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Autoclave Molding
by Joana Peralta

Autoclave molding is a thermochemical processing procedure [1], where controlled pressure and temperature can be applied [2] to a prepreg or fabric laminate to obtain additional consolidation and cure thermoset matrices. Therefore, previous to autoclave curing other procedures are required [3].

1.1 Background
The need of autoclaves for composite production is due to the high quality requirements of composite materials for very demanding industries as aerospace. The autoclave curing provides uniform consolidation of prepreg laminates, with very low amount of voids, e.g. 0.1% [4]. During autoclave curing the heat appliance also finishes cure the resin [5]. Autoclave curing is preferentially used in prepreg thermosets preimpregnated, but it can also be used in thermoplastic resins, e.g., polysulfone and polypropylene [6], with slight differences in the process, as indicated in Table 1.1.
TABLE 1.1 Cycle times in autoclave molding [6]

Step Cutting Layup Flat panel Complex shape Debulking Bagging Autoclave cycling
N/A = not applicable

Thermoplastica prepreg 165 cm/min 0.91 kg/h 0.45 kg/h N/A 1.875 h 5h

Thermosetb prepreg 165 cm/min 0.45 kg/h 0.91 kg/h 20 -30 min 1.25 h 10 h

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a

Carbon fiber/PEEK, typical processing temperature 370 C Carbon fiber/epoxy, typical processing temperature 177 C Source: adapted from ref. [7]
b

Commonly autoclaves are used to consolidate prepregs in the B-time form (not completely cured).

1.2 Autoclaves constitution

An autoclave consists of a vessel that can be heated and pressurized internally.

FIGURE 1.1 Schematics of a typical autoclave vessel operation [5]

Autoclaves dimensions vary significantly from small bench-top laboratory units to the very large equipment (Figure 1.2) used to cure airplane parts [4], e.g. = 4 m, and l = 18 m. The pressure inside the autoclave is mostly achieved by pressurizing air and/or nonflammable gases, such as nitrogen and carbon dioxide. The heat is applied using gas, steam or electricity [6].Additionally there is vacuum applied in the vacuum bag; this vacuum is produced by a pump that is connected to the vacuum bag [8].

Autoclave Molding

FIGURE 1.2 Large autoclave used in the production of a composite skin for the tail-section of a Boeing 777 aircraft (Copyright The Boeing Company) [9]

1.3 Production phases

The overall processing steps using autoclave molding are [8]: Placement of the prepregs at room temperature for thawing; Cutting of the laminate from the bulk prepregs; Cleaning and coating of the mold surface with a release agent; Laying of the prepregs in the mold surface in the required sequence; Removal of the entrapped air between prepreg sheets; Vacuum bag assemblage; Placement of the assembly in the autoclave; Connection of the vacuum bag to the pump and vacuum controllers; Cure cycle in the autoclave; After the cure cycle the vacuum bag is removed and the parts are inspected, trimmed and drilled if required.

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FIGURE 1.3 Vacuum bag schematic for typical composite bagging sequence [10]

While placing the several sets of prepregs, it may be necessary to remove the voids and compress the prepregs to reduce the volume. This can be made using a rod, or more efficiently by applying vacuum to compress the plies together debulking. This procedures also withdraws the excess volatile components, such as residual solvent, low molecular weight resin components, absorbed moisture, or entrapped air [11, 12]. The debulking is done several times during lay-up, the final assembly is then placed in the vacuum bag that will be placed in the autoclave.

FIGURE 1.4 Two different conformations for vacuum bagging [5]

According to the part that is being produced, several different configurations of the vacuum bag assembly are allowed (Figure 1.4). Usually one of the faces is constitute by the mold, but sometimes, especially in long thin parts, a bag involving the part and the mold are used. 1.3.1 Tooling The molds (or tools) are usually single parts. The tools are frequently manufactured from carbon fiber composite because of the properties such as [8]: Dimensional stability; Good surface finish; Durability; High thermal conductivity. The tools can also be made from plaster, metals (zinc, aluminum, steel) and even concrete [8]. The choice of tooling depends on [6]: Complexity of the part; Part volume; Part quality;

Autoclave Molding Surface finish.

FIGURE 1.5 Stages os the consolidation process during autoclave curing [5]

During autoclave curing there is desorption of vapors and gases from fibers and filers, and the pores and cracks are filled with binder (resin). The consolidation process during autoclave curing (Figure 1.5) implies that, since the pressure is applied from the outside, the outside plies are the first to be consolidated. This phenomenon results in additional difficulty in the resin bleeding towards the exterior. Therefore the resin must pass the layers above to be eliminated.

FIGURE 1.6 Typical composite curing autoclave schematic [13]

During the autoclave curing of composites several physical and chemical phenomena occurs, such as, the curing of the thermoset resin, resin

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flow and heat transfer [14, 15]. Additionally parameters such as the temperature, pressure and vacuum inside the vacuum bag are controlled (Figure 1.7).

FIGURE 1.7 Typical cure cycle for a carbon/epoxy prepreg [16]

In the autoclave curing cycle, the first step is to apply the vacuum to the vacuum bag, followed by the temperature raising to a value (dwell temperature) that allow the resin to flow, typical heating rates are between 2 and 4 C/min. The dwelling temperature is maintained for about one hour, and then the pressure is applies with a new raise in the temperature to cure the thermoset resin [8]. After the required curing time the vacuum inside the bag is removed, and the heat is shut, allowing the autoclave to cool. The application of pressure inside the autoclave is interrupted when the temperature is about 100 C. 1.3.2 Control of the autoclave process In autoclave processes many hazards can occur. During the autoclave curing the process controlled can fail and bleeding from the vacuum bag can happen. These problems conduce to the discard of the part, and are easy to detect. However, most commonly, defects such excess voids, rich resin and delamination happen and are very difficult to detect [17]. Therefore a very accurate control of all the process is required. In Figure 1.9 are presented two systems for autoclave curing.

Autoclave Molding

FIGURE 1.8 Autoclave control systems for autoclave curing [5]

The main advantages of autoclave molding are [6]: Uniform distribution of pressure over the mold surface regardless to its complexity[1]; Inexpensive mold materials compared to the overall production costs Pre-molded composite and metallic inserts can be easily incorporated The materials can be cut and stacked minimizing scrap loss Extremely large parts can be produced in one layup and one operation Many small parts can also be cured in the same curing cycle The drawbacks of autoclave molding process are [6]: Cost of the overall process; Labor intensive; Slow process; Only one side is molded; Possible leaking in the vacuum bags during the curing cycle; Finishing as trimming and drilling is usually required. The applications of the materials produced with autoclave molding are: Aerospace industry; Sailing industry; Formula one; Air cashers for energy production;

Polymer and Composites Processing Civil engineering [18, 19]; Others.

Presently efforts are being done in order to develop out-of-autoclave processes and prepreg materials, to reduce the costs and space issues associated with the use of large autoclaves [4].

References
1. A.G. Bratukhin; V.S. Bogolyubov; G.M. Gunyaev; V.I. Mishin; V.A. Sadkov and O.S. Sirotkin. Main tecchnological aspectes of the manufacture of composite parts and assembly. [ed.] A.G. Bratukhin and V.S. Bogolyubov. Composite manufacturing technology. London : Chapman & Hall, 1995. pp. 128. 2. A.K. Kulshreshtha. An overview of composite fabrication, design and cost. [ed.] A.K. Kulshreshtha and C. Vasile. Handbook of polymer blends and composites. Exeter : Rapra atechnology Ltd., 2002. pp. 5-52. Vol. 2. 3. A. Mortensen. Concise encyclopedia of composite materials. 2nd. New York : Elsevier, 2007. pp. 651-658. 4. R.F. Gibson. Principles of composite material mechanics. 3rd. Boca Raton : CRC Press, 2011. pp. 29-33. 5. M.G. Bader and C. Lekakou. Processing for laminated structures. [ed.] P.K. Mallick. Composites engineering handbook. New York : CRC Press, 1997. pp. 371-480. 6. A.A. Watts. Commercial opportunities for advanced composites. 2nd. Baltimore : ASTM STP704, 1985. pp. 33-43. 7. L. Wang and T.G. Gutowski. Cost comparison between thermoplastic. SAMPE Journal, 1990. pp. 19-26. Vol. 26/jno.6. 8. S.K. Mazumdar. Composites manufacturing: materials, product, and process engineering. Boca Raton : CRC Press, 2002. 9. M.E. Tuttle. Structural analysis of polymeric composite materials. New York : CRC Press, 2004. pp. 29-38. 10. A.R. Mallow and F.C. Campbell. Autoclave processing. [ed.] R.S. Dav and A.C. Loos. Processing of composites. Munich : Hanser Verlag, 2000. pp. 296316. 11. A.K. Kulshreshtha. An overview of composite fabrication, design and cost. [ed.] A.K. Kulshreshtha and C. Vasile. Handbook of polymer blends and composites. Exeter : Rapra atechnology Ltd., 2002. pp. 5-52. Vol. 2. 12. A.R. Mallow and F.C. Campbell. Autoclave processing. [ed.] R.S. Dav and A.C. Loos. Processing of composites. Munich : Hanser Verlag, 2000. pp. 296316.

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13. F.C. Campbell. Manufacturing processes for advanced composites. Oxford : Elsevier, 204. 14. K.K. Chawla. Composite materials science and engineering. 2nd. New York : Springer Science+Business Media, Inc., 1998. pp. 133-163. 15. V. Antonucci; M. Giordano; S. Inserra and L. Nicalais. A new methodology for the active control of the heat transfer in autoclave technology. [ed.] S. Pierucci. European symposium computer aided process engineering-10. Oxford : Elsevier Science B.V., 2000. pp. 295-300. 10. D.F. Adams; L.A. Carlson and R.B. Pipes. Experimental characterization of advanced composite materials. Boca Raton: CRC Press, 2003. 17. X. Wang; F. Xie; M. Lee and Z. Zhang. Influence of tool assembly schemes and integral molding technologies on compaction of T-stiffened skins in autoclave process. Los Angeles: Journal of Reinforced Plastics and Composites, 2010. pp. 1311-1322. Vol. 29/no.9. 18 B. Kawahara, H. Estrada and L.S. Lee. Life-cycle cost comparison for steel reinforced concrete and fiber reinforced polymer bridge decks. [ed.] R. Jain and L. Lee. Fiber reiforced polymer (FRP) composites for infrastructure applications. London : Springer Science+Business Media B.V., 2012. pp. 237273. 19. L.C. Hollaway and P.R. Head. Advanced Polymer Composites and Polymers in the Civil Infrastructure. Oxford: Elsevier Science Ltd., 2001. pp. 37-87.