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© Carl Hanser Verlag Zeitschrift Kunststofftechnik / Journal of Plastics Technology 11 (2015) 4
eingereicht/handed in: 12.02.2015 angenommen/accepted: 28.04.2015
Dipl.- Ing Dino Magagnato1, Dipl.-Ing Bernd Thoma2, Prof. Dr.-Ing Frank Henning1,2 1 Institut für Fahrzeugsystemtechnik, Karlsruher Institut für Technologie (KIT) 2 Fraunhofer Institut für Chemische Technologie (ICT), Pfinztal
Experimental characterization to determine the influence of different binder systems on the preform permeability during RTM manufacturing For fixation of the preforms during RTM-manufacturing, mainly adhesive binders are used, where a uniform layer of these binders are applied between the textile layers. Previous investigations [1 – 3] showed that the laminar application of binder leads to a reduction of preform permeability for the injection process. In the following study a new preform fixation approach, called “Chemical Stitching”, is introduced and its influence to permeability is examined. For the permeability measurements, a 1-D test setup is used, which is mainly geared to unidirectional fiber textiles. To do the measurements under suitable conditions, specialized sensors are used to detect the flow front and the pressure history in the cavity.
Experimentelle Charakterisierung des Einflus-ses verschiedener Bindersysteme auf die Per-meabilität des Preforms bei der RTM-Fertigung Für die Fixierung von Preformlingen in der RTM-Fertigung werden aktuell hauptsächlich adhäsive Bindersysteme verwendet, die flächig zwischen die Textillagen appliziert werden. Untersuchungen von [1 – 3] haben gezeigt, dass der flächige Binderauftrag zur Senkung der Preform-Permeabilität im Injektionsprozess führt. Im Folgenden wird ein neuartiges Verfahren zur lokalen adhäsiven Preformfixierung namens „Chemical Stitching“ vorgestellt und dessen Einfluss auf die Preform-Permeabilität untersucht. Für die Permeabilitätsmessungen wird ein 1D-Testaufbau verwendet, der vornehmlich für unidirektionale Faseraufbauten ausgelegt ist. Um die Messungen unter geeigneten Bedingungen durchzuführen, werden speziell ausgelegte Sensoren verwendet, um die Fließfront und den Druckverlauf in der Kavität zu verfolgen.
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Zeitschrift Kunststofftechnik Journal of Plastics Technology www.kunststofftech.com · www.plasticseng.com
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 257
Experimental characterization to determine the influence of different binder systems on the preform permeability during RTM manufacturing
D. Magagnato, B. Thoma, F. Henning
1 INTRODUCTION
Fiber reinforced composites are increasingly used for industrial applications due to the combination of low density and good mechanical properties. For small series productions it is already possible to realize the economic boundary, but for large-batch productions like in the automotive industry, the production of cost-efficient composites parts is still a big challenge. This is because of the high material and production costs coupled with low degree of automation vis-a-vis production of metal parts. The Resin Transfer Molding (RTM) process offers because of good possibilities for automation huge potential for mass production of high quality fiber reinforced structures. All RTM-methods combine a low-viscosity thermoset or thermoplastic matrix with laminar textile reinforcement structures in order to get a fiber composite part after the curing of the matrix. The process can be divided in following main steps as: cutting of fiber textiles, the exact placement of dry reinforcement fibers in a heated cavity, the infiltration of semi-finished fiber materials with matrix resin and the demolding of the cured fiber composite part. Textile fabrics are the starting point for the efficient production of complex-formed composite parts. These are mostly woven fabrics or non-crimp fabrics of carbon, glass, aramid or natural fibers as a semi-finished product. The laminar semi-finished fiber materials are processed into 3-dimensional textile preforms for the production of complex 3-dimensional formed structures. The fixation of the semi-finished stack is ensured by sewing or by the use of adhesive binder, which is applied laminar between the semi-finished stacks. Analysis of preform permeability showed that preforms produced with the help of adhesive binders have a lower permeability compared to stitched preforms or preforms without binders. This results in a longer and time consuming subsequent infiltration process. The main reason for that is the laminar application of the binder [1 - 3]. Due to the fact that a big part of the RTM cycle time is claimed by injection and by curing of the resin/hardener combination, it is reasonable to investigate new preform fixation technologies that might have a less negative influence on the preform permeability. A new approach for an automatic fixation of dry fiber structures is examined in the Fraunhofer Innovations cluster KITe hyLITE. The so-called “Chemical-Stitching” approach is based on a local application of a liquid and fast curing adhesive.
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 258
For this approach the preform is produced by inserting specific amount of adhesive at predefined points, hence resulting in fixation of several reinforcement fiber layers. The required amount, flow and position of adhesive point are ensured with an application unit which is presented in Thoma [4]. In this approach, a consistent coherence of the laminar semi-finished fiber material is created by the cohesion and adhesion forces of the adhesive material unlike the binding force produced by continuous stitching thread. As there is no sewing thread which remains under tension, the ondulation of fibers is reduced significantly. Furthermore, to implement the adhesive, a needle cannula with a diameter far below 1 mm is used, which is smaller than in the case of the sewing process to implement the sewing thread hence reducing the fiber disorientation significantly. Due to the possibility of the introducing of a flexible and local binder, the improvement of the textile permeability and, therefore, the improvement of the flow behavior of the matrix material is expected during the infiltration process.
Figure 1: Chemical stitching - Process flow The step by step process for the application of adhesive is shown in Figure 1. The curing energy (Ec) as shown in the above figure can be in the form of heat or UV radiation. It must be ensured that the adhesive is not reducing the drape properties of the textile and, furthermore, does not have a negative influence on the mechanical properties of the final composite part. The choice of an appropriate adhesive is therefore of high significance.
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 259
2 EQUATIONS
The injection process during the RTM manufacturing is described by the law of Darcy [5]:
)( pv ∇
−=
ϕµK
(1)
Where, v is the velocity of flow front [m/s], ϕ is the porosity [-] and p is the pressure field [Pa] in the cavity. Relevant material parameters are the viscosity, µ [Pa s] of the resin and the permeability, K [m²], of the fibers, which is an anisotropic tensor of second degree. In the principal coordinate system there are three relevant parameters: K1, K2 and K3. For the unidirectional fibers the direction with best permeability, K1, is parallel to the fibers and the worst permeability K2 is normal to the fiber direction. The permeability in thickness direction, K3, can be neglected, because of the small thickness of the composites parts [6]. Unfortunately, there is yet no standard norm to determine the permeability experimentally [7, 8], which results in a certain confusion at the calculation. In this study a new permeability measurement setup is used, which is able to measure the permeability directly during RTM manufacturing. This guarantees a process-oriented approximation of the permeability behavior. The viscosity of the resin-hardener is a function of temperature and curing degree. In this study, a replacement fluid with nearly constant viscosity is used to avoid the influence of the curing process of the resin.
3 EXPERIMENTAL SETUP
The used raw materials, the preparation of the tested samples as well as the permeability measurement setup are explained in the following chapters.
3.1 Materials: Glass fiber fabric of the type 92146 with FK800 finish manufactured by P-D Interglas GmbH is used as the textile reinforcement structure for this study. The areal density of the fabric is 425 g/m². The weave structure is a plain weave with warp to weft ratio of 90:10. In context of the analysis of permeability, three different types of adhesive are examined: • Co-polyamide-binder fleece PA-1541 (Manufacturer: Spunfab Ltd) • Epoxy-binder powder Epikote 05311 (Manufacturer: Momentive Specialty Chemicals) • Acrylat PB 4468 (Manufacturer: DELO Industrie Klebstoffe GmbH)
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 260
To minimize the experimental efforts for permeability measurements, Mesamoll (Manufacture: Lanxess AG) is used, instead of epoxy resin. Mesamoll is a fluid with nearly the same fluid mechanical properties at room temperature (RT) as epoxy resin at typical RTM temperatures (~80°C). Typically, silicon oil is used for permeability measurements [7, 8], but as shown in Magagnato [9], Mesamoll shows even better agreement with epoxy resin. To minimize the influence of temperature changes during permeability measurements, the viscosity of Mesamoll was determined beforehand with a rotation rheometer of the type MCR501 (Manufactured by Anton Paar) at different temperatures [9]. During the permeability measurements, the temperatures are recorded with pressure sensors and subsequently regarded in the evaluation algorithm.
3.2 Preform manufacturing The preform permeability measurements were conducted on flat dry preform stack containing six glass fiber fabric layers with a main fiber direction of 0°. The geometry of the specimens is 520 mm x 222 mm. The specimens are fixed locally by chemical-stitching (see Figure 2), as well as laminar fixation with binder powder and binder fleece. The preforms, which are locally bindered by chemical-stitching, are produced with the help of an application unit as presented in Thoma [4]. The liquid acrylat-adhesive PB 4468 is introduced locally in the dry, six layered fabric stack compacted under vacuum foil and is in-situ hardened with the help of UV-radiation. The duration of exposure of the adhesive to the UV radiation is 10 seconds in each case. The matrix of the adhesive points for fixation is 10 mm in x- and y-direction. Preforms with adhesive doses of were further manufactured for permeability measurements.
Figure 2: Stack of glass fiber woven fabric fixed by chemical stitching The doses of 4 mg; 7 mg and 8 mg for each adhesive point further corresponds to the areal density of 6 g/m²; 10 g/m² and 12 g/m² respectively for the defined stack and fixation matrix. As a reference to the locally bindered preforms, the laminar bindered preforms (with Co-polyamide fleece PA-1541 and Epikote
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 261
05311) are also produced with similar areal density of the adhesives. The binder materials are introduced preferably homogeneous and laminar between each glass fiber layer. Afterwards, the packages of plies are compacted between two steel plates, heated up to 110 °C and kept at this temperature for 15 min for binder fixation and then cooled.
3.3 Measurement setup For this study a measurement setup [9] was used, which is able to determine permeability by tracing the flow front with specialized pressure and temperature sensors of the type MTPS 7868- STS (Manufacturer: FOS Messtechnik GmbH). Apart from the permeability measurement, the setup is also constructed to produce RTM plates by injection of a curing matrix material (for example epoxy resin). The cavity is a plate with 540 mm x 200mm x 2 mm in dimension and both parts of the tool are made of steel and 100 mm thick to guarentee that there is no deformation during the injection process.The pressure sensors are located in level with the cavity on the top part of the tool. Their signals are transferred by an amplifier type pT-Amplifier-7Ch-S (Manufacturer: FOS Messtechnik GmbH) and voltage measurement device of the type NI 9205 (Manufacturer National Instruments Germany GmbH) to a computer system. The tool is placed in a hydraulic press with a maximum press force of 3000 kN to reach necessary locking force. In this study, the test fluid phenyl ester (trade name Mesamoll) is pumped up through an injection line into the cavity by a pressure pot. The schematic of the entire permeability measurement setup is as illustrated in Figure 3.
Figure 3: Schematic of the permeability measurement setup Reprinted from [9], Copyright © 2015 Trans Tech Publications Ltd
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 262
The measurements were done at room temperature with a constant pressure difference of 5.5 bars, which is high enough to keep the influence of capillary effects down. The capillary forces have to be considered in permeability measurements with less than 1 bar injection pressure [10]. In Figure 4 the positions of the sensors in the mold cavity are presented. The analysis of the permeability is done by the seven sensors in the middle corridor of the plate.
Figure 4: Positions of the integrated sensors left: topview of the RTM tool, right: pressure history of the sensors
Reprinted from [9], Copyright © 2015 Trans Tech Publications Ltd
The two sensors (S2b and S5b) along the edge are to ensure a homogeneous flow front. On the right side of the Figure 4, a representative pressure history of the integrated sensors is shown. For the permeability calculation the arrival time of the flow front at each sensor is entered into the analytic solution for the flow in a plate with a line injection, which is derived from Darcy’s law [5]. After transposing the equation, the permeability in flow direction at each sensor position can be determined with formula 2.
ss tpp
tK
)(2)(
0 −=
φµ2sx (2)
where p0 is the injection pressure, ps is the pressure at sensor, ts is the arrival time when the flow front passes the sensor and xs is the sensor position. The output permeability is an average value over all sensors. The output permeability is an average value over all sensors.
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 263
3.4 X-ray computed tomography The analysis is conducted with the help of a x-ray computer tomography (“CT”) type „SkyScan 1076“ (Manufacturer: Bruker). The detector of the device has an image area of 1024 x 1024 pixels. During the image capture, the x-ray source and the detector are rotating around the specimen in an angle of 180°. The chosen step size of 0.7° leads to 257 single images. The acceleration voltage is 60kV, with a current of 0.17 mA. For reconstruction of the taken single images, the software „3D-Creator“ is used. The voxel size has an edge length of 9 µm. The analysis of geometry of the adhesive points is done by image processing.
4 RESULTS AND DISCUSSION
In the following section the obtained results concerning textile permeability are presented and discussed.
4.1 Results
4.1.1 Permeability measurements For this study, preforms with the three different binder systems (Epikote, Spunfab and chemical stitching; see chapter 3.2) are tested against a reference sample without binder. Furthermore the amount of binder is varied from 6 g/m² up to 12 g/m², which is the usual range for industrial applications. For each binder-textile combination at least four permeability measurements in each fiber orientation (0° and 90°) are done for statistical coverage. As usual for these kinds of measurements there is a coefficient of variation of around ±10 %. In Figure 5, the results of permeability measurements in 0°-direction (K1) are presented. The reference sample without binder has the best permeability. The permeability deteriorates with increasing amount of binder for all three kinds of binders. Especially at a low amount of binder, the samples prepared with the “Chemical Stitching” technology show here a significantly better flow behavior than the laminar bindered preforms. Whereas at 12 g/m² the permeabilities of the three binder systems are nearly equal. For permeability measurements normal to fibers (K2) also as seen in Figure 6, the permeability decreases with increasing amount of binder. Here all three kinds of binders are nearly on the same level. It seems that the permeability of laminar bindered samples is even slightly higher than of the samples fixed by chemical stitching, especially at a binder amount of 12 g/m².
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 264
Figure 5: Permeability depending on binder system at 0° fiber orientation (K1)
Figure 6: Permeability depending on binder system at 90° fiber orientation (K2)
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 265
4.1.2 X-ray computed tomography Figure 7 shows the results of the X-ray computer tomography measurements for the chosen adhesive, which has a processing viscosity of 7 Pas. The adhesive column is shown from top view as well as a cut in 90° and 0° direction. It is clearly evident, that the applied adhesive points cause a resin-rich zone, which spreads in an elliptic form in direction of the main fiber direction.
Figure 7: X-ray computed tomography measurements for the adhesive system
Delo 4468
4.2 Discussion Based on theoretical considerations [4], a significant improvement of the permeability for the locally bindered preforms is estimated. Also, after a haptic
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 266
perception of the produced specimen, a better permeability of the local fixed specimens in both directions is expected. This is, as seen in Figure 6, only partially the case. It is quite a surprising result that the K2 permeability of the chemical stitched preforms is even lower compared to the laminar bindered preforms. The CT-images of the chosen adhesive system described in chapter 3.4 deliver an explanation. As illustrated in the schematic Figure 8, the adhesive binder spreads out elliptically. The big main axis (l1) of the ellipse is thereby extended along the main fiber direction and the small main axis (l2) is extended across. This can be explained by the expansion of the fiber rovings in combination with the high fiber stiffness that leads to a local cavity and ultimately to the adhesive enrichment in fiber direction. Another reason is that the permeability in the K1-direction of the preform without binder is generally higher than in the K2-direction.These adhesive volumes cannot be infiltrated by the test fluid and could act like local disorders in the flow front and result in pressure losses. The drag coefficient of these volumes at the 0°-preforms is significantly less than the 90°-preforms, where the major axis of the ellipse is normal to the flow direction. During the infiltration of the textiles in K1-direction, the fluid is forced in a preferred flow direction, which is a sort of a flow channel, because of the introduced adhesive points. In contrary, the adhesive points in Figure 8 (Infiltration in K2 –direction (right)), are forming flow barriers. This is also the explanation for the amplifying of the described effect with increasing amount of adhesive. With an increasing amount of adhesive, the flow channels between the adhesive points are getting narrow, which results in an increasing flow resistance.
Figure 8: Schematic illustration of orientation of adhesive geometry Infiltration in K1-direction (left) and in K2- direction (right) In addition to that, losses that result from the inhomogeneity of the flow front play a less important role at the 0°- fiber direction. The flow here is inhomo-
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Magagnato, Thoma et al. Influence of binder on preform permeability
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geneous by itself because of varying wide gaps between the fiber rovings that result in dual scale flow [11, 12]. In 90°- fiber direction, the flow front is relative homogeneous by itself so that these local disorders have a bigger influence.
5 SUMMARY AND CONCLUSIONS
The results of the measurements show that the application of binder reduces the preform permeability significantly. Derived from Darcy’s law, a reduced permeability has a negative effect to the cycle times for mold filling process during RTM manufacturing. This results in increased production costs for high performance composite materials. The chemical stitching approach offers potential to reduce this effect. Particularly in fiber direction, the negative influence of chemical stitching to the preform permeability is less compared to other binder technologies. In addition to that, the chemical stitching process needs less binder to reach the same fixation strength [4]. So, generally, less binder must be used during preforming, which, again, has a positive impact on the permeability. However the adhesive dose and the disposal of the adhesive points must be carefully chosen. Especially normal to the fiber direction, the adhesive points should not be arranged too close to each other, to avoid local disorders in the flow front. Through local application of adhesive, flow channels can be placed where they are needed. So it is possible to set a targeted flow behavior and to improve the mold filling process in that way. Regarding the future process chain for the sequential preforming of textile semi-finished products to 3d-complex preforms, the chemical stitching approach could be integrated directly into a textile handling unit. So an in-situ fixation of textile patches or sub-preforms could be realized.
6 ACKNOWLEGDEMENTS
These investigations are carried out through the R&D activities of KITE hyLITE Plus project. This project is funded by the European Union through the program “European Funds for Regional Development” as well as state government of Baden-Wuerttemberg in Germany. Administrative agency of this program is the Ministry of Rural Development, Food and Consumer Protection.
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Magagnato, Thoma et al. Influence of binder on preform permeability
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Magagnato, Thoma et al. Influence of binder on preform permeability
Journal of Plastics Technology 11 (2015) 4 270
Stichworte: Permeabilität, Chemical Stitching, Resin Transfer Molding (RTM), Preforming, Binder, Hochleistungsfaserverbunde Keywords: Permeability, Chemical Stitching, Resin Transfer Molding (RTM), Preforming, Binder, high performance composite Autor/author: Dipl.-Ing. Dino Magagnato Dipl.-Ing. Bernd Thoma Prof. Dr.-Ing. Frank Henning Karlsruher Institut für Technologie Institut für Fahrzeugsystemtechnik Lehrstuhl für Leichtbautechnologie Rintheimer Querallee 2 76131 Karlsruhe
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