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Pultrusion of Large Thermoplastic Composite Profiles Up To Ø 40
Pultrusion of Large Thermoplastic Composite Profiles Up To Ø 40
Journal Article
Author(s):
Volk, Maximilian; Wong, Joanna; Arreguin, Shelly; Ermanni, Paolo
Publication Date:
2021-12-15
Permanent Link:
https://doi.org/10.3929/ethz-b-000513801
Rights / License:
Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International
This page was generated automatically upon download from the ETH Zurich Research Collection. For more
information please consult the Terms of use.
ETH Library
Composites Part B 227 (2021) 109339
Composites Part B
journal homepage: www.elsevier.com/locate/composites
Keywords: Pultrusion is a rapid and cost-effective manufacturing technology for continuous fibre reinforced thermoplastic
Pultrusion composite profiles. As the cross-sections of pultruded profiles grow to meet increasing performance require-
Thermoplastic resin ments, manufacturing challenges concerning heat transfer are encountered. In this study, a two-dimensional
Glass fibres
finite element model was used to simulate the heat transfer and fluid flow physics of the pultrusion process
Thermal analysis
for increasing diameters from Ø 5–Ø 40 mm. To facilitate the experimental validation, a novel batch-wise
pultrusion concept is introduced in which the impregnation process is observed in-situ using a transparent die.
The pultrusion studies, conducted on glass-fibre/amorphous polyethylene terephthalate (GF/PET) commingled
yarns, show that – with proper design – pultrusion is able to deliver consistent, high quality (void content <
2%) profiles up to at least Ø 40 mm.
∗ Corresponding author.
E-mail address: mvolk@ethz.ch (M. Volk).
URL: http://structures.ethz.ch (M. Volk).
https://doi.org/10.1016/j.compositesb.2021.109339
Received 25 July 2021; Received in revised form 13 September 2021; Accepted 18 September 2021
Available online 24 September 2021
1359-8368/© 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
M. Volk et al. Composites Part B 227 (2021) 109339
Table 1
Overview about pultruded thermoplastic profile cross-sections.
Author Dimensions Material
Asensio (2020) [12] 20 × 2 mm PET recycled/GF towpreg
Lapointe (2019) [13] Ø 4.8 mm PEEK/CF commingled
Tomic (2018) [6] Ø 8 mm PET/GF commingled
Novo (2016) [14] 20 × 2 mm PP/GF towpreg
Nunes (2013) [15] 24 × 4 U-shaped PP/GF towpreg
Babeau (2015) [16] 50 × 4 mm Low viscosity PA6/GF melt impregnation
Linganiso (2014) [17] 30 × 3 mm PLA/flax commingled
Kamble (2008) [5] 22.75 × 4.5 mm PP/GF commingled
Wiedmer (2006) [18] Ø 4.9 mm, 10 × 3.5 mm PA12/GF commingled
Miller (1998) [19] Ø 2 mm, 20 × 2 mm PP/GF commingled
Jürss (1995) [20] 3 × 1.5 mm PP/GF commingled
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M. Volk et al. Composites Part B 227 (2021) 109339
Table 3
Material properties of E-glass, PET and of the composite with 55% fibre volume fraction.
Material property glass fibre PET composite
Density (20–300 ◦ C) [g/cm3 ] 2.55–2.53 [32] 1.33–1.14 [33] 2.01–1.92
Heat capacity (20–300 ◦ C) [J/(gK)] 0.8-1.1 [34] 1.14–2.1 [35] 1.03–1.34
Viscosity [Pa s] 100–270 ◦ C – 8228–44 –
Glass transition temperature Tg [◦ C] – 80 ◦ C –
Thermal conductivity literature (20 ◦ C) [W/(mK)] 0.72 (longitudinal)
1.05 [32] 0.29 [36]
0.55 (transverse)
◦
Thermal conductivity experimental (20 C) [W/(mK)] 0.7 (longitudinal)
– –
0.6 (transverse)
Emissivity – – 0.94
voids from the surrounding material. Void content was averaged over and processing temperatures. First, a 3D model of the die assembly
5 different measurements evenly spaced out over the length of the was used to determine the placement of the heating cartridges and the
pultruded rod, without considering the first and last sections of the rod. distribution of cooling channels to achieve a homogeneous temperature
distribution of the die surfaces in contact with the commingled yarns.
2.3. Numerical simulation This model was then simplified into a 2D axis-symmetric model with
predefined temperature boundary conditions at the die/pultrudate in-
2.3.1. Pultrusion die geometry terfaces. The fluid flow model follows a similar approach developed for
The geometry of the heating die consists of a tapered and straight tapes by Åström, who treated the material as a fibre filled fluid inside
section, while the cross-section of the cooling die’s cavity remains the tapered section where backflow can occur, and as a solid in the con-
constant over its whole length. A schematic of the die geometry is stant cross-sections of the die where plug flow prevails [37]. To avoid
dividing the pultrudate into different physical phases, i.e. melt and
represented in Fig. 1. In the tapered region of the die, the same ratio
solid, the approach from Haffner [38] of implementing phase change
between diameter change to length change of 1:10 was used for all
through a temperature-dependent viscosity is used. The polymer flow
rod diameters to assure comparability, which corresponds to a taper
is therefore modelled through the superposition of two submodels. One
angle of 5.71◦ . This ratio was chosen due to its favourable compromise
submodel considers the backflow of the polymer through a porous
between impregnation performance, relatively short length, and ease of
media of fibres, while the second submodel accounts for the motion of
manufacture using tapered reamers. The length of the straight section
the pultrudate through the die, assuming Stokes flow. The Brinkman
of the heating and cooling dies was increased linearly with the outlet
equation is used as the governing equation of flow through porous
diameter, effectively increasing the length by a factor of two when media, due to the large variation of fibre volume content through-
doubling the diameter. This allows the total surface areas available out the heating die. The transversely isotropic permeability tensor is
for heating and cooling to scale linearly with the pultrudate volume determined using Gebart’s model [39].
to ensure sufficient heating and cooling power as the rod diameter A more detailed modelling approach for describing the pultru-
increases. The geometrical parameters of the initial Ø 10 mm pultrusion sion of commingled yarns has been developed by Kim et al. [40]. In
die tested are summarized in Table 2. contrast to Åström’s model, Kim’s model considers a dual scale flow
behaviour in which polymer matrix first flows along the dry glass
2.3.2. Model formulation fibres agglomerations before impregnating them. Kim’s approach was
A 2D axis-symmetric coupled heat transfer-fluid flow finite element not applied here because micrographs indicated that the dual-scale flow
model was developed in Comsol 5.4 to simulate the temperature distri- effects were negligible after the first 25% of the die, as the glass fibre
bution inside a Ø 10 mm pultrusion die for different pultrusion speeds agglomerations are completely impregnated with polymer.
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M. Volk et al. Composites Part B 227 (2021) 109339
Table 4
Preheating temperature for a heating die temperature of 260 ◦ C.
Diameter/speed Ø 5 mm Ø 10 mm Ø 20 mm Ø 40 mm
◦ ◦ ◦
25 mm/min 160 C 180 C 200 C 240 ◦ C
◦ ◦ ◦
50 mm/min 180 C 240 C 245 C 250 ◦ C
75 mm/min 220 ◦C 245 ◦C 248 ◦C –
100 mm/min 230 ◦C 250 ◦C 253 ◦C –
◦ ◦ ◦
150 mm/min 240 C 253 C 255 C –
The fluid flow model is directly coupled to the heat transfer model,
which is described through the 2D steady-state heat transfer equa-
tion [10]. Inside the heating die, only conduction is considered while
additional free convection and radiation terms are added once the
material exits the die. The convection heat transfer coefficient is deter-
mined for round cylinders with the corresponding Nusselt and Prandtl
Fig. 2. Micrograph of unconsolidated commingled yarn, with polymer fibres
values for ambient air at 20 ◦ C according to Kind [41], while the emis-
highlighted in violet and surrounded by a dashed line.
sivity value is determined experimentally as described in Section 2.2.
The resulting non-linear multiphysics problem is solved through a seg-
regated solver approach, where the problem is subdivided into several
2.3.7. Heat capacity
steps, solved separately, and joined at the end to compose the final
The temperature dependent heat capacity of the composite is com-
solution. A mesh convergence study was conducted to optimize the
puted based on literature values of amorphous PET [35] and E-glass
mesh refinement and element type for all sub-models while maintaining
fibre [34] using the rule of mixture. A linear regression function is fitted
the robustness of the model.
to the results:
4
M. Volk et al. Composites Part B 227 (2021) 109339
2.4. Experimental cooling die [46]. This liner is easily replaced in case of damage. The
temperature gradient between the heating and cooling temperatures
2.4.1. Batch pultrusion approach was found to be sensitive to the thickness of the liner at the transition
The batch pultrusion approach allows the space- and cost-efficient as well as to the distance between the heating and cooling dies.
pultrusion of large cross-section profiles of limited lengths. Conven- Prior to being drawn into the heating die, the commingled yarns
tional continuous pultrusion requires a bobbin creel and a yarn guid- were preheated in a custom built convection oven. Historically, pre-
ance system for each yarn that is fed into the pultrusion die. For heating set-ups were conductive systems using metal tubes wrapped
the pultrusion of a Ø 40 mm rod, 850 bobbins would be required with heater tape [47], or heated metal plates [48]. Later forced con-
assuming the heaviest available yarn weight of 2690 tex. Batch pul- vection systems using hot air blowing, such as the one used here,
trusion circumvents the space requirements and associated equipment were developed to increase the efficiency and homogeneity of the
and material cost by winding material from a single bobbin into one preheating [26,27]. Other preheating set-ups that have been proposed
thick loop to achieve the required throughput for the pultrusion die. for pultrusion include infrared [49] and microwave radiation [17] or
As illustrated in Fig. 3, the loop is cut on its trailing end after winding hybrid systems in which infrared or microwaves are combined with
and pulled through the die by a steel pulling wire attached to a load forced convection. To achieve the desired temperature distribution
cell and pulling mechanism consisting of a sled on linear rails that is inside the pre-heating oven, a custom forced convection preheating
powered by an electric winch capable of up to 100 kN pulling force concept was developed using a longitudinal airflow of adjustable speed.
and speeds up to 1000 mm/min. The pulling wire can be reused for the The temperature of the preheater was set according to the desired pro-
next experiment after removing the pultruded rod. The pultrusion speed cessing temperature, pultrusion speed, profile diameter, and the time
and pulling forces are recorded at a 2 Hz frequency using a magnetic and temperature dependent degradation behaviour determined through
position sensor with an accuracy of ±15 μm and S-type strain gauge the TGA analysis. It was chosen to be as low as possible to minimize
load cell with an accuracy of ±2 N, respectively. The length of the loop, degradation while also being high enough to enable a homogeneous
and therefore of the pultruded rod, is set to 1500 mm. temperature distribution to be reached at the outlet of the heating die.
Generally, thermoset pultrusion is thought to take several metres A maximum temperature difference of ±5 ◦ C between the centre of
before steady-state pultrusion is reached. This is due to the high pultru- the rod and the surface at the exit of the heating die was allowed. All
sion speeds used in industry and the exothermic reaction of thermosets processing parameters were set according to the results of the numer-
which requires time to develop. In thermoplastic pultrusion, steady- ical simulations. Table 4 shows the preheating temperature required
state conditions can be obtained once the temperature profile is static for the pultrusion of different diameter rods with a die temperature
and the matrix flow has stabilized. Pulling force and temperature of 260 ◦ C at different pultrusion speeds. An intermediate conduction
measurements were used to verify steady-state conditions. High heating heating element set to the preheating temperature was placed between
and cooling capacities were used so that the contact surfaces were the preheating oven and the inlet of the heating die to prevent the
maintained at a constant temperature, not influenced by the transient commingled yarns from cooling down through the transition.
material. Furthermore, shear strength testing and void content analysis All heating modules (preheater, intermediate heater, heating die)
over the length of the pultruded samples confirmed no measurable were heated by electrical resistance and regulated by PID (proportional–
influence of the position within the rod. This combined analysis showed integral–derivative) controllers. The cooling die was water-cooled with
that the pultrusion speed was the most important parameter in deter- the temperature regulated through a PID-controlled heater and fan-
mining the pulling length needed to achieve steady-state conditions. At supported radiator. Temperatures were monitored by strategically placed
the highest speed studied here of 200 mm/min, steady-state conditions thermocouples as well as pyrometers for contactless temperature ac-
were reached after a rod section with a length equivalent to the length quisition. The temperature distribution and evolution predicted by the
of the heating die was pultruded. To analyse only material made under model were validated by inserting a K-type thermocouple into the
steady-state conditions, the first and last section of the rod with the commingled yarn bundle and recording the temperature during the
same length as the heating die were omitted from the analysis. Batch pultrusion process [50]. After the experiment, the exact position of
pultrusion lengths up to 3000 mm were investigated throughout the the thermocouple inside the rod was determined and compared to the
study. A length of 1500 mm was determined to be ideal to reach steady- equivalent location in the simulation.
state conditions interesting for the study of continuous pultrusion while
providing sufficient material for characterization. 2.4.2. Transparent die
The heating and cooling dies were manufactured to the geometries A major concern with the batch pultrusion approach when com-
determined to be most effective by the numerical simulations. The pared with continuous pultrusion is the absence of fibre pretensing and
heating die is machined out of steel, while the cooling die consists fibre guidance. Fibre pretensing and guidance ensure that the fibres are
of an aluminium body with a steel liner. The steel liner protrudes straight and aligned along the pulling direction. Without these systems,
into the heating die and is made from a precision ground tube as yarns may entangle or buckle resulting in poor mechanical properties
represented in green in Fig. 1. This continuous die approach prevents in the pultruded structure. To investigate whether the lack of preten-
the recurring problem of deconsolidation of the material upon exit from sion and fibre guidance had detrimental effects on fibre alignment, a
the heating die, and the shearing and recompression upon entry into the transparent observation die was developed as shown in Fig. 4. The
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M. Volk et al. Composites Part B 227 (2021) 109339
Fig. 5. Temperature distribution during pultrusion of a Ø 10 mm profile based on a preheating temperature of 250 ◦ C, heating die temperature of 260 ◦ C, cooling die temperature
of 30 ◦ C, and pultrusion speeds of (a) 25 and (b) 100 mm/min.
Fig. 6. Temperature distribution of Ø 10 mm pultrudate simulated using preheating temperatures of (a) 250 ◦ C and (b) 230 ◦ C with a heating die temperature of 260 ◦ C, a
cooling die temperature of 30 ◦ C and a pulling speed of 100 mm/min.
6
M. Volk et al. Composites Part B 227 (2021) 109339
Fig. 8. Temperature distributions inside the cooling dies for pultrudate diameters of Ø 5–Ø 40 mm (a). Pulling speeds were fixed at 100 mm/min, and preheating and heating
temperatures were set to 245 ◦ C and 260 ◦ C, respectively. Time required to cool the core of a thermoplastic composite rod from 260 ◦ C to 80 ◦ C assuming a cooling die temperature
of 30 ◦ C (b).
Fig. 9. Total matrix flow through pultrusion die (a), matrix backflow relative to the fibre bed at 50 mm/min and Ø 10 mm pultrusion diameter (b).
7
M. Volk et al. Composites Part B 227 (2021) 109339
Fig. 10. Photographs of Ø 20 mm pultrusion setup during pultrusion of Ø 20 mm rod (a), Ø 40 and Ø 20 mm profiles made from amorphous PET, semi-crystalline PET (b).
Fig. 11. Tapered section of pultrusion die throughout pultrusion experiment with 50 mm/min pulling speed.
The metal pulling wire from Fig. 3 can be seen in Fig. 11(a) Attempts were made to track the resin backflow visually using
highlighted in red pulling in a bundle of commingled yarns through differently sized iron oxide and graphite particles as well as Astrazon
the transparent heating die. The images (a), (b) and (c) in Fig. 11 show BR200 colour dye to determine a flow distribution inside the die.
the development of a resin backflow front, highlighted in blue. The Unfortunately, the solid particles were quickly trapped by the fibres and
polymer volume displaced by the metal pulling wire creates the initial carried along as can be observed in Fig. 11(a), while the coloured dye
backflow. The shear forces created by pulling the yarns through the remained up to ten times longer in the tapered section than the glass
straight section of the die rapidly straighten any initially misaligned fibres as depicted in Fig. 11(e) and (f). While these observations did
fibres. Void extraction can be observed to occur towards the middle of not provide a measurable velocity field, it did confirm the presence of
the tapered die, with bubbles being pushed towards the die inlet. For resin backflow as found in the fluid flow simulation of Fig. 9. The yarn
speeds greater than 100 mm/min some of the bubbles were observed to bundles were observed to increase slightly in diameter upon entry into
be trapped by the fibres, rapidly decreasing in size and likely collapsing the tapered section. As no pretension is applied to the yarns, matrix
due to high matrix pressures at the transition between the tapered can fill the volume between yarns through backflow and capillary
and straight section of the heating die. The fibre straightening and pressure and increase the bundles’ diameter, potentially improving
void evacuation mechanisms observed through the transparent die impregnation.
suggest that the batch pultrusion process introduced here is not signif- The simulated temperature distributions were experimentally vali-
icantly disadvantaged compared to continuous pultrusion systems with dated for different temperature combinations, pultrusion speeds, and
extensive tensioning and fibre guidance systems. A video where GF- diameters using the batch pultrusion system. The results from the
PP commingled yarns are pultruded is accessible through a hyperlink numerical and experimental investigations are compared in Fig. 12
https://youtu.be/qKukzqm0J-I. which shows the temperature evolution at the centre of the selected
8
M. Volk et al. Composites Part B 227 (2021) 109339
Fig. 12. Validation of modelling results for Ø 10 mm at 50 and 100 mm/min at Fig. 14. Void content of different diameter pultruded rods for different pultrusion
preheating, heating and cooling temperature of 245 ◦ C, 260 ◦ C and 40 ◦ C and Ø 40 mm speeds.
at 25 mm/min at preheating, heating and cooling temperature of 220 ◦ C, 240 ◦ C and
30 ◦ C.
might be the main cause of void formation and not incomplete impreg-
nation. The fibre distribution is not completely homogeneous over the
rods during the pultrusion process. Note that the x-position has been
cross-section, indicating that the mingling quality plays an important
normalized to account for the differences in die length between the
role for the final consolidation quality.
Ø 10 and Ø 40 mm die. The temperature evolution over the heating
The results of the void content analysis over the whole diameter
and cooling die length shows good agreement between simulation and
and speed range investigated are summarized in Fig. 14. For all rod
experiment for all the rod dimensions tested even though the model was
diameters, the void content was below 1%, apart from the Ø 20 mm,
initially developed for Ø 10 mm rods. A slight mismatch between the
25 mm/min experiment, where the material degraded due to prolonged
simulated and measured temperatures was consistently found towards
preheating. Experimental results for the Ø 40 mm rod could only be
the end of the pultrusion die. This effect can be explained by shrinking performed for low speeds as space constraints limited the maximum
effects of the rod, not considered in the model, where the pultrudate size of the die. However, there is nothing to indicate that the high
detaches from the wall, decreasing the thermal transfer coefficient and quality of impregnation could not be maintained at higher pulling
causing higher temperatures than predicted. speeds for this profile size. To investigate the speed limits of this
pultrusion set-up, higher speed pultrusion experiments were performed
3.3. Material quality of pultruded profiles for Ø 10 mm profile with the results depicted in Fig. 15. To be able
to achieve pulling speeds above 200 mm/min while still applying
Designing the pultrusion dies and selecting the processing parame- reasonable pulling forces, the volume of material fed through the dies
ters according to the developed finite element models resulted in very was reduced to the extent that a void content of 2% would result from
good material quality. Fig. 13 shows a representative micrograph taken processing the material within the parameter window the dies were
from a Ø 40 mm rod at different magnifications, showing very low void designed for. Under these conditions, void content was observed to
content and good consolidation. The voids were located mainly inside increase linearly with speed until 400 mm/min after which the void
resin-rich areas towards the centre of the rod, indicating that shrinkage content drastically increased. This rapid increase in void content is
9
M. Volk et al. Composites Part B 227 (2021) 109339
Acknowledgements
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