1. Introduction
Fiber-reinforced plastic (FRP) composite materials are known for their combination of high mechanical properties, lightweight design flexibility, and non-corrosive properties and, hence, have been making inroads in aerospace, automotive, and trucking industries where fuel savings are very important [
1]. The most commonly used fibers are synthetic fibers like carbon, glass, aramid, and natural fibers combined with different matrix systems such as thermoset or thermoplastic resin [
2]. Each matrix system has advantages and disadvantages over the other. For thermoplastic material, better recyclability, higher production rates, and better impact behavior are stated [
3]. Thermoset resins are mostly liquid at room temperature and curing due to an exothermal reaction [
4]; therefore, the manufacturing processes can be handled without complex, heated consolidation tools, and the viscosities are lower by 3–4 orders of magnitude [
5,
6], making it possible to use infusion processes for impregnation [
2]. The matrix properties regarding strength and stiffness are usually higher than they are for thermoplastic matrices, but they are more brittle [
7]. The material properties can, hence, be adjusted due to the combination of fiber and the matrix system, where the orientation of the fibers has a major influence on the mechanical properties [
8]. The manufacturing of semi-finished products as a basis for the preforming by the state of the art is performed on textile machines like weaving, braiding, or embroidery machines [
2].
The choice of fiber, matrix, and manufacturing process highly determines the performance and field of application of a composite material [
9]. Carbon fiber is used when high strength, high stiffness, or properties like minimum thermal elongation or electrical conductivity are essential. This includes applications such as aerospace components, measuring systems, and fast-moving machine parts with high positioning accuracy requirements. Glass fibers are usually used when the cost is a more dominant factor [
10] and large amounts of fibers are needed that still offer good performance, like for the rotor blade wings of wind power plants, pipelines in the energy sector, or boat hulls.
The composite material, made of fiber and plastic, is created during the manufacturing process. As a result, different manufacturing methods, process variants, and fluctuations in the process parameters always lead to changes in the material properties, such as fiber volume fraction, void content, strength, and stiffness [
11]. A major challenge in the production of FRP composites is the impregnation process of the reinforcement fibers with a liquid resin. Among several production techniques, Liquid Resin Infusion (LRI) methods like Seeman’s composite resin infusion process (SCRIMP) or vacuum-assisted process (VAP) are often used because they allow the reinforcement materials to be handled dry, have low investment costs, and can be adapted to manufacture a low-to-medium volume of parts [
12]. In general, out-of-autoclave processes are becoming more relevant and show similar results to autoclave materials [
13]. Among the many techniques included in LRI, VAP is a common one in the aerospace industry as it allows the production of high-quality composite parts with reasonable reproducibility. To reach the estimated quantities of future aircraft production [
14], manufacturing processes must be improved by their sustainability to reduce their environmental impact, like waste reduction and, in parallel process, automation to enhance productivity. In particular, LRI processes are difficult to automate, since there is only a one-sided mold, and a complex set-up and integration of different process materials is needed [
15]. Another drawback is the high number of consumables, which become waste after the process. The goal of this study is to verify a new approach that can improve these issues and have similar outcomes regarding the laminate quality. In addition, time-saving is aimed at. The new approach of the vacuum chamber infusion (VCI) offers the potential of a high degree of automation since the process is based on an existing, highly automated process known from the packaging industry. The VAP process has been selected as a reference since it is capable of producing minimum weight, high-performance laminates with properties comparable to those of laminates produced by more expensive processes such as autoclave cured prepreg, and close to what is expected for the VCI [
16]. Since one goal is to improve the overall process efficiency, the material-efficient process DFP as a near-shape preform approach is used [
17]. Additionally, DFP preforms have a low permeability in all three directions in-plane (K1 and K2) and out-of-plane (K3). The range is between 1 × 10
−15 m
2 and 5 × 10
−14 m
2, which is 1–2 orders of magnitude lower than it is for woven fabrics or non-crimp fabrics [
18]. Subsequently, the infusion is challenging, but positive infusion results give a benchmark for other materials and allow a prediction about a feasible infusibility. The infusibility of the used DFP preforms by VAP has been approved and reported in a previous study [
19].
1.1. Vacuum Assisted Process (VAP)—Infusion Processes for Composites
The VAP infusion is a variation of resin infusion, where a semipermeable membrane separates the vacuum outlet from the surface of the part. This creates a full vacuum gradient and continued degassing across the part surface, as opposed to only at the end-edge of the part in traditional resin infusion like, e.g., SCRIMP. VAP and SCRIMP are used for the production of wind turbine blades, boats, aircraft interiors, and prototype parts. The main advantages of the VAP process are that all part sizes up to very large components with low permeable preforms, like, e.g., unidirectional carbon fiber spar cabs (>100 m), are feasible with very high process stability and low void content [
20]. The main drawback is the high cost of the VAP membrane, which is not needed for SCRIMP. The difference between VAP and SCRIMP is that within the SCRIMP process, the air removal is only done on discrete lines or points, whereas in VAP the removal takes place extensively over the whole area of the part. All mentioned processes are well established and deliver high-quality laminates with high fiber volume content and low void content [
21]. They have in common that the vacuum system is an open system with a permanent connection to the surrounding environment since the vacuum pumps are always running during the process. A sealed system is used for the VCI process, which is the main physical difference compared to VAP and SCRIMP.
Figure 1 shows the VAP infusion setup and the principle, which has been used within this study. They have in common that the air outtake is done over the whole surface of the preform.
1.2. The Vacuum Packaging Process
Vacuum packing was invented by Henri de Poix of the Dewey Almy Chemical Company and patented in 1945. The process consists of three steps [
22]:
A product is placed into a flexible and impermeable, plastic bag or container.
The atmosphere in the package is removed by evacuation.
The plastic bag or container is hermetically sealed to prevent transmission of moisture or gases into the sealed package.
The used bags usually consist of multilayer films, having different functions. The film packages and containers are mainly thermoplastic and are often thermoformed. The single layers of a multilayer film can fulfill different functions. One example is a multi-layer film consisting of PA/PE. The PA layer has a very low permeation to oxygen and moisture and guarantees that the vacuum is maintained, while the PE layer is used to enable the film to be welded securely. In addition, the PE layer can be embossed with a structure to create a flow aid for gases or liquids. The possibility of thermoforming specific packing materials like PETG opens the possibility of ensuring wrinkle-free and smooth mold surfaces, adding resin channels, and reservoirs for resin or vacuum reserve, and reducing material. The best case is to use a single-layer material because it is easy to recycle; a drawback of multi-layer film is that it is hardly recyclable [
23]. The overall percentage of worldwide recycled thermoplastic material, which is counted into the annual global production of virgin material of 400.3 Mt (the year 2022), is low, at 8.9%. The percentage of used plastics in packaging in the EU is at 39.5% and, thus, accounts for the largest share of the total demand of 53.9 Mt [
24].
1.3. Scope
The scope of this work is to analyze if similar results in mechanical properties and laminate quality of the VCI process in comparison to the state-of-the-art VAP process can be performed. Emphasis is put on the thermogravimetric and microscopic analysis of void content, fiber volume fraction, and the mechanical properties of tensile and bending strength and stiffness. Additionally, this study compares the economic aspects of the different processes and assesses possible fields of application.
2. Materials and Methods
2.1. Vacuum Chamber Infusion
The VCI process is a method to bring reinforcement fibers and liquid matrix together in a closed system with a flexible surrounding. The process is adapted from the vacuum packaging process. The fibers or the preform are put in a vacuum bag together with the matrix. Both components are positioned inside the bag in a way that they do not touch each other and that a complete evacuation of all free spaces is possible. The filled bag is then evacuated in a vacuum chamber and sealed. In the next step, the chamber is ventilated, and the impregnation process starts. Since a closed system is created, the process is going on until an equilibrium is reached.
This study used a modified vacuum chamber sealing machine Komet S501 (Komet Maschinenfabrik GmbH, Plochingen, Germany), with a chamber dimension of 895 mm × 565 mm × 230 mm, for the infusion trials. The two welding bars have lengths of 740 mm and 455 mm. In
Figure 2, the machine and the modifications are displayed, including the setup for the performed infiltrations of the sample plates. The machine includes two vacuum pumps for evacuation, one before the setup is sealed with a high flow rate and a second smaller one to adjust the vacuum inside the chamber after sealing if the chamber is not ventilated immediately.
To prevent the control from stepping into the sealing and ventilation sequence, a switch has been implemented to hold the vacuum. With this function, a pressure difference between the inside and outside of the bag can be adjusted between 0 and 1000 mbar. The machine has been equipped with a bellow valve to adjust the minimum pressure between 4 and 45 mbar. This is necessary to control the degassing or cocking of the resin during the process. The control panel allows to set a timer on how long the vacuum pump runs before the sealing and ventilation starts. The second function is the adjustment of the sealing time to adapt the sealing to the thickness and material of the vacuum bag.
The VCI process parameters have been kept constant for all trials. For all trials, the resin has been prepared as follows. The resin component A is mixed with the degasser (1%-mass) and mixed by hand for 3 min. The mixture is degassed for 3 min/15 mbar. Afterwards, the hardener component B is added, and the mixture is stirred for 3 min. The last step is degassing for 3 min/15 mbar. The used vacuum bags are non-structured inside and consist of a two-layer film (PA6/PE). The outer PA6 layer is the gas barrier and the inner PE layer works as a sealing medium. The bags, type SR 400 × 600 PA/PE90 (Allfo GmbH & Co. KG, Waltenofen, Germany), have a size of 400 × 600 mm and a thickness of 90 µm. To measure the pressure inside the chamber, a vacuum measurement device is used, with a precision of ±1.0 mbar (Komet Maschinenfabrik GmbH, Plochingen, Germany, vacuum gauge with pressure equalization).
Figure 3 shows the principle of how the infusion is performed. The numbering of the following description list is consistent with
Figure 3; it describes the course of the process:
A rule is set up for the pressure ratio of the inner and outer bag according to Equation (1). The inner bag has to have a lower pressure value than the outer consolidation bag. Otherwise, the inner bag will blow up during the evacuation and a distortion or wrinkling of the already impregnated preform can occur. In this study, a difference of 16 mbar has been chosen.
2.2. Materials
In this study, spread Mitsubishi 30k carbon fibers are processed into a one-sided bindered 20 mm wide tape on a spreading line (M&A Dieterle GmbH, Ottenbach, Germany, fixedTow production line) and placed via a 2D Dry Fiber Placement (DFP) machine (M&A Dieterle GmbH, Ottenbach, Germany, Crosslayer). All used materials are displayed in
Table 1, showing the material properties of the fixedTow after spreading. The Mitsubishi 30k fiber is chosen for its good spreadability and consistent quality. The properties of the fixedTow and the raw fiber are displayed in
Table 2 and
Table 3.
2.3. Preforming: Tape Production and Dry Fiber Placement
To create the fixed tows, the fibers are spread to a width of 20 mm (±0.5) using a mechanical spreader and then secured in place with the binder. The used binder, in powdered form, is applied onto the spread tow and activated through infrared lamps. Subsequently, the tow is consolidated, cooled, and, ultimately, wound onto a film spool. The amount of binder utilized is consistent at 8% for all specimens, and activation of the binder occurs at 110 °C for all fixed tows.
To create the preforms, a DFP machine is used for the placement of the tapes. The fixed tows are placed at a laying speed of 8.5 m/min and an IR halogen lamp output of 360 W. A maximum of six plies were placed on top of each other. To produce preforms with more than six plies, the ply configuration is divided into several sub-preforms and stacked manually afterward. The preform size is 330 mm × 320 mm and the plies are placed on a plain weave glass fiber fabric, which serves as the placement substrate. The substrate only serves as a carrier for the placement process and is subsequently removed before the infusion. For adjacent plies with the same orientation, the layup path is parallelly shifted by 50% of the path distance. The path distance is set to 22 mm for all preforms. With this distance, a gap of 2 mm is implemented between each tape to lower the permeability compared to a layup with no gaps [
4].
Table 4 shows the division of the subpreforms and how they are combined to create a symmetrical laminate.
2.4. Manufacturing of Plates, Sampling, Testing, and Analysis—VCI and VAP
For each sample configuration, the infiltration process, the fiber orientation, and the layer count are varied, as shown in
Table 5. An amount of three plates each have been manufactured, a total amount of 12 plates. The size of the plates of 320 mm × 330 mm is chosen based on the required size of the samples for the mechanical testing, the chamber size, and the ease of handling of the preform and infusion set-up.
The last two columns show what kind of testing methods have been used to test the corresponding configuration mechanically. The curing has been performed for 24 h/RT. After removing the process materials, the plates have been post-cured for 6 h/80 °C in a convection oven. The resin reference samples for the determination of the density of the pure resin have undergone the same curing cycles. Each plate has its own batch of mixed resin.
From each plate, nine specimens of 10 mm × 10 mm have been extracted at three different places (3 × A, 3 × B, 3 × C) to determine the fiber volume fraction, void content, and density (see
Figure 4). Each plate has a resin reference sample from which the density has been determined (three specimens each) to get a higher accuracy for the void content analysis. The samples have been analyzed according to NORM EN 2564. From each of the 1 mm thick plates, six samples have been cut out with dimensions of 250 mm × 15 mm for unidirectional tensile testing. From the 2 mm plates, six samples of 250 mm × 15 mm have been cut for tensile testing, and additionally, six samples of 100 mm × 15 mm for bending tests. The bending test is performed with a Hegewald&Peschke “Inspekt Table 20” testing machine (Hegewald&Peschke Meß- und Prüftechnik GmbH, Nossen, Germnay) and a load cell of 20 kN according to DIN EN ISO 14125. The tensile test is performed with a Hegewald&Peschke “Inspekt Table 250” (Hegewald&Peschke Meß- und Prüftechnik GmbH, Nossen, Germnay) and a load cell of 250 kN, according to DIN-EN ISO 527-5 and DIN-EN ISO 527-4. The microscopic analysis is made with a digital microscope type Keyence VHX 7000 using an objective Keyence VH-Z250 series, type RZx250-x2500 (Keyence Deutschland GmbH, Neu-Isenburg, Germany). The areal void content is measured using the open-source software tool ImageJ (Wayne Rasband and contributors, Version 1.54g, National Institutes of Health, Bethesda, MD, USA) for digital image analysis. To achieve this, each image is calibrated using a scale derived from the Keyence microscope software.
4. Discussion
The results show that using the vacuum chamber infusion process results in similar laminate qualities as the VAP process when using the same dry fiber placement preform layup. In particular, the low void content of less than 2% and fiber undulation indicate a good industrial application in the future for the new process, although it was recognized that there was a slight fiber washing for the unidirectional preform due to a missing compaction pressure during the infusion process. No fiber washing was observed in the 0/90° oriented fibers because the perpendicular orientation keeps the tows in place.
Values between 39% and 45% are observed for the fiber volume fraction for both infusion methods, while the values for the VCI method are in the lower range. The authors estimate that the generally low FVF depends on the preform and not on the process itself. The reason is seen in the used DFP preform, which has a binder content of 8% and a fiber spacing of 2 mm when deposited. [
27] reports a reduction in fiber content for DFP laminates with a 0.8 mm gap of 5% in fiber volume fraction compared to a reference laminate without gaps. Studies with other semi-finished products have shown that fiber volume contents beyond 52% are otherwise reachable with the VAP process [
16,
28]. A possible reason for the low FVF for VCI may be that the amount of resin used was too high. Initially, the amount was chosen to ensure a safe complete impregnation without visible dry spots on the plate surfaces. Since this process is being analyzed for the first time, the amount used and its position are not yet optimized. If the resin distribution inside the bag is optimized, it offers the chance to find an optimum for good impregnation, thereby increasing the FVF. Additionally, the VCI also offers the option of consolidating the impregnated preform by using a press to further increase the FVF. The preform can be kept inside the bag, and placed in the press, and excessive resin can be removed and stay inside the bag. However, it should be taken into consideration that using a press would increase the complexity and diminish some advantages of the VCI in the way described in
Section 2.1. As 39% FVF is too low for high-performance composite applications, the VCI should be further optimized. Studies with unidirectional and multi-axial non-crimp fabrics have to be performed to evaluate the maximum achievable FVF and investigate the void formation and fiber washing for these types of preforms. Additionally, alternative ways of consolidation have to be investigated.
Furthermore, the mechanical properties measured suggest great potential for structural applications in both processes. When the absolute values are normalized to a common fiber volume content of 40%, the VCI values for tensile 0° and bending 0/90° are approx. 10% higher than the measured characteristic values for VAP. The higher normalized values for VCI tensile 0° can be explained by the minor laminate quality of the unidirectional VAP plates, where surface unevenness, high thickness variation, and undulations perpendicular to the 0° fiber direction are overserved in the cross-sections.
The normalized value for the tensile 0/90° configuration shows 26% higher strength values for the VAP process. The stiffness is 4% higher, though it is in the range of the standard deviation. The normalized 0/90° bending value for strength is 11% higher and for stiffness 16% higher for the VCI process. Since the 0/90° laminates show a higher homogeneity for both processes, which is revealed by the microscopic analysis, these values can be regarded as more reliable for comparison and evaluation of the process potential. Since the difference in the result of the two values for bending and tensile is minimal and the differences are within the range of the standard deviations, a similar quality regarding the mechanical properties can be stated for both processes.
Due to this fact and the overall low void content, a correlation between the absolute void content and the mechanical properties of the 0/90° laminates cannot be worked out. Regarding the values of the unidirectional laminates, it can be clearly stated that the bad surface condition of the VAP plates lowered the tensile strength compared to the VCI values. The induced undulation resulting from the resin flow for VCI and the undulation introduced into the VAP laminates by the release fabric results in lower mechanical values than are theoretically possible. For a unidirectional laminate, the theoretical maximums for the VCI and VAP are displayed in
Table 9 with respect to the measured FVF. The calculation is performed according to [
29]:
It can be seen that the reached tensile strength value for VAP is with 25% lower than it is for VCI, with 19%. The theoretical maximum for the stiffness is reached for VCI, whereas the value for VAP is 10% lower. By using an optimized VAP infusion setup, such as adding a caul plate or using a different flow medium, this issue could be addressed. The significant economic finding was demonstrated that VCI requires fewer consumables, and its setup is four times faster compared to VAP. The infusion time was similar because the pressure difference was the same, and the preform was identical. This results in reduced production costs, higher unit output, and lower resource consumption. When vacuum bagging, double the amount in VCI is needed because the entire preform is wrapped in an inner bag. The outer bag can be reused since it does not come into contact with resin, making it easier to recycle and reuse. As a result, the VCI process has a lower environmental impact due to the overall reduction of consumables and the use of only one material type, which makes it easier to recycle.
At the current stage of development, the low fiber volume fraction of 39% is limiting potential applications. The following applications could be possible when only considering the restrictions of the dimensions of the used chamber: for the automotive and aerospace sectors, flat or slightly curved plate structures, possibly with stiffening beads, and simple 2D components such as deflection levers or brackets; in the sports sector, parts such as skateboards, spring elements in shoe insoles, or rackets could be considered. There is also great potential in the field of medical technology, with possible applications including orthoses/prostheses, parts of walking aids, or wheelchairs. In this area, in particular, a low-cost manufacturing process offers high social added value, as it would give more people access to this technology [
30]. To address the issue of size, a test setup using a larger vacuum chamber has to be conducted. Larger vacuum chambers already exist on the market and can be custom-made. An economic analysis needs to be conducted to determine the chamber size at which the cost of building and operating the chamber outweighs the benefits. Additionally, there are expected scaling issues that will need to be addressed. These include handling the preform, any required molds, and the resin system.
5. Conclusions and Prospect
The scope of this work was to analyze if similar results in mechanical properties and laminate quality of the proposed VCI process in comparison to the state-of-the-art VAP process can be performed and which economic benefits can be achieved. The manufacturing approach has been thoroughly investigated for the first time, and the key findings are as follows:
The DFP laminates produced using the VCI process exhibit comparable mechanical properties to those produced using the VAP process when normalized to a similar fiber volume content. The absolute values are in a relevant range for industry applications. The normalized values for the tensile strength and modulus of 0/90° configurations are 772 MPa and 52 GPa for VCI and 975 MPa and 54 GPa for VAP. For the bending strength and stiffness, the size ratio of the values is reversed, with higher values for VCI with 646 MPa and 50 GPa and 851 MPa and 43 GPa for VAP.
The fiber volume fraction for VCI with 39.0% is about six percentage points below the value of VAP. Process optimization has not been performed yet, allowing room for improvement, especially with non-bindered preforms like non-crimped fabrics.
It is shown that the laminate quality of the infusion process of a one-time evacuated and then sealed system (closed system) in terms of void content is equal to an infusion process of a permanently evacuated setup (open system). The void content is below 2% for both the VCI and VAP processes. This result makes it suitable for industrial use [
26]. The low void contents for VAP have been confirmed.
The number of different consumable materials required for VAP can be significantly reduced with VCI, resulting in a drastic 4× timesaving in the preparation of the infusion process compared to the VAP method.
However, for good impregnation, the compatibility between resin viscosity and preform permeability is essential and is also a challenge within the vacuum chamber process. For the VCI, this is even more so, since there is no permanent evacuation. The limitations are predicted to be in the number of layers respectively the thickness of the preforms depending on their permeability. The limitations are predicted to be in the number of layers, with the thickness of the preforms depending on their permeability. Therefore, process optimizing studies have to be performed to analyze the infusion behavior more in detail, increasing FVF by using different dry preforms like fabrics or non-crimp fabrics. Despite having flat plates of 320 mm × 330 mm in size, no complex 3D geometries were manufactured using VCI. These geometries need to be approved in future studies. To achieve more complex geometries, two approaches are possible, and both are recommended for further study:
The final contoured preform is only impregnated using the VCI process. The infusion structure can then be molded and cured in a consolidation tool. It is also possible to remove the impregnated preform from the bag and then place it in a consolidation mold, like using a standard prepreg material.
The VCI process can also be carried out in a sufficiently rigid thin-walled mold. This mold can, e.g., be produced by injection molding or thermoforming from a thermoplastic material. Thin metal sheets are also conceivable.
The limitations of the VCI process arise from the size of the available vacuum chamber, the forming of three-dimensional infusion bags, and the thermoformed molds. Large vacuum chambers measuring 5.5 m in diameter and 12 m in length are available [
31] and thermoforming parts with sizes up to 4 m
2 [
32] are feasible, defining the potential dimensions. It is important to validate the feasibility of implementing geometric upscaling to increase its industrial appeal. In addition, VCI offers the highest potential for automation among all open mold LRI methods, as it requires only one consumable material. It should be noted that the original vacuum chamber process in food packaging is already highly automated [
33]. With this major advantage, the authors see a very large scaling potential with VCI in terms of the number of units that can be produced.