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Composites Part A
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Keywords: Composite laminates are subjected to cryogenic temperatures in exposed aircraft structures during flight or
Composite in cryogenic tanks. The combination of cryogenic temperatures and high velocity impacts represents a threat
Impact to their integrity. This work investigates the behavior of carbon–epoxy laminates under high velocity impacts
X-ray micro-computed tomography
(from 70 to 500 m/s) at room and cryogenic (-150 ◦ C) temperatures and under two different plate orientations
Cryogenic
with respect to the projectile direction. The damage pattern of impacted specimens at low temperature,
revealed by C-scan and X-ray tomography, exhibits a higher density of fiber breaks and shear matrix cracks
which do not translate to a larger projected damaged area. The experimental analysis through interlaminar
shear strength tests and the calculation of ply thermal stresses exclude the association of this particular pattern
to damage mechanisms induced during the temperature decrease.
1. Introduction temperatures ranging from 20 to −150 ◦ C. For all the tested energies,
the coupons impacted at −150 ◦ C displayed a higher damage extension
Since the 1970s, the aerospace industry has made use of composite than those impacted at ambient temperature (damage area increased
materials in secondary and primary structures [1]. The integrity of by up to approximately 100%), which is in agreement with the trends
these structures under different loading cases is critical. Low and high reported by Kara et al. [6]. The effect of cryogenic temperature on
velocity impacts are one of the most dangerous threats, in particular the impact response of composites is attributed to: (i) thermal stresses,
when they occur in the direction perpendicular to the laminate plane. (ii) an alteration of the mechanical properties of the matrix, and/or
Induced damage can reduce the load bearing capacity of the structure, (iii) of the fiber–matrix interface. However there is no agreement on
leading to catastrophic failure in some cases. Drop tool impacts are the most important mechanism [5–14]. For example, Jia et al. [15]
the major concern for low velocity impacts, while bird strikes, ice subjected unidirectional carbon/epoxy coupons to static and dynamic
and metallic debris impacts are for high velocity ones. Drop tool im- three-point bending tests from −100 ◦ C up to 100 ◦ C. Their post-
pacts are always produced under controlled ambient conditions (during mortem photographs evidenced that the specimens tested at lower
maintenance operations or similar), while high velocity impacts occur temperatures developed several cracks following the 0◦ fiber orienta-
mainly during service time, and therefore, under low temperatures.
tion, which the authors explained in terms of the embrittlement of the
Consequently the damage caused is a result of a combination of impact
matrix (arguing that the effect of thermal stresses was secondary). Li
and cryogenic temperature.
et al. [12] also reported a higher number of cracks on quasi-isotropic
Not only are airplane structures (fuselage, wings, empennages, etc.)
tensile and bending specimens tested at cryogenic temperatures. Fol-
exposed to this combined threat, but lightweight fuel tanks containing
lowing a different reasoning Jia et al. [15], French et al. [2] and
liquids at cryogenic temperatures (cryotanks) can also suffer impacts
Kara et al. [6] observed that cooling carbon/epoxy laminates from
and lead to a safety and environmental issue [2]. Cryotanks are crucial
room temperature to approximately −200 ◦ C resulted in matrix cracks
for space transportation, and are expected to be a key driver in the
use of liquid hydrogen in clean aviation and terrestrial vehicles [3] to prior to mechanical loading (i.e., triggered by thermal stresses). Finally,
reduce the carbon footprint of these industries. regarding the impact properties of the neat epoxy matrix, He et al. [11]
Several authors have investigated the mechanical response of com- reported that decreasing the temperature of ‘‘Izod’’ epoxy coupons
posites under cryogenic temperatures [4]. Gómez-del Río et al. [5] from 20 to approximately −200 ◦ C diminished the impact strength by
impacted at low-velocity carbon/epoxy quasi-isotropic specimens at approximately 50%.
∗ Corresponding author.
E-mail address: jpernas@ing.uc3m.es (J. Pernas-Sánchez).
https://doi.org/10.1016/j.compositesa.2023.107456
Received 27 September 2022; Received in revised form 23 November 2022; Accepted 20 January 2023
Available online 2 February 2023
1359-835X/© 2023 The Author(s). 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/).
J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
To the authors’ knowledge, only a few studies have been focused Table 1
Summary of 𝜇CT specimens and pixel size selected.
on the effect cryogenic temperatures have on the high-velocity impact
response of carbon/epoxy laminates [8,9,16]. López-Puente et al. [9] Impact velocity (m/s) Temperature Impact orientation Pixel size (μm)
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J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
Fig. 1. Variation of the laminate elastic and thermal properties with temperature [29,30].
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J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
Fig. 2. Depth of damaged area obtained by ultrasonic inspection at ambient temperature for both normal and oblique (45◦ ) impacts. *Specimen at 132 m/s does not have a
squared shape because it was machined before C-scan inspection.
Fig. 3. Depth of delamination obtained by ultrasonic inspection at cryogenic temperatures for both normal and oblique (45◦ ) impacts. *Specimen at 493 m/s does not have squared
shape because it was machined before C-scan inspection.
previously reported three damage regimes depending on the impact surface (the split was visible to the naked eye). The delamination shape
velocity [9,22]: follows the typical peanut-shape for these materials [35]. With respect
to the impact angle, only minor differences can be observed regarding
• Impact velocity below the ballistic limit (plate not perforated). the damaged area, showing smaller values for the oblique impact
In this regime the damaged area increased linearly with impact conditions. Regarding the influence of temperature on the damaged
velocity. area, the results do not present a significant difference between the
• Velocity slightly above the ballistic limit (plate perforated near impacts at ambient temperatures and those performed at cryogenic
the ballistic limit). The maximum of the damage area is reached temperature.
in this regime. Figs. 4 to 7 summarize damage morphology under the impact
• Velocity above the ballistic limit. The damage area decreased location as observed by 𝜇CT. The 𝜇CT slices of the specimens subjected
mildly with higher impact velocities to normal impact demonstrate that, as impact velocity overcomes the
ballistic limit, the failure modes switched from predominantly delami-
Fig. 2 shows the C-scan damage of representative specimens for both nation to shear damage and plugging removal [9,22]. As can be seen in
normal and oblique impacts at ambient temperature for all regimes, Fig. 4, this applies to both ambient and cryogenic temperatures. At the
while Fig. 3 reproduces the equivalent images but for cryogenic condi- higher velocities, the specimens presented a cleaner perforation with
tions. Each image specifies the measured projected delaminated area. smaller associated delaminations.
The trend of the delamination area versus the impact velocity agrees Fig. 5 shows a detailed view of the specimens impacted at the lowest
with the three regimes described above. The maximum is always ob- velocities. Three types of failure mechanism can be discerned: (i) 45◦
tained for an impact velocity slightly above the ballistic limit. Re- crack induced by shear stresses (‘‘shear cracks’’ [24,26,36]), (ii) delam-
garding the shape of the damage, all specimens qualitatively featured ination and (iii) fiber failure. Regardless the testing temperature, both
a similar damage distribution: delamination distributed through the specimens developed shear cracks in every ply as well as delaminations
thickness of the coupons and a 45◦ fiber split in the non-impacted in all the interfaces between plies with dissimilar orientation (the
4
J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
Fig. 4. X-ray micro-computed tomography (𝜇CT) cross-sections of specimens impacted at ambient and cryogenic temperatures (a) Not perforated, (b) Perforated, close to the
ballistic limit and (c) Perforated, far from the ballistic limit. All impacts performed perpendicular to the laminated plane.
Fig. 5. Zoom of the X-ray micro-computed tomography (𝜇CT) cross-section for not-perforated cases (normal impact).
Fig. 6. Projected damage area of specimen impacted at 72 m/s normal impact and 80 m/s oblique impact under ambient temperature.
delaminations are probably triggered by the intersection of shear cracks Fig. 5); and (b) it also developed a high density of 45◦ ‘‘micro-cracks’’
in the surrounding layers [25,26]). Despite the qualitative similarities accompanying the main shear cracks (labeled as iv in Fig. 5(b)).
in terms of failure mechanisms, the differences between specimens A relevant observation is that these ‘‘micro-cracks’’ only developed
impacted at ambient (Fig. 5(a)) and cryogenic temperatures (Fig. 5(b)) within the region affected by the impact and not outside the boundaries
are two-fold: (a) the coupon impacted at the lower temperature fea- of the damaged area (as observed during careful inspection of the 𝜇CT
tured a significantly higher amount of fiber failure (labeled as iii in stacks).
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J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
Fig. 7. Zoom of the X-ray micro-computed tomography (𝜇CT) cross-section for not-perforated cases at (oblique 45◦ impacts).
Fig. 6 shows the projected delamination area obtained by 𝜇CT. The to the quasi-isotropic nature of the laminate, the stress state created by
most extended delaminations propagated in the central 90◦ /0◦ and the cooling is homogeneous in the plate. For the four ply orientations,
0◦ /90◦ interfaces, where the transverse shear stress distribution is the stress state is very similar with the in-plane normal stresses (𝜎11 and
close to maximum [37]. It is worth noting that, along with the shear 𝜎22 ) being the only significant stresses, while the rest could be neglected
cracks and delaminations, the specimens presented fiber failure con- (𝜎33 , 𝜏12 , 𝜏13 , 𝜏23 ∼ 0 MPa). The in-plane normal stresses as a function of
fined to underneath the center of impact (Fig. 5); careful observation the temperature are represented in Fig. 9. The figure illustrates how
of the entire 𝜇CT volume revealed that such fiber failure events are stresses change as the temperature decreases from the proposed free-
distributed across the thickness of the coupons. stress state (170 ◦ C) to the cryogenic temperature according to both
Regarding the effect of the impact orientation before the ballis- models. Stress along the fiber direction (𝜎11 ) are compressive while
tic limit, the specimens impacted at 45◦ qualitatively displayed the the perpendicular direction (𝜎22 ) shows a tensile state. This is caused
same damage mechanisms as those subjected to normal impacts: shear by the coefficient of thermal expansion along the fiber direction being
cracks, delamination and fiber failure. These findings hold for both smaller than in the perpendicular direction (𝛼1 < 𝛼2 ). However, the
ambient and cryogenic temperatures. The difference was that in the stress magnitude is similar in both directions due to the equilibrium
oblique impacts, the stress distribution induced a non-symmetrical achieved in the quasi-isotropic plate. The difference in the maximum
damage profile with respect to the impact center (Fig. 6). Additionally, stress proposed by both formulations is due to the fact that the CLT
the oblique impacts developed similar low temperature failure mech- does not take into account the variation of properties with tempera-
anisms than the normal impacts: a higher amount of fiber failure and ture. Nevertheless, both numerical and analytical methodologies reach
multiple shear ‘‘micro-cracks’’ (Fig. 7(b)). similar maximum values (≃ 60 MPa). Finally, it has to be remarked
that the stresses could be slightly overestimated since the stress-free
3.3. Interlaminar shear strength tests condition may be below glass temperature (170 ◦ C) as is proposed by
F. Lauri [42], which should lead to a even lower stress states (≤ 60
The purpose of the interlaminar shear strength experiments was MPa).
to evaluate whether the pre-cooling cycle to −150 ◦ C induces some
forms of damage that reduces the pristine material properties. Besides 4. Discussion
being widely used for material screening purposes [38,39], the ILSS
experiment was selected because the failure of quasi-isotropic coupons This research aims to shed light on the behavior of composites
depends on the development of shear cracks and delaminations [40]. subjected to high velocity impact under cryogenic temperatures. To
In other words, the ILSS experiments will provide quantitative insight this end, an extensive impact campaign varying the impact velocity,
into the effect that the pre-cooling cycle has on the matrix and interface the impact orientation and the temperature were performed.
properties. Figs. 2 and 3 demonstrated that, regardless the testing temperature
ILSS coupons were subjected to the same cooling cycle as the or the impact orientation, the projected damage area of all the batches
impact specimens. According to the work of French et al. [2] boundary qualitatively displays the same tendency. First, the damaged area in-
conditions have an important effect on the thermal stresses. Conse- creases linearly with the impact velocity until a maximum value, which
quently, we used the same boundary conditions for the plate used to is reached for velocities slightly above the ballistic limit. Then, the dam-
extract the ILSS coupons as in the impact tests. Fig. 8(a) presents the aged area decreases gently with enhanced impact velocity. 𝜇CT analysis
load–displacement curves of representative ILSS specimens (pristine (Fig. 4) shows that this behavior is related to a shift in the failure
and cooled) tested until failure. Both types of specimens qualitatively mechanism: from mainly delaminations to predominant shear damage,
displayed the same load response: linear growth followed by a non- fiber failure and plugging removal. Below the ballistic limit, plate
linear region and a catastrophic load drop (the non-linear part of the behavior is associated mainly with bending deformation, producing a
load response is typically attributed to the non-linear plastic response of similar failure pattern as in a low velocity impact test (drop-weight
the epoxy as well as to fiber rotation phenomena [41]). A similar failure tower test) [26,43]. As the velocity increases, fiber failures develops,
morphology was visually observed after the experiments: shear cracks promoting perforation. Beyond the ballistic limit, higher velocities
in the ±45◦ /0◦ plies and delamination spanning the interfaces between induce shear damage and plugging removal during the first instants of
off-axis plies. The similarities in terms of force response and damage the impact, generating a more localized plate bending deformation and
scenario resulted in similar strength values (Fig. 8(b)): 53.5 ± 4.6 and therefore smaller delaminations [9,22].
54.6 ± 3.8 MPa for the cooled and pristine specimens, respectively. The C-scan results demonstrated that, for impact velocities lying
Then it can be concluded that the cooling cycle does not cause shear under the ballistic regime, the specimens subjected to oblique impacts
cracking or other forms of damage in the laminate that could lead to display a lower damage area than those impacted at 0◦ (Fig. 2). The
differences in the force displacement history or the strength. reason behind this behavior is that the projectile normal force is the
main load component inducing damage and, for the same impact veloc-
3.4. Numerical model ity, this normal component is larger in the case of normal impacts [22].
Besides this, the coupons subjected to oblique impacts delayed the
To evaluate the stress state due to the cooling cycle we used a nu- perforation threshold when compared to the coupons subjected to
merical simulation and an analytical approximation based on CLT. Due normal impacts.
6
J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
Fig. 8. Interlaminar shear results from specimens subjected to cryogenic cycle and pristine situation.
7
J. Pernas-Sánchez et al. Composites Part A 168 (2023) 107456
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Acknowledgments
[19] Wang B, Xiong J, Wang X, Ma L, Zhang G-Q, Wu L-Z, Feng J-C. En-
ergy absorption efficiency of carbon fiber reinforced polymer laminates under
This paper is dedicated to the memory of our dear colleague high velocity impact. Mater Des 2013;50:140–8. http://dx.doi.org/10.1016/
and friend C.S. Lopes. The research leading to the developments de- j.matdes.2013.01.046, URL https://www.sciencedirect.com/science/article/pii/
S0261306913000691.
scribed was funded within the framework of the projects: Young
[20] Artero-Guerrero J, Pernas-Sánchez J, López-Puente J, Varas D. On the
researcher interdisciplinary projects from the University Carlos III of influence of filling level in CFRP aircraft fuel tank subjected to high
Madrid, Spain (call UC3M 2019–2020, project: UNION-CM-UC3M), velocity impacts. Compos Struct 2014;107:570–7. http://dx.doi.org/10.1016/
the Vicerrectorado de Política Científica project 2013/00413/004, j.compstruct.2013.08.036, URL https://www.sciencedirect.com/science/article/
pii/S0263822313004431.
2013/00413/003 and 2020/00123/001. The University of Girona also
[21] Varas D, Artero-Guerrero J, Pernas-Sánchez J, López-Puente J. Analysis of high
acknowledges the financial support of the Spanish Ministerio de In- velocity impacts of steel cylinders on thin carbon/epoxy woven laminates.
novación, Spain through the grant PID2021-126989OB-I00. This work Compos Struct 2013;95:623–9.
is framed in the collaboration between the Lightweight Structure Dy- [22] Pernas-Sánchez J, Artero-Guerrero J, Varas D, López-Puente J. Experimental
namic Group (University Carlos III of Madrid) and the AMADE team analysis of normal and oblique high velocity impacts on carbon/epoxy tape
laminates. Composite A 2014.
of the University of Girona. Funding for APC: Universidad Carlos III de [23] Kundu T, Ehsani M, Maslov K, Guo D. C-scan and L-scan generated images of
Madrid (Read & Publish Agreement CRUE-CSIC 2023). the concrete-GFRP composite interface. NDT E Int 1999;32:61–9. http://dx.doi.
org/10.1016/S0963-8695(98)00044-9.
[24] García-Rodríguez SM, Costa J, Singery V, Boada I, Mayugo JA. The effect
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