Cool-Clave: History
Please note this is an old version of this entry, which may differ significantly from the current revision.

Out-of-autoclave (OOA) manufacturing techniques for composites result in lower fibre volume fractions than for fully compressed laminates. The lower fibre volume fraction produces a higher resin volume fraction, which becomes resin-rich volumes (RRV). Textile reinforcements with clustered fibres and consequent RRV generally have low strength but high in-plane process permeability, whereas the opposite is true for uniformly distributed fibres. The inevitable increase in resin volume fraction of OOA composites often compromises composite performance and leads to relatively higher weight and fuel consumption in transport applications. The retention of autoclave processing is recommended for highest performance when compression press moulding is not appropriate (for example, for complex 3D components). The traditional autoclave processing of composites heats not only the component to be cured but also parasitic air and the vessel insulation. Subject to minor modifications of the pressure vessel, electrically heated tooling could be implemented. This approach would need to balance insulation of the heated tool surface (and any heater blanket on the counter-face) against the quenching effect during the introduction of the pressurised cool air. This process optimisation would significantly reduce energy consumption. Additionally, the laminate on the heated tool could be taken to the end of the dwell period before loading the autoclave, leading to significant reductions in cure cycle times. Components could be cured simultaneously at different temperatures provided that there are sufficient power and control circuits in the autoclave. While autoclave processing has usually involved vacuum-bagged pre-impregnated reinforcements, implementation of the cool-clave technique could also provide a scope for using the pressure vessel to cure vacuum-infused composites.

  • autoclave
  • cool-clave
  • vacuum
  • heated tooling

1. Introduction

Composite materials are widely used in industrial applications due to their unique characteristics of high-stiffness-to-weight ratio, excellent durability, chemical resistance, and better recycling potential as compared to metallic components. High performance composites, mainly used in aerospace applications, are produced in the autoclave by applying elevated pressure and temperature [1][2]. However, autoclave processing of composites involves long curing cycle times, expensive tooling, and high energy consumption [3][4]. As a result, there is an interest across the range of composites manufacturing processes for cost reduction with a current focus on out-of-autoclave (OOA) processes [1][5], especially OOA prepreg [6] and resin infusion under flexible tooling [7][8][9]. The OOA process involves manufacturing composites by applying vacuum and heat outside of the autoclave, but has limitations on the maximum laminate fibre volume fraction due to compressibility characteristics of the reinforcement. As a result, composites manufactured by vacuum-only processes cannot achieve high fibre volume contents, which is a primary requirement in high performance composites for aerospace, automobile, and defence sectors. Compression moulding in a hydraulic press creates limited compaction perpendicular to the line of action of the press. The autoclave is the best process for consolidation of complex three-dimensional components, but suffers from several limitations: (a) pre-impregnated (prepreg) reinforcements incur a high-cost premium, (b) high energy input for heating and air circulation: flow speeds in the range 1.4–2.1 m/s [5], (c) non-uniform heating of the components in the vessel due to turbulent flow, windward vs. leeward location, flow stagnation and consequent temperature differences, (d) thermal lag due to the tool or consumables between the heat source and the composite, and (e) long cycle times, which may be a “bottleneck” constraint [10][11].
However, with minor modifications of the pressure vessel, there is potential to improve the efficiency of autoclave processes. The traditional autoclave not only heats the composite parts to be cured but also inert gasses and vessel insulation. Significant energy savings can result from using electrically heated tooling to only heat the essential parts of the process (the tool and composite), and by cool-air pressurisation of composites [12]. Further to the potential for significant reductions in energy consumption, the laminate on the heated tool could be taken to the end of the dwell period before loading the autoclave, leading to significant reductions in cycle times. Autoclave loading efficiency could be improved by curing different composite systems simultaneously with the composites brought to their respective curing temperatures before loading the autoclave, provided there are sufficient power and control circuits in the autoclave, which would further enhance process efficiency [12].

2. Autoclave

Autoclaves have become indispensable equipment to process high-quality polymer composite materials for structural industries, such as aerospace, automotive, and defence sectors [13]. Today, for example, in the aircraft industry, investments in such equipment are strategically important. Autoclaves are now being used to produce very large aircraft components, such as wing and fuselage sections. They can process a wide variety of materials, including thermoset [14] and thermoplastic [15]-based composite parts with varying contours and complex shapes.
The quality requirements of the present high-performance composites for aerospace/defence industries are indeed more stringent. Additionally, there is an urgent requirement to improve the efficiency and cost-effectiveness of high-performance structural composites, along with ensuring reliable and consistent processing methods. Therefore, it is imperative for autoclave design engineers to take into consideration different governing criteria to address the diverse and complex requirements for developing state-of-the-art autoclave systems. In addition to handling a wide variety of consumables, modern autoclaves must respect health and safety requirements [16] and ensure minimum maintenance costs.
Autoclaves are closed pressure vessels used to manufacture high performance composite components. Uncured composites are moulded in an autoclave typically heated using inert gases, such as carbon dioxide or nitrogen, thus allowing the transfer of heat and pressure to the composite component for consolidation and allowing it to cure firmly and uniformly. The application of pressure for consolidation of composites in an autoclave helps in reducing porosity and voids, retains shape around the mould, and enables better control to maintain a higher fibre volume fraction in composite components [17]. The autoclave process draws many similarities with hot pressing technique; however, the main difference pertains to the way heat and pressure are applied [18]. The autoclave operating parameters, such as temperature and pressure are based on the resin systems used. Generally, epoxy resins require temperatures < 200 °C and pressures of 0.7 MPa [17].
Figure 1 shows the internal chamber of the Aeroform autoclave located in the composites manufacturing laboratory at the University of Plymouth. Surrounding the main internal area is a metal inner case which shields the components being cured from twelve electric heating elements positioned at intervals around the chamber’s circumference. Behind the heating elements is a layer of thermal insulation, protected by sheet metal. As the autoclave walls are made up of quality carbon steel, up to 150 mm on some autoclaves [17][18], they act as a heat sink. The insulation is designed to minimise heat transfer from the main chamber to the autoclave walls. The insulation commonly used consists of refractory ceramics or fibreglass insulation. The insulation prevents excess energy loss and is designed to keep the autoclave outer walls down to a maximum temperature of 60 °C.
Figure 1. Internal chamber of 0.67 m working diameter Aeroform autoclave at the University of Plymouth.
The design of autoclave systems is multidisciplinary in nature and encompasses mechanical, process control, and instrumentation engineering. Invariably, the state-of-the-art autoclave systems are completely computer-controlled and are semi- or fully automated. The computer controls of these modern autoclaves are required to execute the selected cure cycle by sequentially starting various subsystems, download set values at regular time intervals to the front-end controllers, acquire, store, and archive the data, monitor cure status and faults, generate alarms, and perform the functions of sequential shut down and reporting [19]. Ease of maintenance, fail-safe operation, and reliability are among the key drivers in modern autoclaves. The low cost of ownership also needs to be considered in today’s context [17]. In recent years, there has been an increasing demand to enhance the service temperature of high performance structural composite components, invariably leading to higher curing temperature and pressure requirements in the order of 300 to 350 °C and up to 1.5 MPa. This necessitates the development of high temperature and high-pressure autoclave systems, which presents a new set of challenges such as the handling of massive door and locking systems, temperature uniformity, special material requirements for door and shell flanges, fabrication, transportation, and, most importantly, low cost and maintenance requirements [17][19].

3. Cool-Clave Technique

Autoclave processing is used to manufacture high performance composites, but overall, the process is very expensive and requires high energy consumption. In a traditional autoclave, the process not only heats up the composite to be consolidated but also any parasitic air and vessel insulation requiring high energy usage. Additionally, autoclave processing is normally used to consolidate vacuum-bagged pre-impregnated reinforcements. Prepreg materials require freezer storage, and the separate impregnation stage incurs further costs. The cool-clave technique has the potential to achieve autoclave consolidation of fibre-reinforced composites by enhancing the energy- and cost-efficiency: (a) without heating parasitic materials (hence saving energy), (b) with shorter cycle times (hence increased production rate), (c) without prepreg, i.e., using infused laminates (for lower cost). A schematic of the cool-clave technique with the bagging process is illustrated in Figure 2.
Figure 2. Schematic of cool-clave processing technique.
Implementation of the cool-clave technique for autoclave consolidation of composites could generate significant cost and energy savings. The equipment required for the cool-clave process consists of:
  • pressure vessel (autoclave)
  • heated mould tool and control unit
  • efficient thermal insulation of the bagged component
Prudham and Summerscales [20] investigated the cool-clave processing technique using the autoclave at the University of Plymouth. The autoclave was used as a pressure vessel, without using the heating aspect of the system. The heat, required for curing, was provided by a mould tool with built-in heating elements.
For implementation of the cool-clave processing technique, temperature uniformity across the face of the mould tool is crucial [18]. During the initial stages of the cure cycle, dwell periods are often used, where the laminate is held at a temperature lower than the curing temperature for a set period of time. This increase in temperature lowers the viscosity of the resin, allowing it to flow. Together with low pressure, the volatiles trapped within the laminate are forced out, thus reducing voids. If the viscosity of the resin is too high it will not flow, trapping the volatiles within the laminate, or if too low, then the resin will flow too much, creating areas of resin starvation. It is important that the temperature across the face of the mould tool remains relatively uniform to maintain uniform viscosity of the resin. Therefore, Prudham [18] performed thermal imaging of the mould tool to gain insight into the temperature uniformity across the mould tool surface.
The results indicated discrepancy between temperatures recorded by the mould tools built-in thermocouple and the temperatures recorded during thermal imaging technique. A greater heat loss near to the edges of the mould tool was recorded by thermal imaging with a maximum temperature difference across the main region of the mould tool being in the range from 5 °C horizontally and 7 °C vertically [18] in the image.
From the thermal imaging results, it was concluded that the mould tool would be suitable for cool-clave processing, demonstrating a convective heat transfer across the surface [18]. Greater heat loss across the edges of the mould tool surface was explained by in-plane anisotropic thermal conductivity of carbon fibre-reinforced epoxy composite used in the study [18][21]. The tests highlighted the need for adequate insulation of the mould tool during the manufacturing stage to prevent greater heat losses as recorded during thermal imaging [18].
A Thermal Insulation Hud (TIH) was constructed to prevent any convective heat loss from the mould tool which would encase the mould tool, allowing vacuum and thermocouple connections but limiting convective heat transfer [18]. One of the main challenges of the cool-clave technique was how to get power to the heated mould tool inside the autoclave. The electrical supply used to power the heated mould tool was provided by a power transformer controlled by an ‘IMO’ PID controller by using a pre-existing access hole on the autoclave chamber, plugged together with a specially made fitting encompassing the electrical wires providing the pressure tight seal required [18].

This entry is adapted from the peer-reviewed paper 10.3390/jcs7020082


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