução de CaCl2 sob autoclavagem (N-autoclave). Nas amostras de folha, determinou-se o teor de N-total. A atividade de proteases foi influenciada pelo local e pela profundidade de amostragem, tendo sido mais elevada na linha de projeção da copa e profundidade de 0-10 cm. A aplicação de fertilizante orgânico causou aumento na atividade de proteases, principalmente na camada de 0-10 cm. O coeficiente de correlação entre atividade de proteases e outros métodos para avaliação da disponibilidade de N dependeu da época, do local e da profundidade de amostragem. A correlação entre o N-foliar, obtido na época indicada para diagnose foliar, a atividade de proteases e as demais formas para avaliar disponibilidade de N (N-amoniacal, N-nitrato, N-autoclave e N-pot) variou com a época de amostragem. A atividade de proteases foi positiva e altamente correlacionada com o N-foliar, obtido na época indicada para fins de diagnose foliar, para amostras de terra retiradas nas entrelinhas (0-10 cm), no mês de dezembro/1998.

Transferência de calor transiente na agitação linear intermitente de latas

Foi estudada a transferência de calor transiente na agitação linear e intermitente (ALI) de embalagens metálicas contendo simulantes de alimentos, objetivando-se sua aplicação em processos de pasteurização ou esterilização e conseqüentes tratamentos térmicos mais eficientes, homogêneos e com produto de melhor qualidade. Foram utilizados quatro meios fluidos simulantes de alimentos de diferentes viscosidades e massas específicas: três óleos e água. Foram combinados efeitos de cinco tratamentos, sendo: meio simulante (4 níveis), espaço livre (3 níveis), freqüência de agitação (4 níveis), amplitude de agitação (2 níveis) e posição das latas (4 níveis). Os ensaios de aquecimento e resfriamento foram feitos em tanque com água à temperatura de 98 °C e 17-20 °C, respectivamente. Com os dados de penetração de calor em cada experimento, foram calculados os parâmetros de penetração de calor fh, jh, fc e jc. Os resultados foram modelados utilizando-se grupos de números adimensionais e expressos em termos de Nusselt, Prandtl, Reynolds e funções trigonométricas (com medidas de amplitude e freqüência de agitação, espaço livre e dimensões da embalagem). Foram estabelecidas as duas Equações gerais para as fases de aquecimento e resfriamento: Nu = ReA 0,199.Pr 0,288.sen(xa/AM)0,406.cos(xf/FA) 1,039.cos((xf/FA).(EL/H).p) 4,556 Aquecimento Nu = 0,1295.ReA 0,047.Pr 0,193.sen(xa/AM)0,114.cos(xf/FA) 0,641.cos((xf/FA).(EL/H).p) 2,476 Resfriamento O processo de ALI pode ser aplicado em pasteurizadores ou autoclaves estáticas horizontais e verticais, com modificações simples. Concluiu-se que a ALI aumenta significativamente a taxa de transferência de calor, tanto no aquecimento como no resfriamento.

Estudo e caracterização de matérias-primas para o desenvolvimento de blocos sílico-calcários

The types of products manufactured calcium silicate blocks are very diversified in its characteristics. They include accessory bricks, blocks, products in dense material, with or without reinforcements of hardware, great units in cellular material, and thermal insulating products. The elements calcium silicate are of great use in the prefabricated construction, being formed for dense masses and hardened by autoclaving. This work has for objective develop formulations that make possible the obtaining of calcium silicate blocks with characteristics that correspond the specifications technical, in the State of the Rio Grande of the North, in finality of obtaining technical viability for use in the civil construction. The work studied the availability raw materials from convenient for the production of calcium silicate blocks, and the effect of variations of the productive process on the developed products. The studied raw materials were: the quartz sand from the city of São Gonçalo do Amarante/RN, and two lime, a hydrated lime and a pure lime from the city of Governador Dix-Sept Rosado/RN. The raw materials collected were submitted a testes to particle size distribution, fluorescence of X rays, diffraction of X rays. Then were produced 8 formulations and made body-of-test by uniaxial pressing at 36 MPa, and cured for 7 hours at about 18 kgf/cm2 pressing and temperature of approximately 180 °C. The cure technological properties evaluated were: lineal shrinkage, apparent density, apparent porosity, water absorption, modulus of rupture flexural (3 points), resistance compression, phase analysis (XRD) and micromorphological analysis (SEM). From the results presented the technological properties, was possible say that utilization of hydrated lime becomes more viable its utilization in mass limestone silica, for manufacture of calcium silicate blocks