Engineering Failure Analysis 79 (2017) 342–350

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Engineering Failure Analysis

journal homepage: www.elsevier.com/locate/engfailanal

A fractographic study on the effects of hygrothermal conditioning

on carbon fiber/epoxy laminates submitted to axial compression
MARK
C.V. Opelta,⁎, J.M.F. Paivab, G.M. Cândidoc, M.C. Rezendea,c
a
Department of Aeronautical and Mechanical Engineering, Technological Institute of Aeronautics, Praça Marechal Eduardo Gomes 50, 12228-900
São José dos Campos, SP, Brazil
b
Department of Production Engineering, Federal University of São Carlos, UFSCar-Sorocaba Rodovia João Leme dos Santos (SP-264), Km 110,
18052-780 Sorocaba, SP, Brazil
c
Institute of Science and Technology, Federal University of São Paulo, UNIFESP Rua Talim 330, 12231-280 São José dos Campos, SP, Brazil

AR TI CLE I NF O AB S T R A CT

Keywords: This paper is part of a series of fractographic studies on fiber-reinforced polymer composites
Composites submitted to compression, which attempts to fill the gap in the composite failure analysis. Here,
Fractography the effect of the hygrothermal conditioning is assessed for composite laminates manufactured
Failure modes from a carbon fiber/epoxy resin prepregs, which used plain weave fiber arrangement. The
Aging
laminate was trimmed into compression test specimens, according to the ASTM D3410 standard.
Failure analysis
After the test, the aspects of the failure were investigated using a scanning electron microscope,
so the compression failure modes could be identified. The fractographic analysis indicates that
the lower compressive strength of the conditioned specimens was caused by a decrease in the
stiffness of the polymer matrix, due to the plasticizing effect of the moisture exposure.

1. Introduction

Commercial aircraft are exposed to worldwide environmental conditions, which create some concern about the influence of
operational and ground-based environment on the durability of the materials and structures used [1]. The primary and secondary
composite structures used in aircraft usually experience cycles of absorption and desorption of water, and this type of non-mechanical
fatigue is considered to be related to long-term durability of composites. In fact, the combination of thermal (generated during
cooling) and hygrothermal stresses may be sufficiently large to influence the failure of composite laminates [2].
According to Tsenoglou and coworkers [3], the moisture absorption, by the polymer matrices commonly used in structural
composites, influence not only the mechanical properties, but also thermal and dielectric properties. However, the degrading effect of
moisture absorption by the matrix is only secondary when compared to the damage of the fiber/matrix interface, since the exposure
to moisture may promote microcracks in the interfacial region [3]. On the other hand, the absorbed moisture increases the free
volume of the polymer molecules, which promotes a drop in the glass transition temperature of the polymer matrix [2,4]. This
process has a plasticizing effect that induces a decrease of the stiffness in addition to an increase of the fracture toughness of the
composite. Furthermore, the continued exposition to high temperature and moisture promotes a relaxation of the residual stresses of
the polymer matrix, which end up in some recovering of the reduced mechanical properties [5].
Although is difficult to predict the exact influence of the environmental conditioning, it is possible to say that the matrix material
will be deeply affected. Thus, when the behavior of the composite is dominated by the fiber properties, the influence may not be so

⁎
Corresponding author.
E-mail address: cvopelt@gmail.com (C.V. Opelt).

http://dx.doi.org/10.1016/j.engfailanal.2017.05.006
Received 16 May 2016; Received in revised form 7 February 2017; Accepted 1 May 2017
Available online 02 May 2017
1350-6307/ © 2017 Elsevier Ltd. All rights reserved.
C.V. Opelt et al. Engineering Failure Analysis 79 (2017) 342–350

Fig. 1. Compression failure modes of fiber-reinforced polymer composites [13].

evident. However, cases in which the behavior is dominated by the matrix properties, such as compressive and interlaminar shear
strength, are highly affected [1]. Regarding the compressive strength, the literature indicates that it can be 60% lesser than the tensile
strength [6], and the possible exposure to high temperature-moisture environments only evidences the importance of the knowledge
of the compressive behavior. Purslow and Potter [7], in their work involving the effect of the environmental conditioning on the
compressive strength of notched specimens, reported a major decrease in compressive strength (approximately 40%) when the
specimens were tested in a hot-wet condition (120 °C and ~1% moisture absorbed). Associated to this decrease, the authors observed
that the fracture propagation left the fiber grooves visible, which indicates that the environmental conditioning degraded the fiber/
matrix interface. This kind of degradation promotes the instability of the fibers during the load application which, according also to
Potter and Purslow [8], governs the compressive strength of notched multidirectional CFRP.
To further hinder the understanding of the compressive behavior, the failure of fiber-reinforced polymer composites may occur by
a number of different modes [9], and for each one there is a sequence of events involved in the fracture propagation. This analysis has
a significant importance, since it can be used to improve the design of composite structures submitted to compressive loads [10].
There are some works in the literature dedicated to study the failure modes of fiber composites submitted to compressive loads
[6,10,11], however the authors do not agree about the existing failure modes as well as the sequence of events that lead to failure.
This is reflected in the lack of knowledge on the mechanisms that lead to compression failure of composite materials which, according
to Pinho and coworkers [12], was evident after the World Wide Failure Analysis.
In this context, our research group developed a classification (as seen in Fig. 1) for the compression failure modes [13,14] that was
based on the cases reported in the literature [6,10,11,15,16], but that can also be used in the analysis of more complex fiber
architectures, e.g. recycled composites [17], stitched woven composites [18] or 3D woven composites [19]. Here in this paper, we are
dedicated to apply this classification to a plain weave fabric carbon fiber/epoxy laminate, as a way to investigate the effects of the
environmental conditioning from a fractographic point of view.

2. Experimental

The composite laminate studied here was manufactured from a carbon fiber/epoxy resin prepreg (HexPly F155, Hexcel
Composites), in which the fiber arrangement used was a plain weave fabric. The epoxy resin matrix used in the prepreg is a first
generation epoxy resin, therefore with a low content of toughening agent. According to Johnston [20], the toughening agent is a
carboxy-terminated butadiene acrylonitrile (a content of nearly 6%), which forms a rubbery second phase. The cure of the composite
laminate was carried at an autoclave using vacuum bag and a metal mold. The pressure in the autoclave was 0.7 MPa following a
temperature profile with a maximum of 121 °C. After the cure the laminates presented a volume fraction of carbon fibers of
approximately 60%.
After the cure, the laminate was bonded to fiberglass laminates (which were used as tabs) and trimmed into compression test
specimens, according to the ASTM D3410 standard. The compression test was carried out in a universal testing machine, using an
IITRI fixture with crosshead speed of 1.27 mm/min, at room temperature. Prior to the test, half of the specimens were submitted to
environmental conditioning in a hygrothermal chamber, in accordance to ASTM D5229 standard. More details about the specimen
preparation and testing can be consulted in the paper by Paiva and coworkers [21], where the characterization of this laminate is
presented.
As for the failure analysis of the specimens, it was conducted in a scanning electron microscope (TESCAN - Vega 3 XMU), mainly
at low magnifications. This analysis is comprised by the failure modes identification and by the analysis of the internal microstructure
of the laminates, as shown in Fig. 2. Here it is necessary to say that during the compression test a specimen is considered to have
failed when it loses its load bearing capacity. This failure may occur within the specimen by a number of different reasons (e.g. fiber
fracture or a delamination that propagates), and is not easily identified. To highlight the compressive behavior of the laminate, the

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Fig. 2. Representation of the analysis of the (a) failure modes and of the (b) internal microstructure of compression test specimens [13].

application of the load was continued even after the failure of the specimen, so the fracture could propagate throughout the specimen
and its aspects could be identified. This propagation occurs according to the laminate properties and so can be used to determine the
behavior of the laminate, although some authors prefer to refer to this as a post-failure mode [16].

3. Results and discussion

The results for compressive strengths are 533.6 ± 29.5 MPa and 492.6 ± 55.0 MPa, respectively, for the non-conditioned and
for the conditioned specimens. In a previous work of our research group [21] this decrease in the compressive strength was attributed
to the loss of stiffness by the polymeric matrix material. As before mentioned, when polymers absorb water they tend to swell and this
mechanism increase the free volume of the polymer chains. This phenomenon may result in a polymer with a higher toughness, but
with a lower stiffness. By means of visual inspection Paiva and coworkers [21] also indicated that all the specimens, independent if
were conditioned or not, fail by shear in compression, although the conditioned specimens appears to had less severe failures. This
kind of failure mode is commonly reported in the literature and reflects the compression loading leading to a minor degree of shear
loading during the fracture process [22]. According to Odom and Adams [11], the through-the-thickness shear failures occur in the
absence of an adequate lateral stability and for this reason the specimens would show some degree of buckling. Another possibility is
the formation of shear planes (in the thickness direction), during the compressive test of the specimens. These shear planes could be
promoted by numerous factors as the coalescence of microcracks in brittle solids (e.g. most of thermoset matrices) [23], stress
concentrations (e.g. surface finishing) [24,25] and the fiber waviness [26], the last being the dominant in the case of textile laminate
composites. Concerning the fracture aspects, this kind of failure can be identified by the angled fracture (in the thickness direction)
usually near the tabs [11], in addition to a large number of debris and some flexural damages on the fracture surface, due to the
sliding of the mating surfaces of the specimen [10,22].
Fig. 3 presents the failure modes for three of the specimens tested without environmental conditioning. To assess whether the
fracture propagation was irregular in the width direction, i.e. if different failure modes occurred in each side of the specimen, both
sides of the specimens are presented. One can see that all specimens in Fig. 3 showed through-the-thickness shear failures, as reported
by Paiva et al. [21], although in Specimen C a layer appears to been crushed during the test and then promoted the propagation of a
large delamination. Besides that, it is possible to see, mainly in the Specimens A and B, that both sides show different fracture aspects,
indicating an irregular propagation in the width direction. In the classification here used this kind of feature is denominated multiple
failure modes [13], i.e. when each side of the specimen presents a different failure mode.
To extend the analysis of this irregular fracture propagation, Fig. 4 shows the Specimen A in more details. In the right side of
figure it is possible to see a typical through-the-thickness shear failure, with an angled fracture (in the thickness direction) and some
debris in the fracture surface. Meanwhile, the left side of the figure shows aspects of two different failure modes, meaning that the
propagation was also irregular in the thickness direction (in addition to the irregular propagation in the width direction). The
classification refers to this kind of feature as mixed failure mode [13], i.e. when one side of the specimen presents aspects of more
than one failure mode. In this case, besides the aspects of the shear failure, it is possible to see a region of the fracture with multiple
delaminations and some layers that apparently suffered buckling. These aspects are characteristics of the delamination buckling
failure [13,14], which tend to occur when the interlaminar shear strength is relatively low [27]. Finally, similar aspects can be seen in
the right side of the Specimen B (Fig. 3), indicating that it also presents a mixed failure mode.
Fig. 5 shows the fracture surfaces of the Specimen A (upper and bottom parts of the fracture surfaces of specimen) related with the
failure modes of each side of the specimen. Analyzing the fracture surfaces (shown in Fig. 5a), it is possible to see that the irregular
propagation of the fracture was caused by a layer which was crushed during the compression test. This layer promoted the
propagation of a delamination, giving rise to a sub-laminate which, because of the higher slenderness, is more likely to suffer buckling
[28]. This buckling process stimulates the development of delaminations in the sub-laminate, leading to the delamination buckling
failure mode [29]. This is rather different from the findings of our previous work [13], on the compression failure modes of laminates
manufactured with prepreg scraps. In that work we find out that the large number of specimens that presented multiple failure modes

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Fig. 3. Compression failure mode of specimens without hygrothermal conditioning.

(43% of all the specimens analyzed) were probably caused by the joining of scraps with different warp and weft directions.
The fracture surfaces are analyzed in more details in Fig. 5b and c. It is possible to see a large amount of debris on the fracture
surfaces, which were caused by the sliding of the mating surfaces. It is also possible to see some small fragments of fibers, indicated by
white arrows in Fig. 5c. These aspects are characteristics of shear failures and support the hypothesis that the irregular propagation of
the fracture (and so the multiple failure modes) only happened because of the layer that was crushed during the test. It is necessary to
highlight that the amount of debris covering the fracture surface hinders the identification of fracture aspects, and so it is not possible
to infer the propagation direction of the fracture. Although is possible to say that the shear failure was not caused by the lateral
instability of the specimen, as in the work of Odom and Adams [11], otherwise it would be possible to identify a neutral axis, which is
characteristic of flexural failures.
Fig. 6 shows the failure modes of some specimens tested after the environmental conditioning. First of all, it appears that the both
sides of all specimens presented similar fractures, indicating that none of them suffered irregular fracture propagation, i.e. none
specimen presented mixed failure mode or multiple failure modes. In addition, all specimens fail by through-the-thickness shear
failure, but with all specimens presenting some layer crushing, which did not influenced in the overall behavior. These characteristic,

Fig. 4. Fracture aspects for the Specimen A, which indicate a mixed mode of failure (through-the-thickness shear + delamination buckling) in the left side and
through-the-thickness shear failure in the right side.

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Fig. 5. Fracture surfaces of Specimen A related to the failure modes of each side of the specimen (a) and in detail (b and c) showing the large amount of debris on the
surfaces. The white arrows (c) indicate fragments of fibers on the fracture surfaces.

namely the pure shear failure and the regular propagation, could be what Paiva and coworkers [21] reported as less severe failure
modes for the conditioned specimens.
Fig. 7 presents the fracture of Specimen E in higher magnification. One can see that, as before mentioned, the fracture occurred as
a through-the-thickness shear with some sign of layers crushed during the test. The layers crushing is a characteristic of the splitting
mode of failure, but here it occurred only in a limited region without influence the overall fracture propagation, so it is classified as a
local failure mode [13,14]. In Specimen E, apparently two outer layers were crushed during the test. One possibility is that these
layers resisted to the shear fracture propagation and, as the compressive load was further applied, failed by suffering a large axial
deformation [6]. It is also possible to see a large number of debris on the fracture surface as well as the angled propagation of the
fracture (in the thickness direction); both were indicated in Fig. 7 by dotted lines.
The fracture surfaces of Specimen E (Fig. 8) show that, differently from the aforementioned, the amount of debris is quite low.
Actually, there are a large number of fragmented layers, which appears as debris when analyzing the failure modes. However the
cause of these fragmented layers is the same of the debris in Fig. 5, i.e. the sliding of the mating surfaces in the shear failure. Here it is
possible to state that, for relatively brittle composites, the shear failures exhibit fracture surfaces with a large amount of debris and
small fragments of fibers. Whilst, increasing the toughness of the composite, the size of this debris also increases, until a point where
the fragments do not separate from their respective layers, giving rise to a fracture surface with various fragmented layers. Once again
there is no evidence of a neutral axis, indicating that the shear failure was likely caused by the fiber waviness of the plain weave

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Fig. 6. Compression failure mode of specimens with hygrothermal conditioning.

fabric here used.

Using higher magnification it is possible to identify some features which would be hindered in the case of a fracture surface with a
higher amount of debris. Firstly, it is possible to see resin rich region, within the white circles in Fig. 8b. This resin accumulation
occurs in the interstitial sites, which are formed due to interlace of the fiber tows in fabrics, as indicated by Greenhalgh [22].
Focusing in this resin rich region it is possible to see the formation of scarps (white arrows in Fig. 8c), which indicate that the fiber
tows neighboring this interstitial site failed at different planes. Moreover it can be seen the occurrence of cusps, pointed by black
arrows in Fig. 8c. Finally, the formation of these relatively large cusps suggests a certain degree of toughness of the polymer matrix,
which can be an effect of the hygrothermal conditioning.
Comparing the behavior of the two groups of specimens, one can see that a considerable lower number of delaminations
propagate due to the compressive load. This fact confirms the findings of Paiva and coworkers [21], that the epoxy matrix suffered a
toughening effect due to the moisture absorption. Looking closely to the fiber surface (see Fig. 9), it is not possible to see any fiber
grooves, which indicates that, even after the fracture, a thin polymer layer stayed bonded to the fiber, i.e. the fiber/matrix interface

Fig. 7. Fracture aspects of the Specimen E, which indicate a through-the-thickness shear failure with a local splitting mode (layers crushed during the test).

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Fig. 8. Fracture surfaces of Specimen E related to the failure modes of each side of the specimen (a) and in detail (b and c) showing fragmented layers. The white
circles indicate resin rich regions. The white and the black arrows respectively point-out the occurrence of scarps and cusps.

Fig. 9. Smooth fiber surface without visible grooves indicating that there was no degradation of the fiber/matrix interface after the hygrothermal conditioning.

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was not degraded by the exposure to moisture. This behavior is far different from the one observed by Purslow and Potter [7], and
explains the minor decrease in the compressive strength (approximately 8%). Finally, most of the specimens tested without being
exposed to moisture showed aspects of two types of failure modes, i.e. the shear failure (through-the-thickness shear) and
interlaminar failure (delamination buckling). Meanwhile, all specimens tested after the environmental conditioning presented shear
failure (through-the-thickness shear). This difference in the failure behavior suggests that the conditioned specimens had lower
lateral stability, caused by the decrease in the stiffness of the polymer matrix. Besides that, the occurrence of less delaminations in the
conditioned specimens indicates a matrix with higher toughness, due to the plasticizing effect of the hygrothermal conditioning. All
of this ended up in a lower compressive strength for the conditioned specimens.

4. Conclusions

The effect of the hygrothermal conditioning on the compression failure was studied for 2D carbon fiber/epoxy resin composite
laminates, from a fractographic outlook. The analysis showed that the specimens tested without conditioning suffered irregular
fracture propagation. For this reason, it is possible to see characteristics of two different failure modes, i.e. through the thickness
shear and delamination buckling. In the case of the conditioned specimens, the compression test caused only failure by through-the
thickness shear.
The differences on the fracture propagation were attributed to the plasticizing effect of the moisture exposure. In this case, the
polymer matrix absorbed water which end up increasing the polymer free volume. This probably caused a decrease of the stiffness of
the polymer together with an increase of the toughness. In the fracture analysis, this plasticizing effect can be seen in the lower
number of delamination and the pure through-the thickness shear of the conditioned specimens. It is also possible to see the
plasticizing effect on the size of the fragments which result from the shear failures (more specifically the sliding of the mating
surfaces), i.e. debris on the surface of the non-conditioned specimens and fragmented layers on the surface of the conditioned
specimens. This effect results in the lower compressive strength for this specimens tested after the environmental conditioning.

Acknowledgements

The authors are grateful to the Technological Institute of Aeronautics (ITA), CAPES/PVNS and CNPq (projects 439129/2016-8,
870484/1997-4, 303287/2013-6 and 150697/2014-7) for the financial support. In addition, the authors would like to thank the
organizing committee of the Meeting on Aeronautical Composite Materials and Structures – MACMS 2015, where a short version of
this paper was presented.

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