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Yalcinkaya 2019
Yalcinkaya 2019
Composites Part A
journal homepage: www.elsevier.com/locate/compositesa
a
University of Oklahoma, Aerospace and Mechanical Engineering, 865 Asp Ave., Norman, OK 73019, USA
b
Koç University, Mechanical Engineering Department, Rumelifeneri Yolu, Sariyer, 34450 Istanbul, Turkey
Keywords: Applying external pressure on the vacuum bag in heated-Vacuum Assisted Resin Transfer Molding (heated-
Liquid composite molding VARTM) is a new approach for manufacturing high quality composite laminates with minimal voids. The present
Microstructural analysis study focuses on the effects of external pressure and resin flushing on the microstructural features of the la-
Defects minates, including spatial variation and size distribution of the voids as well as the compaction of fiber tows. The
Mechanical properties
microstructural analysis performed on glass/epoxy composites reveal that external pressure reduces void content
and average void size, and leads to more uniform spatial distribution of voids. Significant increase in fiber
volume fraction from ∼50% up to ∼62% and a low void content of less than 1% are achieved by applying
modest gauge pressure levels up to 138 kPa on laminates with various thicknesses. The increase in fiber volume
fraction coupled with low void content improves the flexural properties as much as 20%, while the short-beam
shear strength of the laminates remains unchanged due to low void content in all laminates.
⁎
Corresponding author.
E-mail address: altan@ou.edu (M.C. Altan).
https://doi.org/10.1016/j.compositesa.2019.03.040
Received 11 December 2018; Received in revised form 10 March 2019; Accepted 25 March 2019
Available online 30 March 2019
1359-835X/ © 2019 Elsevier Ltd. All rights reserved.
M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
Fig. 1. Pressurized VARTM experimental set-up. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this
article.)
the lay-up have been proposed. These compaction methods include relative ease and low-cost tooling.
using an inflatable bladder [21,22], permanent magnets [23–27], or Hence, in this study, the following critical aspects of applying ex-
pressurized air [9,28,29]. ternal pressure in heated-VARTM are addressed:
High void content in the fabricated laminates can cause significant
reduction in the mechanical properties and also accelerate the en- • What are the discernable effects of external pressurization, either
vironmental aging by enhancing the moisture absorption [30,31]. In alone or when coupled with resin flushing, on the geometry, size,
liquid composite molding processes, voids are formed due to three and spatial distribution of voids throughout the laminate?
major phenomena: (i) bubbles already present in the resin resulting • What is the effect of pressure magnitude on the improvement of
from insufficient or no degassing before the infusion [32,33], (ii) vo- flexural properties, fiber volume fraction, and average void content?
latile release during curing reaction [34], and (iii) dual-scale flow • Are the fiber tows deformed due to pressurization, changing the
through porous fabric preform [35–37]. As widely discussed in various laminate microstructure?
studies, voids due to dual-scale flow can be formed in the tows (i.e., • Does the effect of pressure diminish with increased laminate thick-
intra-tow voids) when resin flow in between the tows is faster than the ness? Does the interlaminar shear strength improve due to decreased
flow inside the tows. On the other hand, larger voids can be formed in interlayer spacing under external pressure?
between the tows (i.e., inter-tow voids) when resin flow inside the tows
is faster than the flow in between the tows due to capillary effects 2. Experimental work
[35–37]. A few studies focused on adjusting the flow rate by controlling
the inlet pressure and reported that the impregnation velocity sig- 2.1. Materials used
nificantly affects the final void content of the laminates [38–40]. In
addition, process parameters such as vacuum pressure and mold tem- An 8-harness satin woven E-glass (Fibreglast) with an areal density
perature, resin bleeding, and placing a resistance to flow at the exit of 295 g/m2 was used as the fabric. The bulk fiber density, ρfiber was
have been reported to significantly affect the void content [1,3]. measured as 2.599 ± 0.012 g/cm3 with a gas pycnometer (AccuPyc II
However, in common applications of VARTM, formation of voids are 1340). EPON 862/Curing Agent W epoxy resin system was used as the
usually inevitable and therefore, mobilization and removal of voids are matrix material. The hardener and resin were mixed at 26.4:100
required to achieve laminates with low void content [41–43]. Various (hardener:resin) weight ratio for 15 min at 250 rpm prior to infusion.
studies have previously shown that voids may be mobilized towards the The mixture was degassed for 2 h to remove the air bubbles introduced
exit of the mold and could be removed by various approaches such as during mixing to prevent excessive voids in the final part. Density of the
vibrating the mold [44] or continuing resin flow after complete mold cured resin was measured as 1.195 g/cm3 by following ASTM D 792.
filling (a.k.a. resin flushing) [4,9].
Another drawback of VARTM is that the low-viscosity resin systems 2.2. Manufacturing of laminates
suitable for infusion at room temperature have often lower mechanical
properties and service temperatures compared to the resin systems Manufacturing of laminates involved two main stages: (1) mold
processed at higher temperatures [45]. Hence, the performance of most filling and (2) post-filling. During mold filling, liquid resin was infused
VARTM-manufactured parts is lower than that of autoclave molding or to impregnate the dry preform, which was placed on a heated alu-
RTM. Even though the higher performance resins are not commonly minum mold at 121 °C (see Fig. 1). After the preform was completely
used in VARTM process due to their high viscosity, heated-VARTM wetted, various combinations of resin flushing (F) and external pres-
could be a convenient method to reduce their viscosity and enable surization (P) were performed as post-filling actions.
vacuum infusion, which would significantly improve the mechanical In order to investigate the individual and coupled effects of resin
performance of composite laminates [46,47]. It has also been reported flushing and external pressurization on laminate properties and void
that low void content can be achieved by heated-VARTM [45,48], morphology, 6-ply laminates were manufactured by applying four dif-
making this process a viable choice for high performance applications. ferent combinations of resin flushing and external pressurization at the
Regarding the aforementioned advantages of heating, this study utilizes post-filling stage. Table 1 describes what these combinations are and
heated-VARTM to enable infusion of a high-viscosity resin suitable for how they are implemented during the manufacturing of laminates in
high performance applications. As an added benefit, reducing the detail. Flushing time and external pressure level, Pext, were selected as
viscosity of the resin will allow quick removal of excess resin when 30 min and 138 kPa (i.e., 20 psi), respectively. In all cases with external
external pressure is applied on the lay-up. This enhancement over the pressure, pressurization started 5 min after the mold was filled and
conventional VARTM can be achieved at modest pressure levels below continued until the part was completely cured. It was observed that
138 kPa and, thus, may be utilized for small to medium parts with applying external pressure during flushing not only resulted in a low
354
M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
Table 1
Fabrication scenarios (i.e., cases) to investigate the effect of applying various combinations of flushing and external pressure (i.e., 138 kPa gauge pressure) during the
post-filling stage. F: flushed, NF: non-flushed, P: externally pressurized, and NP: non-pressurized.
Case Post-filling actions
void content, but also significantly reduced the resin consumption after thickness cross-sections; (ii) average laminate thickness and fiber vo-
mold filling significantly by up to ∼85% compared to non-pressurized lume fraction; and (iii) flexural strength and stiffness.
fabrication.
Furthermore, 12- and 18-ply laminates were manufactured by
combining resin flushing and pressurization (F + P) as outlined in 3.1.1. Planar distribution of voids
Table 1. External pressure levels of Pext = 0, 34.5, 69, and 138 kPa (all In a number of studies, spatial distribution of voids was investigated
gauge pressure) were used to investigate the effect of external pressure by analyzing a set of samples that were often taken along the laminate
on the quality of thicker laminates. It should be noted that, when ex- (i.e., the flow direction, x-axis) under microscope [1,3,49,50] or using
ternal pressure was applied during resin flushing, excess resin was re- the resin burn-off method [1]. Even though these approaches have been
moved through both inlet and exit gates. commonly used in the literature, they usually require extensive analysis
For each combination of (i) resin flushing and external pressuriza- of high number of samples to acquire accurate information on spatial
tion, and (ii) number of plies and external pressure level, two distribution of voids. In fact, most of these studies focus only on
152 mm × 203 mm (6 in × 8 in) laminates were manufactured. All la- through-the-thickness cross sections of the laminate, and do not in-
minates were cured for 4 h at 121 °C after the impregnation of the vestigate the planar variations of the void content throughout the la-
preform. The exit gate was kept at ∼100 kPa of gauge vacuum pressure minate (on x-y plane). In this study, a new approach is introduced to
(i.e., ∼0 kPa absolute pressure) until the end of curing. quickly capture the planar distribution of voids throughout the entire
laminate surface by scanning the laminates using a high-resolution
flatbed scanner (Microtek ScanMaker 5900). For this purpose, 6-ply
3. Results and discussion laminates were fabricated to achieve semi-transparency through-the-
thickness, which provided a clear contrast between defect-free regions
3.1. Coupled effect of flushing and external pressure on laminate properties and voids. It is important to mention that as the laminate thickness is
increased (e.g. 12- and 18-ply), the transparency critically decreased
The preliminary results in our previous study showed that the resin and thus, the similar void analysis could not be performed.
flushing was essential for mobilization and removal of process-induced The four types of 6-ply laminates described in Table 1 were scanned
voids [9]. However, the coupled effect of flushing and external pressure (see Fig. 2) at a high-resolution of 2400 dpi (corresponding to a pixel
on laminate properties, including void size, geometry, and their spatial size of ∼11 µm × 11 µm. The scans were analyzed by using the image
variations were not investigated. Therefore, a detailed analysis is per- processing software, ImageJ. The gray-scale value of each pixel was
formed to identify the effect of applying various combinations of resin measured and plotted to identify the planar distribution of voids, and
flushing and external pressure (see Table 1) on the following properties also to illustrate the formation of highly nonuniform, localized void
of 6-ply laminates: (i) planar distribution of voids; (ii) areal number aggregates of various sizes as shown in Fig. 2. As the void occurrence
density, size, and aspect ratio of voids obtained from through-the- increased through the thickness, the transparency of the laminates at a
(a) NF + NP (b) F + NP
Exit side
Inlet side
(c) NF + P (d) F + P
x No-void
d More voids through the thickness
M
Fig. 2. Effect of flushing and external pressure on spatial distribution of voids. On the left side: scans of the laminates, on the right side: color maps of void
distribution. (a) Non-flushed and non-pressurized case (NF + NP), (b) Flushed and non-pressurized case (F + NP), (c) Non-flushed and pressurized case (NF + P),
and (d) Flushed and pressurized case (F + P). The color-maps illustrate the gray-values of pixels with voids and indicate how densely voids were localized through
the thickness. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
0.6 currence from 0.41 to 0.32, but also led to a more uniform void dis-
tribution along the laminates (compare black and red lines in Fig. 3).
Despite this significant improvement, removal of voids was limited and
0.4 a significantly low void occurrence could not be achieved by only ex-
ternal pressurization (NF + P). On the other hand, utilizing the resin
flushing in the absence of external pressure (F + NP) led to no visible
0.2
voids and the lowest void occurrence of zero (see Fig. 2(b)). However,
long flushing with no external pressure in F + NP yielded excess resin
0 intake which not only caused resin waste but also significantly de-
0 0.2 0.4 0.6 0.8 1 creased fiber volume fraction in the fabricated laminates.
Position along the laminate, x/L The best case was obtained by the combination of resin flushing and
external pressurization (F + P) where the average void occurrence was
Fig. 3. Effect of various combinations of flushing and external pressure on decreased to a very low value of 0.02 as Fig. 3 shows. F + P was ex-
distribution of voids along the x-axis (i.e., mold filling direction) of laminates. pected to yield high fiber volume fraction due to external pressure and
Void occurence indicates the ratio of number of pixels with voids to total low void content as a result of resin flushing. The void occurrence of
number of pixels across the width (i.e., y-axis) of laminates. Dashed lines il-
0.02 corresponds to a very small amount of voids which started to
lustrate the void occurrence averaged over the laminate length. (For inter-
appear during resin bleeding under external pressure. This was mainly
pretation of the references to color in this figure legend, the reader is referred to
the web version of this article.)
due to the growth of immobile microvoids that were entrapped in be-
tween the highly compacted fiber tows as a result of reduction in hy-
drostatic resin pressure. These immobile voids could not have been
removed with the flushed resin which was significantly reduced in size
particular location changed which resulted in pixels with lighter color due to lower permeability of the preform when external pressure was
(i.e., higher gray-scale value) as seen in the scans in Fig. 2(a), (c), and applied. After flushing was complete and excess resin was continued to
(d). On the other hand, the regions with no-voids had lower transpar- be bled out of the exit, these immobile voids grew due to reduction of
ency (i.e., the darker regions in scans) and thus, the corresponding resin pressure. Eventually, the high external pressure only compressed
pixels had lower gray-scale values. The color-maps in Fig. 2 illustrate the fabric plies and did not increase the resin pressure. Hence, the void
the regions with no-voids with white color, whereas the color ap- size could not be further reduced. Despite this minor increase in voids
proaches to red as the voids get denser through the thickness. No voids in F + P compared to F + NP, the F + P laminate will likely to yield the
were identified by the scan of F + NP laminate as shown in Fig. 2(b), best mechanical properties among the combinations of F and P due to
which confirms the favorable effect of resin flushing. significantly increased fiber volume fraction and very low void content.
In order to quantify the spatial distribution of voids along the la- However, the void content and morphology in fabricated laminates and
minates, the processed images in Fig. 2 were binarized, which resulted their mechanical properties should be investigated in detail to obtain a
in rows and columns of pixels with values of 0 or 1 (i.e., regions with comprehensive understanding of effect of flushing and pressurization
no-voids or voids, respectively). The pixel values were then averaged on the overall quality of the composites.
across the width of laminates (i.e., y-axis) to calculate the void occur-
rence at a particular distance from the inlet. The void occurrence cor- 3.1.2. Void morphology: size, areal number density, and aspect ratio
responds to the ratio of the number of pixels with voids to the total The effect of applying various combinations of flushing and external
number of pixels across the width of laminates (e.g. void occurrence is pressure on void morphology was also investigated by performing de-
zero at a particular x location if all pixels along y-direction are void- tailed microscopy examination on the through-the-thickness cross-sec-
free, and it is equal to one if they all have voids in them). It should be tions of the laminates. A 152 mm (6 in) long sample along the filling
pointed out that the void occurrence analysis was performed to char- direction (i.e., x-direction) was taken from each laminate. Every single
acterize the spatial distribution of voids throughout the laminate, and void identifiable at 50-500X magnification on the entire through-the-
the actual void volume fraction of laminates was not quantified with thickness cross-section of these samples was captured with a MEIJI light
this method. microscope and (i) its equivalent diameter, Deq (i.e., the diameter of the
Fig. 3 demonstrates the void occurrence along the fill direction (i.e., circle with the same area of the void) and (ii) aspect ratio (i.e., the ratio
x-axis) in laminates fabricated by applying various combinations of of major to minor axes of a fitted ellipse on the void circumference)
flushing and external pressure. The red line in Fig. 3 shows that in were calculated using ImageJ software. It should be noted that no voids
NF + NP laminates (see Fig. 2(a)), voids were mostly concentrated in the fiber tows (i.e., intra-tow voids) were seen among the examined
around both the inlet and the exit sides (i.e., x/L < 0.2 and x/ laminates.
L > 0.6). The high void occurrence (up to ∼0.7 in Fig. 3) at the inlet The results given in Table 2 show that the areal number density of
side was possibly due to the high resin velocity at or near x/L = 0. voids (i.e., number of voids per unit area of samples) was significantly
Some of these voids were mobilized towards the exit with the advan- reduced by resin flushing. Comparison of the areal number density of
cing flow-front during filling and also by the resin flow after the inlet voids in NF + NP and F + NP laminates (i.e., 2.69 and 0 voids/mm2,
was closed (i.e., resin bleeding), which might have caused an increase respectively) reveals that voids were removed with the resin outflow
in the void occurrence towards the exit. However, these mobilized voids during flushing. It should be noted that the areal number density of
could not be removed due to the limited amount of resin flow during voids in F + NP was calculated as zero due to no voids being observed
resin bleeding since the inlet was closed. It should be noted that the in the examined cross-sections of the F + NP laminates even at the
voids became visible during resin bleeding which indicated that the highest magnification of 500X. The advantage of flushing can also be
reduction in resin pressure due to resin bleeding led to void formation seen in the presence of external pressure when NF + P and F + P la-
and growth [51]. Therefore, voids should be mobilized and removed minates are compared. In F + P case, 80% reduction in areal number
with the resin outflow before resin pressure critically decreases during density of voids was achieved compared to NF + P case.
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
Table 2
Effect of applying various combinations of flushing and external pressurization on the laminate properties. F: flushed, NF: non-flushed, P: externally pressurized, and
NP: non-pressurized.
Case Average thickness, h Fiber volume Void content, Vv Areal number Equivalent void Void aspect ratio Flexural Flexural stiffness,
[mm] fraction, Vf [%] [%] density, [voids/ diameter, Deq [μm] strength, σ E [GPa]
mm2] [MPa]
NF + NP 1.246 ± 0.005 57 ± 0.2 2.4 ± 0.5 2.69 169 ± 8 4.97 ± 0.22 629 ± 26 26.4 ± 0.4
F + NP 1.401 ± 0.003 50 ± 0.2 0.35 ± 0.0 – – – 650 ± 6 24.3 ± 0.3
NF + P 1.106 ± 0.004 60 ± 0.2 1.4 ± 0.2 2.11 108 ± 7 5.23 ± 0.33 730 ± 12 30.6 ± 0.6
F+P 1.137 ± 0.003 62 ± 0.2 0.86 ± 0.2 0.42 110 ± 15 3.93 ± 0.43 736 ± 27 29.1 ± 0.6
50 60
a NF+NP NF+P F+P 55
b NF+NP NF+P F+P
45
50
40
45
35
40
Frequency [%]
Frequency [%]
30 35
25 30
20 25
20
15
15
10
10
5 5
0 0
0-50 50-100 100-150 150-200 200-250 250-300 300-350 >350 <2
0-2 2-4 4-6 6-8 8-10 10-12 12-14 >14
Equivalent diameter, Deq [μm] Aspect ratio
Fig. 4. Distribution of (a) void size and (b) aspect ratio when various combinations of flushing and external pressure were applied.
In addition, Table 2 shows that the external pressure led to a sig- The effect of voids on mechanical properties can vary for different types
nificant decrease in average void size (i.e., Deq) from 169 μm for of fabrics and impregnation schemes. For example, if a distribution
NF + NP to 108 μm for NF + P laminates. It is also observed that ex- medium is used over much of the laminate surface to speed up the
ternal pressure not only reduced the size but also the areal number impregnation, the formation and morphology of voids can be sig-
density of voids, which was 22% lower in NF + P than NF + NP. As a nificantly affected.
result, a significant reduction in void content by applying external
pressure was achieved. Hence, notable improvement of the laminate 3.1.3. Average thickness, fiber volume fraction, void content, and flexural
quality is expected when both resin flushing and external pressure are properties of the laminates
applied, since laminates with fewer voids and higher fiber content have Thickness of the laminates was measured at a grid of 35 equally
better mechanical performance. spaced locations using a micrometer. Fiber volume fraction, Vf and void
The frequency distributions of size and aspect ratio of voids are content, Vv of laminates were determined by conducting resin burn-off
depicted in Fig. 4(a) and (b), respectively to give a more detailed method according to ASTM D 3171 on 3 samples from each laminate
analysis on the effect of external pressure on void morphology. Fig. 4(a) (i.e., 6 samples for each fabrication scenario) with planar dimensions of
clearly demonstrates that when external pressure was applied (i.e., 13 mm × 51 mm (0.5 in × 2 in). In addition, flexural testing of 16
NF + P and F + P cases), frequency of large voids decreased sig- samples for each case was performed at a span to thickness ratio of 24
nificantly and almost 45% of the voids had an equivalent diameter of by following ASTM D 790. The results are tabulated in Table 2 with a
50–100 μm. On the other hand, the void size distribution in NF + NP 95% confidence interval to characterize the variation in the experi-
case showed that very large voids with more than 350 μm equivalent mental data.
diameter could be present in the part, which could create weak spots As shown in Table 2, resin flushing caused a significant increase in
and micro-cracks, leading to premature delamination and significant laminate thickness in non-pressurized cases (i.e., NF + NP and F + NP),
decrease in the mechanical properties. In addition, resin flushing re- which decreased the fiber volume fraction due to additional resin in-
sulted in removal of voids larger than 300 μm and with aspect ratio take. However, higher flexural strength was achieved in F + NP case
higher than 8 whereas, voids with large dimensions and very high as- due to the decrease in void content from 2.4 to 0.35% with resin
pect ratio were entrapped in non-flushed laminates (i.e., NF + NP and flushing. The higher variation of flexural strength of ± 26 MPa for
NF + P cases). Hence, notable improvement of flexural properties in NF + NP laminates compared to ± 6 MPa for the F + NP laminates
F + P case compared to NF + NP and NF + P cases was expected. The could be correlated to the higher variation in void occurrence (i.e.,
statistical distribution of void size and aspect ratio as given in Fig. 4 higher spatial variation in void content) shown in Fig. 3. On the other
could be useful when investigating the effect of voids on the mechanical hand, external pressurization resulted in substantial decrease in average
properties of composites particularly by using micromechanical models thickness of laminates, which significantly increased fiber volume
[52]. In various studies [52–54], the effect of void geometry was ac- fraction, Vf, up to 62% and thus, improved flexural strength, σ, and
counted for in micromechanical models and void morphology was modulus, E, up to 736 MPa and 30.6 GPa, respectively, compared to
shown to have a detrimental effect on the elastic moduli of composites. Vf = 57%, σ = 629 MPa, and E = 26.4 GPa in NF + NP case. Although,
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
4.5 64
a 6 plies b
4.0 62
12 plies
58
3.0
56
2.5
54
2.0
52 6 plies
1.5 12 plies
50
18 plies
1.0 48
0 20 40 60 80 100 120 140 0 20 40 60 80 100 120 140
External pressure, Pext [kPa] External pressure, Pext [kPa]
0.24
c 6 plies
0.23 12 plies
Thickness per ply, h/N [mm]
18 plies
0.22
0.21
0.20
0.19
0.18
0 20 40 60 80 100 120 140
External pressure, Pext [kPa]
Fig. 5. Effect of external pressure on (a) thickness and (b) fiber volume fraction, and (c) per-ply thickness of 6-, 12-, and 18-ply laminates.
NF + P and F + P cases resulted in similar average flexural properties, 12-, and 18-ply laminates at a certain Pext was similar, indicating that
the decrease in void content due to flushing improved the flexural the removal of excess resin and reduction of laminate thickness were
strength slightly from 730 to 736 MPa. These outcomes emphasized the effectively performed even at increased laminate thicknesses (i.e.,
importance of applying resin flushing and external pressure together higher number of plies). Additionally, the similar per-ply thicknesses
(i.e., F + P case) to achieve superior laminate properties with low void indicated that the number of plies would have almost a negligible effect
content below 1% and high fiber volume fraction up to 62%. Moreover, on the consolidation behavior of the laminates. This could be due to the
large and high-aspect ratio voids, which could be detrimental in me- reduced effect of nesting on thickness at increased number of plies as
chanical properties of composite laminates, were significantly reduced reported in the previous studies [55,56].
in the F + P case. Therefore, all subsequent 6-, 12- and 18-ply laminates Fig. 5(b) shows the effect of different pressure levels on fiber volume
used in this study were manufactured by combining the resin flushing fraction, Vf, for 6-, 12-, and 18-ply laminates. It is seen that Vf of 6-, 12-
and external pressurization (i.e., F + P case). and 18-ply laminates at Pext = 0 kPa was increased from approximately
50 to more than 61% at Pext = 138 kPa. As expected, the significant
3.2. Effect of laminate thickness on the consolidation, fiber volume fraction, increase in Vf occurred due to the removal of excess resin and further
and void content compaction of the impregnated preform under increased compaction
pressure, Pc (i.e., Pc = (Patm − Pvent) + Pext ≈ 238 kPa), which was not
The consolidation of laminates made of 6, 12 and 18 plies was in- possible at the highest available compaction pressure (i.e.,
vestigated by analyzing the average laminate thickness, fiber volume Pc = (Patm − Pvent) ≈ 100 kPa) in conventional VARTM, when vent
fraction, and per-ply thickness as shown in Fig. 5. It should be noted pressure, Pvent is around absolute vacuum and Patm ≈ 100 kPa. More-
that the error bars showing the 95% confidence intervals are barely over, a similar improvement in fiber volume fraction is expected to be
noticeable in Fig. 5(a–c) due to almost uniform thickness distribution. achieved by applying external pressure at lower process temperatures
Fig. 5 shows that at Pext = 138 kPa, a significant thickness decrease [28].
of 19 and 17% in 12- and 18-ply laminates was achieved, respectively. Fig. 6 shows the void content, Vv, measured from 6 samples for 6-,
For 6-ply laminates, this was reported as 19% decrease in our previous 12- and 18-ply laminates. Compared to the non-flushed cases, 30-min
study [9]. Moreover, Fig. 5(c) shows that the per-ply thickness values flushing applied in all cases shown in Fig. 6 seems to help reduce the
(i.e., average laminate thickness divided by the number of plies) of 6-, overall void volume fraction for all laminates, regardless of the
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1.2
3.3. Microstructural analysis of 6-, 12-, and 18-ply laminates
6 plies 12 plies 18 plies
1 To better ascertain the effect of external pressure on the micro-
structural features of the laminates, a detailed microscopy analysis that
includes the characterization of tow deformation was carried out. The
Void content, Vv [%]
0.8
qualitative observations from the microscopy images coupled with
quantitative analysis of void size and shape distributions as well as tow
0.6 deformation could reveal unique microstructural features, which might
be observed only in the pressurized VARTM processes.
Fig. 7(a–c) reveal that voids were seldom seen and most of the
0.4
sample cross-sections were void free, especially at lower pressure levels,
which agreed well with the void occurrence analysis and resin burn-off
0.2 tests. However, some voids were occasionally seen at the inter-tow
regions of laminates fabricated at high levels of external pressure as
0 seen in Fig. 7(d). This implied that while voids were mobilized and
0 (i.e., VARTM) 34.5 69 138 removed with the flushed resin, some voids were restrained in between
External pressure, Pext [kPa] the compressed fiber tows. Fig. 8(a) and (b) shows close-up micro-
Fig. 6. Comparison of the void content of 6-, 12-, and 18-ply laminates man- graphs that elaborate these observations by showing the clear contrast
ufactured under various external pressure levels. Resin flushing was applied for between the voids observed in a non-pressurized and pressurized
30 min in all cases. (Pext = 69 kPa) 18-ply laminate, respectively. Fig. 8(a) depicts the only
void along the whole 152 mm microscopy sample of a non-pressurized
laminate and indicates that the large inter-tow regions enhanced the
laminate thickness. The minor increase in Vv in all 6-, 12-, and 18-ply mobility of voids. Additionally, due to lower compaction pressure, a
laminates with the increase in the level of external pressure could be low void aspect ratio is observed in Fig. 8(a). On the other hand, the
caused by the entrapment of mobilized voids in between the compacted void in Fig. 8(b) was compressed and elongated due to reduced inter-
fabric layers during pressurization. However, it is clearly seen that the tow gap especially at Pext = 138 kPa.
average Vv of all laminates was below 1% at all Pext levels. Therefore, Other interesting observations regarding the void shape and loca-
the possible negative effect of slight increase in void content on me- tion through the thickness of laminates include voids with tortuous
chanical properties was expected to be minor or unnoticeable. More- morphology and intra-tow voids seen in warp tows. Fig. 9(a) depicts
over, the substantial increase in fiber volume fraction due to the applied that larger voids were broken up into smaller ones at high external
pressure would have a more dominant effect on the mechanical prop- pressure, resulting in clusters of more tortuous voids, mostly extending
erties and fully compensate the detrimental effects of the slightly in- along a horizontal plane. In addition, an extensive inspection of nu-
creased void content. merous micrographs revealed that at certain locations, minor intra-tow
Fig. 7. Micrographs from 12-ply laminates: (a) a void free section from a non-pressurized and (b) a pressurized (Pext = 138 kPa) laminate. (c) A perfectly wetted void-
free tow, and (d) a region with localized, inter-layer void clusters (Pext = 138 kPa).
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
Weft tow
Resin
Intra-tow voids
Fig. 9. Micrographs demonstrating (a) several tortuous voids in a 12-ply pressurized laminate (Pext = 138 kPa) and (b) intra-tow voids in warp tows due to branching
of inter-tow voids at high external pressure.
60 60
a b
6 plies 12 plies 18 plies 6 plies 12 plies 18 plies
50 50
40 40
Frequency [%]
Frequency [%]
30 30
20 20
10 10
0 0
0-50 50-100 100-150 150-200 200-250 250-300 300-350 >350 <2
0-2 2-4 4-6 6-8 8-10 10-12 12-14 >14
Equivalent diameter, Deq [μm] Aspect ratio
Fig. 10. Microscopy analysis of captured voids in laminates manufactured under Pext = 138 kPa: (a) equivalent diameter and (b) aspect ratio of the voids.
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
90 90 90
0.75 0.75 0.75
80 80 80
Fig. 12. Change in tow height and cross-sectional area with external pressure in (a) 6-, (b) 12- and (c) 18-ply laminates. Tow cross-sectional area was normalized by
the average tow area of VARTM laminates and illustrated with the black squares (values appear on the right vertical axis).
1.20 1.25
a 6 plies 12 plies 18 plies b 6 plies 12 plies 18 plies
1.20
1.15
Normalized flexural strength
1.15
1.10
1.10
1.05
1.05
1.00
1.00
0.95
0.95
0.90 0.90
0 (i.e., VARTM) 34.5 69 138 0 (i.e., VARTM) 34.5 69 138
External pressure, Pext [kPa] External pressure, Pext [kPa]
Fig. 13. Effect of external pressure on the normalized (a) flexural strength and (b) flexural stiffness of 6-, 12-, and 18-ply laminates.
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65 65
a b
55 55
50 50
45 45
40 40
0 (i.e., VARTM) 34.5 69 138 0 (i.e., VARTM) 34.5 69 138
External pressure, Pext [kPa] External pressure, P ext [kPa]
Fig. 14. Short-beam shear strength of (a) 12- and (b) 18-ply laminates manufactured by applying various levels of external pressure.
analyzed and it was observed that external pressure did not have an Hence, only 12- and 18-ply laminates were tested to investigate the
influence on the width of tows, but significantly decreased the area of effect of slight increase in void content on SBS. Six samples from each
tows (shown with black squares in Fig. 12), which was due to the re- laminate were tested at a span to thickness ratio of 4:1. Fig. 14 shows
duction in tow height. The reduction in tow area implied that the in- that SBS of laminates was affected neither by the increase in fiber vo-
crease in Vf was not only due to removal of excess resin in the inter-tow lume fraction nor by the decrease in void content. These results were in
regions and nesting of fabric layers, but also due to the decrease in good agreement with Ref. [65] that showed, for Vf from 40 to 60%, SBS
intra-tow space in between individual fibers. was not influenced by the Vf, since the shear fracture occurred in the
matrix. Furthermore, previous studies [63,64] demonstrated that void
3.4. Flexural and interlaminar properties of 6-, 12-, and 18-ply laminates content below the critical value of ∼1% did not significantly affect the
shear strength, whereas the shear strength decreased exponentially at
The effect of external pressure on flexural properties of laminates is high void content. Therefore, it could be concluded that similar SBS
demonstrated in Fig. 13, which clearly depicts that, even at a low ex- could be achieved at various laminate thicknesses and external pressure
ternal pressure level of 34.5 kPa, flexural strength and stiffness im- levels due to low void content.
proved significantly in all laminates. The results are presented as nor-
malized flexural strength and stiffness with respect to the laminates 4. Conclusion
fabricated by conventional VARTM without external pressure. The in-
crease in flexural strength at Pext = 138 kPa was ∼13, ∼7, and ∼11% The effect of applying external pressure on the lay-up in heated-
in 6-, 12- and 18-ply laminates, respectively. The average flexural VARTM was investigated to enhance mechanical properties and overall
strength at Pext = 0, 34.5, 69, and 138 kPa were (i) 650, 695, 709, and quality of the composite laminates of various thicknesses. This was
736 MPa for 6-ply; (ii) 606, 632, 639, and 648 MPa for 12-ply; and (iii) demonstrated by: (i) identifying the individual as well as synergistic
594, 640, 607, and 658 MPa for 18-ply laminates. Although, flexural effects of external pressure and resin flushing, and (ii) analyzing the
strength increased with external pressure in all laminates, the level of changes in laminate thickness, microstructural features, and flexural
increase was slightly different in 6-, 12-, and 18-ply laminates, possibly and interlaminar properties of 6-, 12-, and 18-ply, satin-weave glass/
due to the inherent variations in laminate fabrication, and presence of epoxy laminates.
voids with various morphologies affecting the flexural strength. Despite It was shown that external pressurization alone decreased the
the small effects of voids expected at low void content [30,58], the void average void content from 2.4 to 1.4% when resin flushing was not
morphology might be an important factor affecting the mechanical applied. Coupling external pressure and resin flushing further reduced
properties [59,60]. The relatively modest improvement in strength for the void content to 0.86% and yielded a more uniform spatial dis-
12- and 18-ply laminates could be correlated to the presence of higher tribution of voids, while achieving high fiber content of approximately
aspect ratio voids and formation of localized void clusters which could 62% due to higher degree of compaction with external pressure.
contribute to the initiation and progression of micro-cracks [59,61]. On Applying external pressure was shown to reduce the void size while
the other hand, Fig. 13(b) shows that the increase in flexural stiffness resin flushing helped removal of high-aspect-ratio voids in pressurized
(i.e., from 24 GPa to above 28 GPa, representing more than 15% in- laminates. In addition, both flexural strength and stiffness of laminates
crease) was more consistent and followed an expected trend in all 6-, manufactured by applying flushing and external pressure together were
12-, and 18-ply laminates and further confirms the minor effect of voids substantially improved. Therefore, applying resin flushing and external
on the flexural stiffness [62]. pressurization together would be most effective for improving laminate
To further investigate whether the small amount of voids formed at quality.
higher external pressures affected the laminate quality, short-beam The analysis of the 6-, 12-, and 18-ply laminates clearly showed that
shear strength (SBS) of fabricated laminates were determined. SBS is the similar levels of thickness reduction and fiber volume fraction in-
sensitive to void content and can significantly deteriorate if the void crease could be achieved by the pressurization regardless of the lami-
content is above a critical level [63,64]. The SBS of the 6-ply laminates nate thickness. The further analysis of the laminate compaction re-
could not be tested, since the thickness of the specimens did not satisfy vealed that the thickness reduction was not only governed by the
the requirements of the short-beam testing standard (ASTM D 2344). nesting of fabric layers, but also by the consolidation of individual fiber
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M.A. Yalcinkaya, et al. Composites Part A 121 (2019) 353–364
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