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PII: S1359-835X(98)00055-4
A comparison of physical properties of glass bre epoxy composites produced by wet lay-up with autoclave consolidation and resin transfer moulding
Comparisons are reported for composite samples of similar resin and bre systems which were processed using the wet lay-up with autoclave consolidation and resin transfer moulding (RTM) by vacuum impregnation. Similar degrees of cure were obtained for laminates using the two methods of processing and the arising thermal and physical properties (tensile, exural, interlaminar shear strength (ILSS), void content and thickness variation) were measured. The bre dominated properties (i.e. exural and tensile strength) were found to be higher for the autoclaved samples due to the higher volume fraction arising from the superior compaction pressure, although when normalised on the basis of bre volume fraction the results were similar. The matrix dominated ILSS values were higher for the RTM samples and this was attributed to improved wetting, reduced void content and a slightly lower degree of cure. Thermal analysis also indicated that the autoclaved (60% glass bre by volume) composite attained a slightly higher glass transition temperature than that achieved by RTM (50% bre by volume) for similar cure times and cure temperatures. The signicance of the results in an industrial context is discussed. 1998 Elsevier Science Ltd. All rights reserved
(Keywords: composites manufacture; E. resin transfer moulding (RTM); E. autoclave)
INTRODUCTION Aerospace composites manufacturing The aerospace sector remains rmly rooted in traditional autoclaving routes for processing the majority of their composite parts. Autoclaving is a well understood and mature technology which is capable of producing material of consistently high quality, with high (greater than 55%) bre volume fraction and low (less than 2%) void content. Numerous studies of autoclaving have been published, although most of these relate to pre-preg. Stringer1 investigated autoclave consolidation for wet layup carbon/epoxy laminates and reported a bre volume of 58% and less than 2% voidage by incorporating a dwell period at the start of the cure cycle before applying the consolidation pressure. Wenger2 has investigated autoclave cure cycle optimisation for the facility used in this investigation, varying the point of pressure application, dwell temperature, dwell period and heat-up ramp, and studying the quality of the nal composite component.
Aerospace resin transfer moulding Despite the traditional use of the autoclave (almost universally with pre-preg.), interest and condence is increasing for resin transfer moulding (RTM), usually driven by materials costs. This has led to the production of aircraft components such as radomes3, bullet fairings4, and propeller blades5. Previous development studies for structural components by aerospace operators includes missile airframes6 and a highly loaded crank7. With the development of automated methods of preform production8,9, parallel research on processing methods is aimed at fast and reliable methods of impregnation with reduced capital and running costs compared to either traditional wet lay-up or vacuum bag and autoclave (pre-preg.) moulding. RTM offers a useful alternative in several industrial sectors, since it reduces the labour costs and environmental concerns associated with wet lay-up and provides substantial savings in materials costs when compared with the use of pre-pregs. A further advantage of RTM is the wide range of process variants, which range from relatively simple vacuum impregnation processes requiring little by way of capital
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the degree of visual porosity and moulding translucency. Qualitative comparison showed that vacuum impregnation and peripheral gating produced the best quality mouldings. Clearly, the properties of vacuum impregnated mouldings are also strongly dependent upon the bre volume fraction which is achieved. Unlike conventional RTM, which is carried out in a xed height cavity, the use of a exible membrane to close the cavity means that the degree of fabric compaction (thus the bre volume fraction) depends upon the pressure difference across the membrane15. Autoclaving versus RTM from a manufacturing perspective Table 1 summarises the main features that characterise autoclaving and RTM. It is evident that autoclaving is the favoured method when the need for high product quality dominates over production rate (as evidenced by its continued dominance of aerospace manufacture), while RTM appears to offer lower cost manufacture and entry to higher volume markets, typied by the growing interest from within the automotive sector. In addition to the savings on materials costs compared with pre-pregs and the improvements in the working environment compared with wet lay-up, RTM offers considerable advantages over either alternative, due to a reduction in the labour content and higher production rates. Operator exposure to liquid resins is also much reduced. An approximate time analysis for the two (laboratory) processes is shown in Table 2, which suggests that RTM offers a signicant time saving of 1.5 h (25%) over the equivalent
Autoclave Low (10 1 10 2/annum) Low ( 2%) High High (5070%) Aerospace industry, Formula 1 automotive, sporting goods
Table 2 Comparison of Wet lay-up with autoclave consolidation and RTM: breakdown by operations for laboratory scale processes Wet lay-up and autoclave Production step Mould preparation H Fabric cutting H (including preparation) Resin mixing H I (including preparation) Hand lay-up H I Vacuum bagging H Autoclave cycle Autoclave debagging H Total processing time Resin post-curing at 145 C Total production time Manual processing time (% of total production time) Direct Contact with resin (% of total production time)
a b
RTM Time (min) 22.5 a 25 25 120 b 30 192 10 424.5 452 876.5 232.5 (26.5%) 145 (16.5%) Production step Mould preparation H Fabric cutting H (including preparation) Resin mixing H I (including preparation) Resin degassing Tool assembly testing H Resin injection H Resin curing Tool cooling Tool ejection and preparation for next run H Total processing time Resin post-curing at 145 C Total production time Manual processing time (% of total production time) Direct contact with resin (% of total production time) Time (min) 22.5 a 25 25 60 30 12 99 30 30 333.5 368.4 701.9 144.5 (20.6%) 25 (3.6%)
Autoclave and RTM mould preparation takes 90 min, but the preparation will endure a minimum of four production runs. Autoclave hand lay-up takes two operators working for 60 min. H, these steps involve manual processing. I, these steps involve direct operator contact with the resin.
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Figure 1
(a) i, RTM temperature cycle; ii, RTM pressure cycle. (b) i, Autoclave temperature cycle; ii, Autoclave pressure cycle
The temperature was ramped at 4 C/min to 50 C, and then held at this temperature for 1 h before being further ramped at 3 C/min to 100 C, where it was held for 1.5 h before being nally ramped down at 4 C/min to 40 C. As well as there being a vacuum applied to the mould cavity, the autoclave pressure was raised to 12 bar (gauge). After the thermal cycle, the tool was removed from the autoclave and the at plaque demoulded before subsequent post-cure at 145 C for 452 min. Preparation and analysis The plaques were sectioned using a diamond wheel. Specimens were then polished to the required dimensions using 320 grit wet and dry paper. A grid size of 10 mm was drawn on the plaques to map thickness variation and the thickness was measured at the line intersections using a
micrometer tted with barrels of 6.8 mm in diameter. The Composite Research Advisory Group (CRAG) standards for tensile, exural and ILSS methods 302, 200 and 100 respectively were used19. The DMA method required a 60 mm 10 mm sample which was a exure bar cut from the composite plaques, whereas the DSC technique only required a 10 mg sample weight. Void content was calculated by comparing the composite density calculated by resin burn off (to ASTM D2584-94) and the value calculated by the liquid displacement method. The latter used a Sartorius Density Determination Kit (Model Number YDK 01-OD) coupled to a Sartorius MC1 series balance (Model Number RC 210 D). Prior to the tests, the samples were conditioned in a humidity chamber at 23 C and 50% relative humidity for 40 h. Five samples were taken from along a length of the mouldings, in order to give a representative void content.
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Figure 2
RESULTS The properties of the RTM and wet-layup/autoclave plaques are compared in Table 3. The results (Table 3b) show that autoclave moulding achieved an extra 13.5% bre volume fraction due to the superior compaction pressure of 13 bar. This produced increases in exural and tensile strength and modulus. However, it is worth noting that the RTM plaque was compacted and impregnated at a bre volume fraction of 50% using only the pressure difference caused by evacuating the mould cavity. It is also interesting that the ILSS arising from the RTM technique was 70% higher than that from the autoclave method. Since ILSS is generally accepted to be a good indicator of matrix quality and void content, this suggests that RTM more than adequately matches the autoclave process in terms of matrix quality. However the slightly lower degree of cure of the RTM sample (Table 3c) is also likely to be a contributing factor here. In order to determine the inuence of the processing method on the other mechanical properties, two approaches were considered. The rst was to normalise the properties on the basis of the volume fraction of bre. The nominal
Table 3 Laminate properties arising from wet lay-up with autoclave consolidation and RTM Property (a) Mechanical Properties ILSS (MPa) Flexural strength (MPa) Flexural modulus (GPa) Tensile strength (MPa) Tensile modulus (GPa) Calculated theoretical tensile strength (MPa) Calculated theoretical tensile modulus (GPa) (b) Physical properties Calculated V f from mean thickness (%) Mean thickness (mm) Voidage (%) (c) Thermal properties T g (DMA) T g (DSC) RTM Autoclave RTM% difference 2.4), normalised 16.35 5.3), normalised 893.8 5.6), normalised 41.36 6.6), normalised 521.0 10.5), normalised 25.60 69.7% 27.2% 25.7% 17.7% 15.0% 17.4% 19.3% 21.1% 27.3% 3.8% 6.8% 4.7%
17.73 (%CV 4.9), normalised 415.7 (%CV 3.8), normalised 19.63 (%CV 3.2), normalised 274.0 (%CV 8.2), normalised 13.91 (%CV 7.9), normalised 348.3 19.87 50.4 1.775 (%CV 4.3) 1.507 (%CV 13.4) 145.0 (%CV 0.4) 142.9 (%CV 2.1)
10.45 (%CV 571.2 (%CV 26.43 (%CV 332.9 (%CV 16.36 (%CV 421.6 24.61
63.9 1.394 (%CV 2.1) 1.566 (%CV 14.1) 155.6 (%CV 0.6) 149.9 (%CV 2.2)
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entire length of the bre; that the bres and matrix were perfectly bonded; that all bres broke simultaneously after application of the tensile load; and that there were no variations in constituent properties or bre volume fraction. In practice, crimp and misalignment of the yarns during handling means that some departures from the ideal architecture are inevitable. Consequently, the properties will be reduced compared to the estimated values. The use of a plain weave, which maximises crimp, magnies these effects. Also, prior to separation, damage mechanisms such as disbonding and delamination mean that the tensile load will no longer be shared by the two phases in the simple way assumed by the ROM. In addition, manufacturing induced defects such as bre breakage, matrix cracking and voidage all contribute to reductions in measured strength and modulus. Micrographs taken from representative areas of each laminate type are shown in Figure 3. The effects of the higher autoclave pressure are immediately apparent from the high degree of compaction which is evident in both the 90 bre bundles which are visible and in the lenticular 0 tows running out of the section. Also, there are fewer visible resin rich areas in the autoclaved sample, which is again attributed to the higher pressure which caused nesting of the plies and compaction of the tows. These two effects are consistent with the higher bre volume fraction of the autoclaved sample. It is also interesting to note that neither micrograph displays any signicant voidage, which conrms the quantitative results produced by the density measurements at approximately 1.5% in both cases. The results suggest generally that the only inferiority in the vacuum impregnation technique, compared to the wet lay-up and autoclave alternative for glass bre/epoxy, arises from the lower bre fraction which was achieved. Clearly, the bre fraction could be raised (for vacuum impregnation) by introducing a secondary consolidation process, although it remains to be seen if such laminates can be lled satisfactorily using the low pressure gradient which is available from vacuum impregnation if the entire compaction process is carried out beforehand. If this is not the case, then a shift to conventional, pressure-driven RTM process is indicated. Mould stiffness is critical in such processes to control the bre volume fraction and minimise the part thickness variation. However, tooling costs are required to be minimised to reduce the part cost and increase the exibility in production volumes. In this study, a exible upper tool was used. Atmospheric pressure was used to compact and impregnate the fabric reinforcement. Comparison of the thickness distribution compared with that for an autoclave consolidated plaque (Table 3b) shows that the coefcient of variation (CV) for the RTM plaque was twice that from the autoclave. It seems reasonable to expect corresponding variations in the bre volume fraction
and mechanical properties within the plaque (particularly in intensive properties such as the strength values). However, no signicant difference in the variability of properties is evident from Table 3. DMA and DSC were used to determine the T g of both composites. DMA is often reported18 to give T g results that are 10 C higher than those given by DSC. Five tests on each moulding were completed for both methods and the mean values are listed in Table 3c. The results from both techniques suggest that the T g of the RTM composite is slightly lower than that from the autoclave with the DMA results, suggesting a greater difference between the two processes. This difference arises not from any inherent differences in the processing methods, but rather in the different cure schedules which were used. The results indicate that the RTM post-cure cycle was inadequate. This was attributed to the reliance on data from simulated thermal cycles using a dielectric analyser (DEA) to determine the post-cure requirements. The latter were conducted using similar bre volume fractions, whereas the different consolidation pressures during the two processes produced different volume fractions. Clearly, this factor will
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CONCLUSIONS
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RTM, based upon vacuum impregnation, offers materials and labour cost savings compared with conventional autoclaving, operational and health and safety benets compared to wet laminating and reductions in tooling costs compared to normal (positive pressure driven) RTM. This study has shown that laminate quality from vacuum impregnation is comparable with autoclave consolidation when the same materials are used. However, the bre fractions available from vacuum impregnation are somewhat lower due to the lower consolidation pressure and this inuences the mechanical and thermal properties of the laminate. A secondary consolidation process would overcome this problem.
ACKNOWLEDGEMENTS The authors would like to thank CS-Interglas for supplying the glass bre and also David Hurry of Ciba Polymers for supplying the epoxy resin. Also, thanks are due to Roy Carton and Maurice Jamieson for their assistance in processing and testing the samples respectively. Financial support from the European Regional Development Fund (ERDF) and the Technology Development Programme (TDP) is also gratefully acknowledged.
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