Abstract
The paper presents a comparison of the test results for the fiber volume fraction, static bending and Charpy impact strength of glass fiber reinforced polymer laminates reinforced by 0/90 fabric and chopped strand mat, produced by the hand lay-up and the vacuum-assisted resin infusion (VARI) method. The laminates were produced under equivalent conditions, with polyester matrix and lay-up areal mass 2100 g/m2. In the comparison of the obtained measurement results, similar mechanical performance was stated in the case of the hand lay-up and the VARI production. However, significantly smaller scatter of results and better uniformity of the reinforcement in the matrix with smaller amount of local structure defects was observed for the samples obtained by VARI method. The laminates obtained by VARI method show a much more advantageous coefficient of variation than that of the hand lay-up method, especially in the case of the mat reinforcement.
Introduction
Vacuum-assisted resin infusion (VARI) is currently one of the primary techniques in the manufacture of fiber reinforced polymer (FRP) composite products. It enables the production of big elements of a complicated shape, such as energetic windmill blades or yacht hulls.1–3 In comparison to the classic technology – hand lay-up – VARI makes it possible to shorten the average process time, to improve the health and safety conditions in the process surroundings and to reduce the negative impact of the process on the environment.1,2 The authors’ previous experience, also gained in the industry sector, showed that the quality of the laminates properly manufactured by the VARI and the hand lay-up methods is comparable. However, in the case of the hand manufacture, there is a very significant discrepancy in repeatability. This characteristic, resulting from the elimination of the human factor from the proper saturation process, is the main trump card of pressure technologies, 4 including the VARI method. It should be noted that, as regards the product properties, the VARI technique is comparable with the resin transfer molding (RTM) methods,5,6 and both methods are complimentary; there is a range of products impossible to be manufactured by RTM. Pressure technologies are necessary in the manufacture of products with advanced types of reinforcements, especially of the 3D type.7–9 It was also stated that the VARI method is, by all means, the best solution for the natural fiber reinforcements.10–13 VARI is also one of the alternatives in the production of innovative experimental constructions, such as: composite flexible structures, 14 innovative building elevations, 15 and braided pipelines. 16 Another advantage of a fundamental importance is the possibility of running the process without (or with minimal) emission of solvent vapours, which makes it possible to fulfill all the announced implementations of the Industrial Safety Standard, as well as those of the environment protection.
One of the disadvantages of pressure technologies (especially VARI) is the necessity of designing the processes before their run. This requires applying numerical methods, characterized by a high degree of complication, especially at the pre-calculation level. Analyzing the fibrous structures, both for the purposes of mechanical property design4,17,18 and the analysis of the resin flow in the preform,4,19–22 is very complex in regard to the calculation apparatus23,24 and requires entering numerous experimental data of the charge. 19 Also problematic is the provision of the optimal time of resin cure; the resin has to fill the required area of the preform, which requires the least possible viscosity, and next – to harden as fast as possible. 21 In order to “steer” the properties of the resin, various modifications are applied: ion crosslinking, 25 the addition of: nanotubes,26,27 silica,28,29 halloysite, 30 nanoclay, 31 and the introduction of biodegradable components. 32 The problem of process designing and the difficulties in acquiring a good repeatability also concerns metal matrix composites,33–36 especially the technology applying ceramic framed reinforcements and continuous fibers.37–39 In the manufacture of very small products and those of small sizes, the VARI technique is not the best solution, as it is connected with significant investments. However, it is indispensible in the case of bigger series, especially of products with a large surface area, such as yacht hulls. With the correctly designed process, the saturation of the hull of a 30-meter unit takes 40 min.1,2,40 Even including the preparation time, this result is impossible to achieve by means of other methods.
The study presents a simple comparative analysis of laminated boards made by the hand lay-up and the VARI method. The standard percentage deviation of the measurement series results was assumed as the repeatability criterion: of the fiber volume fraction, of the flexural strength and of the Charpy impact strength. Two reinforcement-type laminates were produced and compared: plain weave fabric and chopped strand mat.
Materials and methods
Fibrous preforms made of two different structures: chopped strand mat and plain weave fabric, were impregnated with polyester resin, alternatively by hand lay-up and vacuum-assisted resin infusion (VARI). Fourteen layers of the chopped strand mat (150 g/m2, vinylsilane finish, emulsion binding agent) by KROSGLASS, Poland, were applied for the first type of preform. Alternatively, 6 layers of the plain weave fabric (350 g/m2, vinylsilane finish) by KROSGLASS, Poland, were applied for the second one. ESTROMAL 14 terephthalate polyester resin by ERG PUSTKOW, Poland, was applied as the matrix of the composites. LUPEROX (solution of methylethylketone peroxide in dibutyl phthalate) was used as the catalyst in the amount of 1.5 wt%.
The hand lay-up procedure was implemented with the use of a brush and a roller. The board laminating process was conducted by a person with a significant experience in the use of this method – he has produced about 1000 laminate panels in laboratory conditions, by about 10 years. The amount of the applied resin guaranteed a good saturation of the layers, and its excess was removed by means of the roller, with the avoidance of applying too strong pressure (local “squeeze-out”). The impregnation with the roller was performed for each layer in the “K1” and “K2” direction (Figure 1). After impregnation of the last layer, the laminates remained under ambient conditions (temperature 22℃, humidity 50%) for 20 h. Next, the cured panel was hardened at the temperature of 50℃ for 4 h and left again at room temperature for 20 h.
Scheme of the VARI process stand.
The VARI processes were conducted on the stand whose scheme is presented in Figure 1. The stand consisted of a flat rigid board-form, a partial vacuum resin transport system and an air-tight elastic shell (foil), which enclosed the working area.
A vacuum system with a TEPRO pump, Poland, power of 1100 W, was applied. The obtained pressure gradient equaled about 0.69 bar in the case of all the conducted processes. The inner diameter of the supplying tubes and the spiral tubes which formed the “resin inlet edge” and the “vent edge”, equaled 10 mm. Just before the preform was filled with the resin (when previously determined amount of the resin was used), the resin inlet was closed. It made possible to distribute the resin excess from the area of the inlet edge. The saturated preform remained under vacuum till its hardening was stated. After the vacuum’s disconnection, the pre-hardened preform was left under foil. The hardening process was conducted in the same way as in the case of the hand lay-up laminates.
All – the hand and the infusion – laminated panels were made during one day, in order to provide repeatability of the ambient conditions. In the case of both types of reinforcement, two panels were prepared for both applied technologies (a total of 8 panels).
The distribution of the samples on the panels (Figure 2) was mainly aimed at a “statistical” elimination of the effect of the resin flow direction on the properties of the infusion laminates.
Scheme of the sample distribution in the produced laminated panels on the example of a hand lay-up laminate with a plain weave fabric base.
Number of specimens from all laminate types for individual experiments.
VARI: vacuum-assisted resin infusion.
The gravimetric method was used to determine the fiber volume fraction in the manufactured laminates. The measurements were conducted on the fabric (and mat) sheets which were simultaneously used for the manufacturing. They were cut from a central area of the beam (Figure 3).
Schema of sheets-cutting area within the fabric (mat) beam.
Areal mass of the preforms and cured laminates used for determination of fiber volume fraction.
VARI: vacuum-assisted resin infusion.
Flexural strength of laminates produced by hand lay-up and VARI.
VARI: vacuum-assisted resin infusion.
The fiber volume fraction for individual specimens is presented in Figure 3.
If high accuracy of measurement tasks is kept, gravimetric method will ensure a precise determination of fiber volume fraction in the laminate. Occurrence of significant mistake caused by a local disturbance in areal mass is unlike, because of relatively low area of the preforms (stacks). It was assumed that the fluctuations of the volume fraction within the cured panels are the effect of – more or less uniform – saturation with the resin, which is largely related with the manufacturing technology.
The static three-point bending tests were performed according to the PN-EN-ISO 14125/2001 Standard. A constant ratio of support spacing–specimen thickness was established at L/h = 24. The deformation rate was selected according to the formula given in the Standard, depending on the sample thickness, with the accuracy of 0.5 mm/min.
The Charpy impact strength tests were conducted according to the PN-EN-ISO 179-1/2006 Standard. A constant ratio of support spacing-sample thickness was established at L/h = 17. The sample lengths were at a much approximated level within particular populations, and so they were not corrected. A pendulum of the striking energy of 15 J and the maximum speed of 3.7 m/s was used.
Both in the bending tests and those of impact strength, all the samples were placed on the supports, at their smooth side (reflecting the surface of the board – mold).
The structure of the produced laminates was observed with the use of light microscopes. A stereoscopic microscope Nikon SMZ 1000 and a metallographic microscope Nikon Epiphot 200 were used. A Nikon DS-FI 1 video camera, together with the dedicated software, was applied for the rerecording and acquisition of images.
Analysis of the results
Fiber volume fraction determined for laminates produced by hand lay-up and VARI.
VARI: vacuum-assisted resin infusion.
Charpy impact strength of laminates produced by hand lay-up and VARI.
VARI: vacuum-assisted resin infusion.
For the evaluation of the test variation degree, the classic measure of distribution variation was applied, which is the coefficient of variation. It is a relative measure which depends on the arithmetic mean value. The coefficient of variation Cv, expressed in percentage, was calculated according to the following equation
The fiber volume fraction of the laminates with a fabric base, produced by two different methods, are comparable. It was also stated that, in this case, the coefficient of variation differences are relatively slight (Table 3). However, the coefficient of variation is clearly lower for the VARI laminate, which proves an even distribution of the fraction in the panel. A much bigger difference in the coefficient of variation of the volume fraction is observed in the case of the mat reinforcement. For the hand lay-up laminate, it is over 4 times higher than for the VARI laminate (Table 3). In this case, the volume fraction itself demonstrates a very big difference – it is higher almost by half for the VARI laminate than that for the hand lay-up one.
The flexural strength of the laminates with the fabric base is comparable for the laminates produced by the alternative methods – it is even slightly higher for the hand lay-up laminate. However, the coefficient of variation is over 2 times higher for the hand lay-up laminate (Table 4). This is probably a result of the slightly more uniform distribution of the volume fraction in the board obtained by VARI. An almost 2.5 times higher percentage deviation of the flexural strength is demonstrated by the hand lay-up laminate with the mat base, as compared to the equivalent VARI laminate. The latter also demonstrates a flexural strength itself which is higher by half (Table 4). Undoubtedly, this is connected with the big difference in the volume fraction between the both laminates (Table 3).
The Charpy impact strength is comparable for the laminates with the fabric base, produced by the hand lay-up and VARI methods. The coefficient of variation is higher by over a half for the hand lay-up laminate than for that for the VARI one (Table 5). This is confirmed by the trend of the flexural strength results. An over 2 times higher coefficient of variation of the impact strength results is exhibited by the hand lay-up laminate with the mat base, as compared to the equivalent VARI laminate. The mean impact strength value is almost 1/3 higher in the case of the VARI laminate (Table 5). This means that the big difference in the volume fractions between both laminates (Table 3) has an essential effect both on the impact strength and the flexural strength.
Figures 4 to 6 present the distribution “maps” of the measured values on the schemes of the laminate panels.
Fiber volume fraction distribution in the produced boards: black – VARI, grey – hand lay-up, bold – fabric, italics – mat. Flexural strength (larger squares) and Charpy impact strength (smaller squares) distribution in the laminate panelss – plain weave fabric. Black – VARI, grey – hand lay-up. Flexural strength (larger squares) and Charpy impact strength (smaller squares) distribution in the laminate panelss – chopped strand mat. Black – VARI, grey – hand lay-up.


In the case of the hand lay-up laminates, both with the fabric and the mat base, one can see a higher volume fraction in the central area of the board than that in the area closer to the edge (Figure 4). This may be connected with the removal of a larger excess of the resin from the central section – the resin is removed with a roller towards the edges and, as possible, outside the laminate. Probably, a consequence of such a “gradient” of the fiber volume fraction is a similar trend demonstrated by the flexural strength and impact strength (Figures 5 and 6).
Also in the case of the VARI laminates, a higher volume fraction, flexural strength and impact strength were observed in the central areas of the boards (Figures 4 to 6). In the case of the applied technique, such a trend is probably caused by the diversified conditions of the vacuum bag’s pressure in the central area and on the edges of the preform. It results from the difference in the resin flow rate in those areas, which has been observed in the VARI processes. 41 However, a clearer, increasing, trend, both in the fiber volume fraction distribution and the flexural and impact strengths of the VARI laminates, is observed in the direction from the resin inlet edge to the vent edge (Figures 1, 4, 5, and 6). This is, undoubtedly, a result of the more thorough “suction” of the resin from the areas closer to the vent than in the case of the further areas. This effect occurs though application of metered amount of resin (only with very little surplus) and closure of the inlet respectively before the resin fulfilled the all preform. In the VARI process, the area filled with the resin, located a few tens of millimeters behind the resin front, is practically devoid of the vacuum bag’s pressure. This has a negative effect on the fiber volume fraction, especially in the areas significantly distant from the vent edge, where one can observe “swelling” of the flowing resin and accumulation of its excess. The difference in the resin’s local volume fraction and the way of filling the preform is significant for the laminate properties. 42 The observed property gradient is similar for the laminates based on fabric and those based on mat (Figures 4 to 6).
The differences in volume fraction between the hand lay-up and the VARI laminates may arise from the different uniformity of pressure put on the preform during saturation. In hand lay-up process, the excess of resin was removed without applying a strong pressure, but only by local squeezing. While, in VARI process the pressure applied was probably uniform within all preform area (however, pressure changes in each point of the panel – it is different up to the passing of the resin front and after this moment). This difference of pressure uniformity may be the main cause determining the obtained volume fraction distribution.
The obtained results show that the mechanical properties of the laminates, independently on the structure and the manufacture method, strongly depend on the volume fraction of the fibers. It is its value which determines the flexural and impact strength values, whereas its variation in the laminate board determines the variation of those properties. Figure 7 presents linear approximations of the mechanical property dependences on the reinforcement volume fraction for the respective laminates.
Linear approximations of the results depending on volume fraction: (a) impact strength – laminate with fabric; (b) impact strength – laminate with mat; (c) flexural strength – laminate with fabric; (d) flexural strength – laminate with mat.
The value of R2 (correlation coefficient) of the presented approximations (Figure 7) confirm that the effect of the volume fraction on the properties is fundamental. The lowest value of R2 (0.86) proves an 86% effect of the reinforcement volume fraction on the impact strength of the fabric laminate made by VARI.
The inaccuracy of the linear model, in the explanation of the effect of the volume fraction on the flexural and impact strengths, results – to some extent – from the stochastic factors, such as technological defects. However, it probably also results from the different than linear, shape of the function describing those dependences. Especially the values of parameters “b” in the approximating functions (Figure 7) point to the fact that, with a lower fiber volume fraction than that obtained within this work, the drop of the mechanical properties together with the drop of the volume fraction will be less intense. In the opposite case, for example, the impact strength of the fabric hand lay-up laminate (Figure 7(a)) would equal 0 kJ/m2 by the volume fraction of 58.5%, which is absurd. The presented approximations should thus be treated as a comparative tool only within the range of the analyzed populations.
Comparison of volume fractions of laminated boards obtained by hand lay-up and VARI.
VARI: vacuum-assisted resin infusion.
A very good repeatability of the boards produced by the VARI method was achieved, both with the fabric and the mat base (coefficient of variation below 1%). The highest repeatability was obtained for the hand lay-up laminate with the fabric base. This value is not, however, significantly different from the results for the equivalent VARI laminate. Yet, this proves that it is possible to achieve a perfect repeatability of the products manufactured by the hand lay-up method, especially in the case of the use of fabric. The hand lay-up laminate with the mat base demonstrated a less advantageous coefficient of variation (over 7%).
Comparison of thickness of the laminates obtained by hand lay-up and VARI.
VARI: vacuum-assisted resin infusion.
Comparison of Pearson corellation coefficient between thickness of the studied laminates and their fiber volume fraction.
VARI: vacuum-assisted resin infusion.
The mat laminates and and the plain weave fabric laminates showed very similar, not very bad correlation between volume fraction and thickness. However, very low correlation present (in both cases) the VARI laminates. It is probably caused by the already mentioned “gradient” distribution of fiber volume fraction and thickness (Figure 4 and Table 7). In this case the Pearson correlation coefficient is determined from two “parallel” line-shaped sets of points, instead of one. It results in undervaluation of the coefficient.
In order to explain the differences in the tested properties between the laminates and the local variations in the observed trends, a microscopic observation of the structures was performed. Selected images are presented in Figures 8 to 11.
Fabric-based laminate: (a) VARI – visible “chambers” filled with air on band crossings; (b) hand lay-up – visible non-uniform saturation of bands. Stereoscopic microscope Nikon, magnification 20×. Mat-based laminate, hand lay-up – visible structural defects: (a) surface damage and an air bubble; (b) magnified surface damage; (c) magnified air bubble. Metallographic microscope Nikon. Fabric-based laminate, cross-section: (a) VARI (cut from the panel section close to the sucking edge – the scheme; resin “pools” between the strands are not visible – arrows); (b) hand lay-up – visible local defects caused by undesaturation. Stereoscopic microscope Nikon, magnification 20×. Mat-based laminate, cross-section: (a) VARI; (b) hand lay-up. In both cases, visible local defects caused by undersaturation – smaller for VARI laminate. Stereoscopic microscope Nikon, magnification 20×.



The laminate based on fabric, produced by the VARI method, characterizes in a good quality in the visual evaluation. It has a unifrom transparency, without visible opacities. In a more accurate microscopic analysis, one can clearly see partially closed “chambers” filled with air (Figure 8(a)). They occur in the area right next to the surface, at the crossing of the fiber bands. They are formed as a result of the “collapse” of the gelating resin under the effect of shrinkage. A film of resin remains glued to the bag adhering the surface of the preform and cures on it, thus sealing the “chamber”. Defects of this kind, undoubtedly, have an adverse effect on the laminate mechanical properties; they can constitute an area of crack initiation.7,44,45 However, the “chambers’ are distributed uniformly on the whole surface of the board, and so they do not locally disturb the material’s properties or the global scatter of results (their negative effect is uniform for the whole panel surface). The cross-section of the structure of the fabric laminate produced by VARI demonstrates a good adhesion of the layers, without any visible undersaturated areas (Figure 10(a)). However, there is a significant difference between the structure of specimens cut from the section of the panel close and distant from the sucking edge – compare Figures 10(a) and 12. Evident reduction of the laminate thickness is visible with approaching to the sucking edge. Moreover, the specimens cut distant from the sucking edge (Figure 12) show “pools” of resin visible at the upper surface of the laminate, in pockets between the fiber strands.
Fabric-based VARI laminate cross-section: (a) specimen cut from the middle-close panel section; (b) specimen cut from the panel section close to the inlet edge; the cutting areas indicated in the scheme. The “pools” of resin are visible at the upper surface of the laminate – arrows. Metallographic microscope Nikon.
Such “pools” are almost imperceptible in the specimen cut close to the sucking edge (Figure 10(a)). Moreover, the pockets themselves are hardly visible.
The observed differences in structure of the VARI laminates’ structure without the doubt affect the fiber volume fraction and thereby – mechanical properties in various parts of the laminate panels. The volume fraction is probably lower in the areas distant from the sucking edge – flexural strength and impact strength are evidently lower for the specimens cut from these areas (see Figures 5 and 6). The differences in structure have also influence on a distribution of fiber volume fraction through the thickness of the VARI laminate. In the section of the panel distant from the sucking edge, it is probably lower in the area close to the upper layers, where the excess of a resin – caused by under-pressure of the bag – collects (Figure 12). The through the thickness distribution of the volume fraction is rather uniform in the section close to the sucking edge (Figure 10(a)), as well as in the hand lay-up laminates (Figures 10(b) and 11(b)).
The cross-section of the mat-base laminate, produced by the VARI method also characterizes in a compactness of the chambers, and, with the magnification of 20×, reveals only few local undersaturations (Figure 11(a)).
The fabric laminate produced by the hand lay-up method is characterized by a good quality in the visual evaluation. However, contrary to the VARI laminate, it has randomly distributed opacities, proving a non-uniform resin saturation. The microscopic analysis showed no “chambers” with air, characteristic for the infusion laminate (Figure 8(b)). The lack of “chambers” does not mean the lack of surface flaws in the band crossing area; in the hand lay-up laminate, those areas are, simply, “open”. The defects are distributed evenly on the whole surface of the panel, and so their negative effect on the mechanical properties is uniform, analogically to the case of the VARI laminate. The cross-section, which reveals the laminate structure, shows a big number of local defects resulting from undersaturation (Figure 10(b)). The local undersaturation of the laminate is additionally confirmed by a certain number of fiber bands which have evidently come unstuck from the remaining structure, probably while the laminate was being cut with a rotating disk. Such bands are not observed in the case of the VARI laminate (Figure 10(a)). The structure of the hand lay-up laminate with the mat base demonstrates local flaws (Figure 11(b)), which are larger and more numerous than in the case of the infusion laminate (Figure 11(a)). Despite the fact that the difference in the volume fraction of the fibers between the mat-base laminates produced by the two respective methods is big (Table 3), the difference in the structure is not as significant as in the case of the fabric laminates.
The main reason for the differences in the properties of the laminates produced by the two alternative methods and in the scatter of measurement results are probably the structural defects introduced during the hand lay-up lamination. The main types of such defects are: local undersaturations, air bubbles, and surface damages (Figure 9). Such exemplary flaws are stochastic in character and their presence strongly affects the local distribution of the fiber volume fraction and the mechanical properties. It has also an effect on the global scatter of measurement results.
Conclusions
The volume fraction of the plain weave fabric in the laminates manufactured by the hand lay-up and VARI methods is comparable. In the case of the mat reinforcement, the VARI laminate showed a fiber volume fraction by half higher than that of the hand lay-up one. The flexural and impact strengths of the plain weave fabric-based laminates produced by the hand lay-up and VARI methods are comparable. In the case of the mat reinforcement, the VARI laminate demonstrated a flexural and impact strength 1/3 higher than in the case of the hand lay-up laminate. The hand lay-up laminated panels show a gradient of the fiber volume fraction and the flexural and impact strengths towards the center of the board. The panels produced by VARI demonstrate a similar gradient and, additionally, a distinct gradient of those properties in the direction of the “sucking edge”. The coefficient of variation of the fiber volume fraction in the laminate reinforced by plain weave fabric is over 1/3 higher for the population of samples produced by the hand lay-up method than for that produced by VARI. In the case of the mat-reinforced laminates, this difference equals over 4 times. The coefficient of variation of the flexural and impact strength of the laminates reinforced with the plain weave fabric is, respectively, 2 times and by half higher, for the hand lay-up laminates than for the VARI ones. In the case of the mat-reinforced laminates, the difference in both the flexural and the impact strength equals over 2 times. The level of the flexural and impact strength is strongly dependent on the fiber volume fraction, both in the global and the local scale. The gradient or the disturbance of the volume fraction result in, approximately proportional, disturbances of the mechanical properties. In the case of the fabric reinforcement, both for the VARI and the hand lay-up method makes it possible to achieve a good repeatability of the fiber volume fraction in the produced panels. In the case of the mat reinforcement, a much better repeatability is provided by the VARI method (9 time difference in the coefficients of variation). The repeatable structural defects in the hand lay-up and VARI laminates are distributed uniformly and regularly. They have thus little effect on the repeatability of the mechanical test results. The random local technological flaws much more often occur in the hand lay-up laminates. They are the main cause of the local disturbances in the mechanical properties of the laminate and negatively affect the scatter of test results. The VARI laminates as well as the hand lay-up laminates show specific gradiented instability of the structure caused by the pressing forces acting during impregnation process. The VARI laminates characterize in a distinctly better repeatability with respect to the volume fraction and the mechanical properties, as compared to the hand lay-up ones.
Footnotes
Funding
This study has been financed by the National Centre for Research and Development (NCBiR) of The Republic of Poland in the scope of the project LIDER/08/31/L-2/10/NCBiR/2011.
Conflict of interest
None declared.
