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Composites Part B 247 (2022) 110329

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Composites Part B
journal homepage: www.elsevier.com/locate/composites

Non-linear elastic longitudinal behaviour of continuous carbon fibres/epoxy


matrix composite laminae: Material or geometrical feature?
V. Keryvin a ,∗, A. Marchandise a,b , J.-C. Grandidier c
a Univ. Bretagne Sud, UMR CNRS 6027, IRDL, F-56321 Lorient, France
b
Avel Robotics, F-56100 Lorient, France
c
ISAE-ENSMA, F-86360 Chasseneuil-du-Poitou, France

ARTICLE INFO ABSTRACT

Keywords: Carbon fibres and unidirectional continuous carbon fibre composites exhibit a non-linear elastic behaviour.
A. Carbon fibres There has long been a debate on the physical origins of such a behaviour for these materials. Indeed, two
A. Polymer–matrix composites (PMCs) main mechanisms have been proposed: either the reorientation of graphene sheets in the carbon fibre or that
B. Elastic behaviour
of the fibre itself due to initial fibre waviness arising from composite manufacturing. This paper addresses this
B. Non-linear behaviour
issue by performing, on the one hand, specific mechanical tests to extract the non-linear elastic coefficients
C. Elastic properties
in a reliable way, and, on the other hand, using specific finite element analyses with a non-local model. It
is shown first that the proposed experimental method is adequate. Besides, the simulations allow us to show
that, while both contributions for non-linear elasticity indeed come into play for the non-linear elasticity of
carbon fibres, the intrinsic behaviour of fibres can be considered as the main contributory factor. Composites
with glass fibres stay fully linearly elastic, due to the limited stiffness of these fibres.

1. Introduction an experimental protocol based on four-point bending tests to char-


acterise simultaneously the non-linear elastic behaviour of UD both
The non-linear elastic behaviour of carbon fibres was reported as in tension and compression [6]. The values of non-linear parameters
early as the 1960’s [1] and then more recently [2]. This mechanism derived from UD plies are rarely compared to those determined from
is linked to the reorientation of graphene crystallites in the direction single fibre tension tests [14]. This element of comparison is clearly
of the tensile loading [3]. Unidirectional CFRP plies (UD) exhibit a lacking.
non-linear elastic behaviour under tension [4] (stiffening) or compres- The origins of the non-linear elastic behaviour of UD plies in tension
sion [5] (softening). The changes in axial moduli close to failure can be and compression have been the subject of debate. Indeed, since non-
dramatic reaching one-third of reduction in IM fibres for instance [6].
linear behaviour has not been reported for GFRP [13], this non-linearity
As stated by Murphey et al. [7], this is not taken into account for
should arise from the carbon fibre in CFRP. Yet, an additional factor
the design of thick composite parts since they operate at relatively
might come from the initial fibre waviness originating from the curing
low strains, but thin parts subjected to bending may undergo large
step of the manufacturing process. We refer to fibre waviness as the
strains for example in deployable structures. This non-linear behaviour
has consequences on the bending behaviour and in some cases studies undulation of fibres inside a lamina. The misaligned fibres should
have applied two different values of elastic moduli in tension and straighten during tension and contribute fully to the UD stiffness.
compression [8,9]. On the contrary, during compression, these fibres should bend more
The quantification of this UD non-Hookean behaviour has mostly and more, decreasing the UD stiffness during the loading. According
been addressed either with moduli depending progressively and lin- to Vandreumel and Kamp [4], for a given value of fibre waviness,
early on the axial strain (most of the time) [5,7,10,11] and sometimes fibre misalignments have no influence on Young’s modulus in the case
in a non-linear way [12,13]. The characterisation of this behaviour is of tension. Mrse and Piggott [15] concluded that fibre waviness does
usually carried out either in one step accounting for only one type not appear to be a major factor affecting the decreasing compressive
of non-linearity (tension or compression) but not the other (e.g. by modulus with increasing fibre strain.
bending tests [10]), or in two steps by tension and compression tests [5] Hsiao and Daniel [16] proposed a model taking into account the
or by tension and bending tests [12]. We have recently proposed waviness, which they consider as being the origin of non-linearity.

∗ Corresponding author.
E-mail address: vincent.keryvin@univ-ubs.fr (V. Keryvin).

https://doi.org/10.1016/j.compositesb.2022.110329
Received 1 March 2022; Received in revised form 21 July 2022; Accepted 27 September 2022
Available online 1 October 2022
1359-8368/© 2022 Elsevier Ltd. All rights reserved.
V. Keryvin et al. Composites Part B 247 (2022) 110329

However, these authors considered ply waviness instead of fibre wavi- 2.2. Mechanical testing
ness and used misalignment angles up to 15◦ . For Meng et al. [17], due
to the fibre misalignment and manufacturing defects, the compressive Tensile tests on single carbon and glass fibres were carried out at
modulus of continuous fibre composites is reasonably expected to differ controlled conditions of temperature (23 ◦ C) and relative humidity
from the tensile modulus. These authors also add that this will be (48%) following the ASTM D3379 standard. Before the test, the fibre
more obvious in CFRP than GFRP composites since the diameter of is glued on a paper frame with vinyl paper glue. The latter is chosen
carbon fibre is normally smaller than that of glass fibre. This latter so as not to affect the mechanical response of the fibre in tension. The
point raises finally three factors that may come into play: (i) the paper frame is then clamped onto a universal MTS-type tensile testing
possibility of a material characteristic being derived from the intrinsic machine equipped with a 2 N capacity load cell, with an accuracy
non-linear behaviour of carbon or glass fibres; (ii) the possibility of a of 0.01%. The gauge length is 50 mm. The tests are performed after
geometrical feature originating from the initial fibre waviness; (iii) a cutting the edges of the frame. The mechanical analysis of tension is
complementary possibility, due to the influence of fibre diameter, fibre carried out using the engineering strain and the engineering stress,
waviness and fibre stiffness (material/geometrical feature). since only small strains will be developed. The strain is 𝜖𝖿 = (l-l0 )/l0 ,
where l0 is the initial length measured before starting the test and l
In this paper, we attempt to address two questions: (i) are the values
the current length, adjusted to take into account the compliance of the
of the non-linear elastic parameters extracted with the experimental
traction device (0.1246 mm/N). The stress is calculated from 𝜎𝖿 = F/S0 ,
bending protocol, as proposed by Keryvin et al. [6], in line with results
where F is the measured force and S0 the initial cross-section area (the
obtained by other testing methods on UD or single fibres? (ii) what are
diameters are measured by Scanning Electron Microscopy, Jeol JSM
the respective contributions to non-linear elasticity due to the type of
6301 F). The accuracy of the displacement sensor is 1 μm. An adequate
material (carbon fibre) and geometry (fibre waviness) ? For this pur-
number of experiments need to be performed to obtain meaningful
pose, we first carried out mechanical experiments on different carbon
statistics for the mechanical behaviour. We therefore carried out ∼100
and glass fibres as well as on several carbon or glass fibres/epoxy resins
monotonic tensile tests at a constant displacement rate of 1 mm/min
composite laminates. The non-linear elastic parameters measured from
(strain rate of 10−3 s−1 ). Other details can be found in Ref. [19]. The
these different tests are compared, as well as with results from the initial modulus of fibre E𝑇𝖿 0 and the non-linear elastic parameter 𝛽𝑓 are
literature. Then, we investigate the effect of geometrical features (fibre extracted according to Eq. (1) over the range of strain [0.1–0.5] %.
waviness, fibre diameter) on unidirectional lamina stiffness by Finite
Element simulations with a specific non-local modelling. 𝜎𝖿 = E𝖿𝑇 0 𝜖𝖿 (1 + 𝛽𝑓 𝜖𝖿 ) 𝖲𝖥𝖳 (1)

Uniaxial compression tests were carried out on [90/0]3𝑆 laminates


2. Materials and methods following the ASTM D3410 standard. 25 samples were tested. Fibre
glass tabs (±45◦ /thickness = 0.8 mm) were bonded at the end of
2.1. Materials the sample with an epoxy adhesive to reduce the risk of breakage in
the jaws. The gauge length of the samples is 10 mm and the width
Each UD ply is composed of an epoxy resin matrix (Se84LV or 10 mm. Each face of each sample is equipped with a strain gauge
Se84nano with different nanofiller contents [18] from Gurit, M79 and (Kyowa, length = 2 mm), to compare the strains and monitor any
M81 from Hexcel, R374-1 from Structil or XB3515 from Vitech) and bending behaviour. The loading rate is 1 mm/min. The compressive
C is determined as the mean value of the two strain gauges
strain 𝜖𝖴𝖣
either carbon fibres (intermediate modulus – IM – IM2C from Hexcel
and high modulus – HM – HR40 from Mitsubishi) or glass fibres (EC14 while the compressive stress is calculated as for the tension tests. The
compressive stress of the 0◦ ply 𝜎𝖴𝖣 C is determined from the stress
from Valmeria). The prepreg batch had a resin weight content of 35%
and fibre weight of 300 g/m2 on average for all composites. The ply applied on the laminate using Classical Laminate Theory. The initial
compressive modulus E𝐶0 𝖴𝖣 and the non-linear elastic parameter 𝛼 is

thickness is around 300 μm. The fibre volume fraction is 50% for GFRP C .
extracted according to Eq. (2) over the range [0.1–0.5]% of strain 𝜖𝖴𝖣
and 55% for CFRP.
This parameter for the unidirectional ply is the same as that for the
For bending tests (see Section 2.2), the laminate is composed
laminate by assuming that the 90◦ plies stay linearly elastic.
of 11 blocks of plies with the following stacking sequence: [+45◦
|06 ◦ |+45◦ /−45◦ |04 ◦ |−45◦ |02 ◦ |]𝑆 . The plate was manufactured by C
𝜎𝖴𝖣 = E𝐶0 C ′ C
𝖴𝖣 𝜖𝖴𝖣 (1 + 𝛼 𝜖𝖴𝖣 ) 𝖢𝗈𝗆𝗉𝗋𝖾𝗌𝗌𝗂𝗈𝗇 (2)
AVEL Robotics, the layup being performed by a C1-Coriolis Composites
Four-point bending tests (4PB) were carried out with a universal testing
Automated fibre Placement robot. The layup was made in a one-shot
machine (Instron 5567, 30 kN load cell) using a distance of 90 mm
sequence, and the sole compaction force of the robot head was used to
between the upper rollers, where pure bending occurs, and a distance of
create adhesion between the plies, without any intermediate debulking.
460 mm between the lower rollers. Polyethylene plates were put under
The layup contact pressure was greater than 5 bars for all plies. The
the rollers to minimise stress concentrations. Mono-axial strain gauges
stacking sequence used for materials from tool surface to bagging
(10 mm in length – Kyowa) were glued onto both the compression and
materials was as follows: a 12 mm thick aluminium tool, a non porous
the tension sides. Eight to ten monolithic samples were tested. Other
release-film, the prepreg carbon/epoxy stacking, another non-porous
details can be found in Ref. [20]. The force on the assembly and the two
release-film, a 3 mm thick aluminium caul plate, a polyester breather
strain gauges signals were recorded during loading and synchronised.
and a vacuum sealant. The thickness of each block of plies of the same nature were measured
The curing cycle consisted of a one-shot curing. The prepreg stack by optical microscopy (OM, Olympus BX51). The position of the neutral
was monitored and did not undergo any exothermic reaction. The max- axis vis-a-vis the mid-axis is given by the two strain gauges signals on
imum pressure and temperature were respectively 7 bars and 120 ◦ C, the compressive side (𝜖𝑐𝑔 ) and the tensile side (𝜖𝑐𝑔 ).
respectively, during the whole cycle. The plates did not suffer from any 𝑔 𝑔
warping during demoulding and conserved their planarity. The average ℎ 𝜖𝑐 + 𝜖𝑡
𝜆=− (3)
thickness of the plates, ℎ, was around 10 mm after curing. 2 𝜖𝑐𝑔 − 𝜖𝑡𝑔
Plates were precisely machined by water-jet cutting into 500 × 30 The procedure for extracting the elastic properties of the unidi-
× 10 mm3 samples. For each sample, the thickness ℎ and the breadth rectional plies in the beam direction has been reported in Ref. [6]
𝑏 were measured with a calliper. The thickness of each block of plies and will not be reproduced here for sake of clarity. Let us note that
were measured by optical microscopy. The samples were found to be this procedure has also been validated by Finite Element Analyses [6].
completely symmetric for this measurement accuracy. It consists in minimising the relative error between the experimental

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V. Keryvin et al. Composites Part B 247 (2022) 110329

bending moment and an estimated value. The latter involves four Consequently, the strain energy inside the beams must be equal
parameters: the initial moduli in tension, E𝑇𝖴𝖣0 , and in compression, E𝐶0
𝖴𝖣 , to the strain energy of the fibres. For reasons of computation time
as well as the linear decreases of the elastic modulus in tension 𝛽 with limitations, the simulations are performed in a two-dimensional frame-
T and in compression 𝛼 with strain 𝜖 C . They are extracted
strain 𝜖𝖴𝖣 𝖴𝖣
work with a plane constraint assumption (additional motivations are
according to Eq. (4) on the range [0.1–0.5]% of strain. given in [24]). To generate a pure compression or tension state, one
side is blocked in one direction and the displacement is imposed
T
𝜎𝖴𝖣 = E𝑇𝖴𝖣0 𝜖𝖴𝖣
T (1 + 𝛽 ′ 𝜖 T )
𝖴𝖣
𝟦𝖯𝖡 − 𝖳𝖾𝗇𝗌𝗂𝗈𝗇
(4) on the opposite side and permits Poisson’s effect. The displacement
C
𝜎𝖴𝖣 = E𝐶0 C ′ C
𝖴𝖣 𝜖𝖴𝖣 (1 + 𝛼 𝜖𝖴𝖣 ) 𝟦𝖯𝖡 − 𝖢𝗈𝗆𝗉𝗋𝖾𝗌𝗌𝗂𝗈𝗇 imposed on the model corresponds to a mesoscopic deformation of
In doing so, the coefficients 𝛼 ′ = 𝛼
and 𝛽 ′ = 𝛽
are introduced, 0.5%. The macroscopic logarithm strain is deduced from the length of
E𝐶0 E𝑇𝖴𝖣0
𝖴𝖣 the structure at the end of the loading and the mesoscopic Cauchy stress
with respect to Ref. [6].
is deduced from global force and transverse section.
To be able to compare the different fibres and the different mechan-
To define the properties of beams, it is assumed that the ten-
ical tests, the range of deformation is chosen to be [0.1–0.5]% for all
sile/compressive modulus is equal to the tension modulus of fibres 𝐸𝑓 ,
tests since CFRP with HM fibres fail at around 0.5% during bending
which are assumed to have a linear elastic behaviour. The cross-section
tests [21].
area 𝑆𝐵 𝑖 and second moment of area 𝐼𝐵 𝑖 of beams 𝑖 can be defined to
Instead of performing flexural tests, tension and compression tests
obtain similar energy to compression/tension. The following relations,
could have been carried out for addressing the objective of this paper.
Eq. (7), can be written as:
The use of a single test (bending) with respect to two (tension and
𝑛𝑏 𝑛
compression) makes it possible to identify the non-linear behaviour ∑ 𝑙𝑖 ∑
𝑓
𝐸𝑓 𝑆𝑓 𝑙𝑖
𝑉𝑓 𝐸𝑓 𝑢′ 𝛿𝑢′ 𝑑𝛺 = 𝐸𝑓 𝑆𝐵 𝑖 𝑢′ 𝛿𝑢′ 𝑑𝑙𝑖 = 𝑢′ 𝛿𝑢′ 𝑑𝑙𝑖 (7)
simultaneously on the same sample with the same manufacturing con- ∫𝛺 ∫0 𝐴 ∫0
𝑖=1 𝑖=1
ditions including curing. The stacking used for bending specimens
has some off-axis plies. It is representative of nautical uses for racing where 𝑛𝑓 is the number of the fibres and 𝑛𝑏 the number of the beams
yachts [22]. The same experimental studies could have used performed of length 𝑙𝑖 , 𝑢 is the displacement in the fibre direction and ()′ the
on beams without off-axis plies. A previous study showed that their derivate operator in the fibre direction. A is a coefficient that depends
influence is negligible on the elastic behaviour [6]. The compression on Poisson’s ratio to obtain the stiffness of the unidirectional composite.
test could have also been performed on unidirectional coupons. In this In the 2D framework, the number of beams is very close to the number
study, their results are only used for reasons of comparison. In all cases, of fibres and is calculated in accordance to 𝑉𝑓 . The second moment of
the low levels of strains (below 0.5%) limits possible spurious effects. area of beams is determined in the same manner. The following equality
concerns the bending energy:
𝑛𝑏
2.3. Numerical simulations – Beam Non Local model (BNL) 𝐼𝑓 ∑
𝑉𝑓 𝐸𝑓 𝑣′′ 𝛿𝑣′′ 𝑑𝛺 = 𝐸𝑓 𝐼𝐵 𝑖 𝑣′′ 𝛿𝑣′′ 𝑑𝑙𝑖 (8)
∫𝛺 𝑆𝑓 ∫𝑙𝑖
𝑖=1
It is possible that geometry via fibre waviness could be the cause
of non-linear elasticity. This hypothesis is investigated by numerical The representative volume element (RVE) chosen here is a square
simulations. The idea of the model presented here is to take into of 1.6 mm × 1.6mm, which is meshed with 6400 beams and 6480
account local bending of fibres with beam elements linked to contin- plane stress elements, while the number of nodes is 19 763. The initial
uum elements as in [23,24], but without describing each fibre. This default is assumed to be constant (fibres undulate in phase) in the
approach is similar to that proposed by Wisnom [25], but, in our study, structure, being taken as sinusoidal and described by two parameters:
the concept is extended to the mesoscopic scale. In this formulation, the its amplitude and wavenumber. The wavenumber is chosen as equal
equilibrium of the medium is characterised by the principle of virtual to 4 and the amplitude of the defect is equal to either 2.22 or 4.44
works. A variational form of equilibrium equations for all kinematically μm which corresponds to a maximum misalignment angle of 1 and 2◦
admissible displacement fields K.A. to zero is written in Eq. (5) as respectively.
proposed by Drapier et al. [26]: The anisotropic properties of the 2D continuum medium (stiffness
{ } tensor 𝐿≈
𝖢𝖬
) are defined through the composite cylinder assemblage
− 𝑉𝑓 𝐸𝑓 𝑟2𝑔𝑓 𝑣′′ 𝛿𝑣′′ + 𝑆 ∶ 𝛿𝐸 𝑑𝛺 + 𝐹 ⋅ 𝛿𝑢 = 0 ∀ 𝛿𝑢 𝖪.𝖠. to 0 (5) homogenisation scheme [27] with the determination of the in-plane
∫𝛺 ∼ ∼
shear modulus being made following the generalised self consistent
where 𝑉𝑓 is the fibre volume fraction, 𝐸𝑓 , the fibre axial modulus,
√ scheme [28] for a unidirectional composite. The fibre volume fraction
𝐼𝑓
𝑟𝑔𝑓 = is the fibre gyration radius, 𝑆𝑓 the fibre cross-section is taken as 50% for GFRP and 55% for both CFRP. The fibre properties
𝑆 𝑓
are taken from datasheets (tensile modulus) and literature results [29].
area and 𝐼𝑓 second moment of area of the section, 𝑣 the transverse
The matrix is assumed to be a classical epoxy resin [21] with a Young’s
displacement, 𝑣′′ , the local fibre curvature field, 𝑆

is the second Piola
modulus of 3.5 GPa and a Poisson’s ratio of 0.4. In the fibre direction,
Kirchhoff stress tensor and 𝐸∼
is the Green Lagrange strain tensor. 𝐹 and
the contribution of the fibre on stiffness is supported by the beam and
𝑢 are the external load and displacement fields and 𝛿 is the variational
should be subtracted from the 2D medium stiffness. All necessary pa-
operator. Taking into account 𝑣′′ makes the model non-local.
rameters of the model are reported in Tables 1 and 2. The code Abaqus
The terms of integrals are estimated with (first part) quadratic three
v6.17 (Dassault Systèmes) is used with elements B22 (2D beams) and
nodes finite Timoshenko beam elements linked (using the same nodes)
CPS8 (plane stress continuum elements). A description of the model is
to quadratic continuum elements (second part), to take better account
shown in Fig. 1. The nodes of the beams and the 2D medium are shared,
of the shape of initial waviness and to ensure the continuity of the
so the displacements are identical, only the rotations of the straight
fields of displacement. In the Beam Non Local (BNL) model, beams
sections of the beams are not related to the continuous medium, they
represents the bending and the tension/compression of the fibres in
their direction, and a continuum medium represents the behaviour of a allow us to understand the micro-bending energy.
composite without bending and tension/compression of fibres (transverse Within the framework of this article, where one wants to understand
behaviour of the composite and its shear). It is possible to rewrite the the physical origins of the elastic non-linearity, it is necessary and
second term in the integral of Eq. (5) as follows: sufficient to build a model with the consideration of the fibres (stiffness
and diameter) and the initial defects at the ply scale. There were two
𝑆 ∶ 𝛿𝐸 𝑑𝛺 = 𝑆 𝖢𝖬
∶ 𝛿𝐸 𝑑𝛺 + 𝑉𝑓 𝐸𝑓 𝑢′ 𝛿𝑢′ 𝑑𝛺 (6) possible ways to address this. Firstly, a 2D or 3D description of the
∫𝛺 ∼ ∼ ∫𝛺 ∼ ∼ ∫𝛺 arrangement of fibres and matrix can be conducted on a representa-
where 𝑢 is the longitudinal displacement, 𝑢′ its spatial derivative and tive elementary volume with necessarily conditions of periodicity and
𝖢𝖬
𝑆

is the stress on the continuum medium. a limited dimension [30–33], within the framework of the classical

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V. Keryvin et al. Composites Part B 247 (2022) 110329

Fig. 1. Description of the non-local model including boundary conditions, the connectivity between the continuum medium and the fibres (top). An example of output field (axial
stress here) in the continuum medium and the fibre (beam).

continuum mechanics. It requires a complete description of the mi- Table 1


𝖢𝖬
Properties of BNL homogeneous continuum media: stiffness tensor 𝐿 components in
crostructure with the modelling of the matrix, the fibres and their ≈
GPa. (Only necessary components are considered in the 2D numerical analysis; 1 is
connections. The mesh must be fine enough to describe the micro the fibre axis).
bending and wavinesses with 2D or 3D finite elements which are not L𝖢𝖬
1111
L𝖢𝖬
1122
L𝖢𝖬
2222
L𝖢𝖬
1133
L𝖢𝖬
2233
L𝖢𝖬
3333
L𝖢𝖬
1212
L𝖢𝖬
1313
L𝖢𝖬
2323
made for and which can lock in bending, Secondly, an alternative is CFRP (IM2C) 1.67 1.48 11.7 1.48 6.05 11.7 3.70 3.70 2.80
to position oneself in the context of non-local media by integrating a CFRP (HR40) 1.84 1.56 11.0 1.56 5.80 11.0 3.70 3.70 2.60
GFRP (EC14) 2.17 0.92 16.2 0.92 8.03 16.2 3.40 3.40 3.60
term of micro-curvature in the energy expression. It is important to GFRP (EC7) 2.17 0.92 16.2 0.92 8.03 16.2 3.40 3.40 3.60
emphasise here that the beams are not an exact representation of the
fibres, they are present to calculate this micro-curvature energy of the
Table 2
non-local model. Beams and solid elements share the same nodes. The Geometrical properties of BNL beams (thickness, fibre diameter in 2D and width) and
displacements at these nodes are strictly identical. The rotation part material properties: axial Young’s modulus for fibre (𝑓 ) and lamina elastic properties
in the beams only makes it possible to calculate the micro energy of of the ply (fibre axis L and transverse axis T).

curvature of the nonlocal medium; this is the reason for this choice of Property Beam Beam E𝑓 E𝐿 E𝑇 G𝐿𝑇 𝜈𝐿𝑇
Width Thickness
structural elements. This term of rotation is not related to the solid, it Material [μm] [μm] [GPa] [GPa] [GPa] [GPa] [–]
is indirectly related by the field of displacement and takes part in the CFRP (IM2C) 2.11 5.2 296 164 8.4 3.7 0.31
equilibrium like a Timoshenko beam where the rotation of the section CFRP (HR40) 1.58 7 360 200 7.8 3.7 0.31
is independent of the transverse displacement. However, it is this term GFRP (EC14) 0.71 14 80 42 11 3.4 0.32
GFRP (EC7) 1.42 7 80 42 11 3.4 0.32
which is necessary to account for the structural effect without having
to create a complete model describing the microstructure. That is the
key point of this second approach we have selected. Table 3
Papers [34,35] showed and mathematically demonstrated that this Initial UD moduli in tension E𝑇𝖴𝖣0 and compression E𝐶0
𝖴𝖣 for M81/IM2C, M81/HR40
(carbon fibres) and XB3515/EC14 (glass fibre) by 4PB tests.
description is consistent in the context of micromechanics. It is even
M81/IM2C M81/HR40 XB3515/EC14
capable of understanding boundary layer effects under compression and
E𝑇𝖴𝖣0 [GPa] 165 ± 4 195 ± 6 40 ± 1
bending, as shown by calculations on a complete microstructure. This
E𝐶0
𝖴𝖣 [GPa] 164 ± 3 195 ± 5 40 ± 2
homogeneous approach by the nature of the finite elements does not
raise questions about the quality of the numerical result; the calcula-
tions are short and above all it is possible to distribute the defects at
the mesoscopic scale in connection with the wavelengths observed in
different papers.

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V. Keryvin et al. Composites Part B 247 (2022) 110329

Table 4
Comparison between non linear elastic parameters (dimensionless numbers) extracted
by different mechanical tests on IM2C and HR40 fibres. SFT stands for single fibre
tension test, 4PB for four-points bending tests and COMP for compression tests.
Tension Compression
Test 4PB SFT 4PB COMP
Parameter 𝛽′ 𝛽𝑓 𝛼′ 𝛼′
Fibre
HR40 21.6 ± 4.4 17.7 ± 4.2 21.8 ± 3.6 n.d.
IM2C 13.7 ± 3.9 n.d. 8.0 ± 3.4 12.3 ± 1.3

Fig. 4. Compression test on [90/0]3𝑆 Se84LV/IM2C laminate used to determine the


parameter 𝛼 ′ using Eq. (2). The inset indicates the evolution of the secant modulus
(relative to E𝐶0,𝖫𝖠𝖬 ).

Fig. 2. Single fibre tensile tests on HR40 carbon fibre used to determine the initial
tensile modulus E𝑇𝖿 0 on [0–0,1] % of tensile strain and that of 𝛽𝑓 on [0.1–0.5] % of
strain, using Eq. (1). The inset indicates the evolution of the secant modulus (relative
to E𝑇𝖿 0 ).

Fig. 5. Four-point bending tests on M81/IM2C, M81/HR40 (carbon fibres) and


XB3515/EC14 (glass fibre): neutral axis position during the loading as defined
in Eq. (3).

Table 3 shows the initial moduli of three different composites


introducing the three different fibres studied here. These moduli are the
same in tension and compression. Eq. (4) is used to determine the non-
linear parameters from four-point bending tests (4PB) on eight batches
of five different epoxy matrices and IM2C fibre (Se84LV, Se84 nano
Gen1, Se84 nano Gen 2, R374-1, M79, M81), giving a linear increase in
tension modulus 𝛽 ′ = 13.7 ± 3.9 and a linear decrease in compression
Fig. 3. Single fibre tensile tests on glass fibres EC14 used to determine the initial tensile
modulus E𝑇𝖿 0 on [0–0,1]% of tensile strain. A constant slope (modulus) is observed up
modulus 𝛼 ′ = 8.0 ± 3.4. For the other eight batches of six different
to 0.5%. The inset indicates the evolution of the secant modulus (relative to E𝑇𝖿 0 ). epoxy matrices (Se84 nano Gen1, Se84 nano Gen 2 with three different
nano-fillers contents, R374-1, M81) and HR40 fibre, Eq. (4) gives 𝛽 ′ =
21.6 ± 4.4 and 𝛼 ′ = 21.8 ± 3.6. It is important to specify that, for a
given fibre, we find no influence of the matrix on these latter values.
3. Results
The position of the neutral axis during the loading, which was taken as
Examples of SFT results are presented in Fig. 2 (HR40 carbon an indicator of non-linear elasticity in [6], is plotted in Fig. 5 for glass
fibre) and Fig. 3 (EC14 glass fibre). Data analyses, using Eq. (1), give fibre EC14 and carbon fibres IM2C and HR40. No evolution is observed,
an initial tensile modulus of 358 ± 22 GPa and a linear increase in for the glass fibre, in conformity with a linear elastic behaviour: the
tension modulus 𝛽𝑓 = 17.7 ± 4.2 for HR40 carbon fibre. They also neutral axis and the mid-axis coincide, as recently reported by Cocchi
give an initial tensile modulus of 81 ± 4 GPa for the glass fibre; et al. [13]. The shift towards the tensile zone is more pronounced for
no noticeable changes in this modulus are detected in the range of HR40 than for IM2C, which is in agreement (see Table 4) with the
strains investigated (below 0.5%). Note that unlike the initial tensile non linear parameters 𝛼 ′ and 𝛽 ′ which are higher for HR40 than for
modulus, the determination of 𝛽𝑓 is not sensitive to uncertainties in IM2C. All non-linear parameters values are reported in Table 4 for
the measurement of fibre diameter. comparison.
Fig. 4 shows an example of the determination of 𝛼 ′ from single com- Figs. 6 to 8 describe the evolution of the axial modulus of a UD
pression tests (COMP) on Se84LV/IM2C. Data analyses, using Eq. (2), ply of epoxy/fibre composite in tension and compression for IM2C
give a linear decrease in compression modulus 𝛼 ′ = 12.3 ± 1.3. carbon fibre, HR40 carbon fibre, and EC14 glass fibre. The moduli,

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V. Keryvin et al. Composites Part B 247 (2022) 110329

Table 5
Non linear elastic parameters (𝛽𝑓 from SFT, 𝛽 ′ from TUD and 4PB, 𝛼 ′ from CUD and 4PB) taken from the literature for
different types of carbon fibres. Acronyms are: SFT (single fibre tension), TUD (tension UD), CUD (compression UD), 4PB
(four-points bending). Mod. (modulus) denotes a tangential (T) definition of the modulus or a secant definition of the modulus
(S) [the coefficients determined by the tangent method are divided by two in this table]. |𝜖𝗆𝖺𝗑 | is the fracture strain .
Type Name Source Test Mod. 𝛽𝑓 𝛽′ 𝛼′ |𝜖𝗆𝖺𝗑 | [%]
SM T300 Hughes [2] Tension (Tow) T 8 1.6
T400 ′′ ′′ ′′ 8 1.9
T700 ′′ ′′ ′′ 8 1.7
T300 Kant and Penumadu [14] SFT T 13 1.2
′′ ′′ ′′
T400 13 1.6
′′ ′′ ′′
T700 13 1.4
T300 Allix et al. [10] 4PB S 19 1.2
T300 Djordjević et al. [11] TUD/4PB T 13 13 1.6
T300 ′′ TUD/4PB T 14 6 1.6
Thornel A ′′ TUD/4PB ′′ 12 1.6
′′ ′′
HTA SFT/TUD 8 13 1.6
′′ ′′ ′′
Grafil 9 1.6
XAS Wisnom [5] TUD/CUD S 4 14 1/0.5
IM T800 Hughes [2] Tension (Tow) T 9 1.7
T800 Kant and Penumadu [14] SFT T 13 1.7
IM6 Allix et al. [10] 4PB S 24 1.1
IM7 Murphey et al. [7] TUD/4PB T 11 12 1.3/1.5
′′ ′′ ′′
IM10 12 13 1.5/2
IM2C Keryvin et al. [6] 4PB S 5 22 1.2
IM2C This work 4PB S 14 8 0.5
′′
IM2C COMP S 12 0.5
HM M40 Hughes [2] Tension (Tow) T 12 0.6
M50 ′′ ′′ ′′ 14 0.5
M40 Kant and Penumadu [14] SFT T 13 1
′′ ′′ ′′
M50 14 1.2
HR40 This work SFT/4PB S 18 22 22 0.5
UHM M55 Murphey et al. [7] TUD/4PB T 11 14±134 0.5

for different fibre waviness levels, vary as a function of the out-of-


plane misalignment angle 𝜃, derived from the numerical simulations
described in Section 2.3. At 0.5% in strain for the highest angle of
2◦ considered here (a value beyond reported values, see [20,22,36]),
we find an increase of ∼0.5 h in tension and a decrease of ∼0.7 h
in compression are reported for the GFRP, which are non-significant
differences. On the contrary, at 0.5% of strain, UD with carbon fibres
show an increase in their tensile moduli by ∼0.7% for IM2C (compared
with 1% for HR40) and decreased their compressive moduli by ∼1.2%
for IM2C (respectively 1.8% for HR40), for the same 𝜃. Fig. 9 finally
compares the behaviour of these different fibres.

4. Discussion

4.1. Relevance of the values of the non-linear parameters extracted by 4PB

Fig. 6. Evolution of axial modulus for IM2C carbon fibre in an unidirectional For HR40 carbon fibre, the increase in tensile modulus given by 4PB
epoxy/fibre ply as given by the non-local numerical model. is a little higher than that given by SFT (see Table 4), even if this result
is somewhat mitigated by the data scatter. Since the fibres are straight
in the SFT tests, we cannot exclude a possible contribution, even if
minimal, due to initial geometrical defects such as fibre waviness in the
UD plies. This is investigated in Section 4.2. For IM2C carbon fibre, the
decrease in compression modulus as given by 4PB is a little lower than
that given by COMP (see Table 4).
In Table 5, we have compared our data with literature results. For
four main reasons, it is problematic to compare the values for non-
linear elastic parameters to other literature sources. Firstly, there is a
large number of experimental methods for which comparisons are not
relevant. For instance, Kant and Penumadu [14] extracted 𝛽𝑓 by SFT
and compared it to previous results from Hughes [2] obtained from
tension tests on tows. While some fibres yield similar results (HM),
others show a large difference (Standard Modulus – SM). Secondly,
we should highlight that two different moduli can be extracted form
experimental data in the literature, i.e. the secant modulus, which is
the ratio of stress to strain [10], and the tangent modulus, which is the
Fig. 7. Evolution of axial modulus for HR40 carbon fibre in an unidirectional derivative of stress versus the derivative of strain [7]. In the following,
epoxy/fibre ply as given by the non-local numerical model. we use only the secant modulus values from Table 5. The non-linear

6
V. Keryvin et al. Composites Part B 247 (2022) 110329

Table 6
Contribution of fibre waviness to the increase of stiffness in tension and decrease in
compression for an epoxy/fibre UD composite at a strain of 0.5% (absolute value). All
values are in %. 4PB refers to experimental data determined by four-points bending
while BNL stands for numerical simulations with a fibre waviness 𝜃 of 1 or 2◦ . The
‘contribution’ is the ratio BNL to 4PB.
Strain 0.5% - 𝜃 = 1◦
Tension (increase in stiffness) Compression (decrease in stiffness)
Fibre 4PB BNL Contribution 4PB BNL Contribution
IM2C 7 0.2 3 4 0.3 8
HR40 11 0.25 2 11 0.5 5
EC14 ∼0 ∼0 n.d. ∼0 ∼0 n.d.
EC7 ∼0 ∼0 n.d. ∼0 ∼0 n.d.
Strain 0.5% - 𝜃 = 2◦
Tension (increase in stiffness) Compression (decrease in stiffness)
Fibre 4PB BNL Contribution 4PB BNL Contribution
IM2C 7 0.7 10 4 1.2 30
HR40 11 1 9 11 1.8 16
Fig. 8. Evolution of axial modulus for EC14 glass fibre in an unidirectional epoxy/fibre
EC14 ∼0 0.05 n.d. ∼0 0.07 n.d.
ply as given by the non-local numerical model.
EC7 ∼0 0.05 n.d. ∼0 0.07 n.d.

coefficients differ by a factor of 2 according to whether we use the


secant modulus or the tangent modulus. (Actually, this is the case only
if the stress is a second-order polynomial function of the strain. In
some studies, the non-linearity can be described as a power-law, again
making it difficult to make comparisons between sources.) Thirdly, to
our knowledge there are no data available for IM2C and HR40, so we
make some comparisons with similar types of fibres. Finally, the non-
linear elastic behaviour, described only in our case via 𝛼 ′ and 𝛽 ′ , may
vary depending on the strain level (see Figure 6 in Ref. [6]). Our value
of 𝛽𝑓 = 18 for the HM carbon fibre HR40 is comparable to the values
reported for HM fibres [2,14].
In terms of values obtained from composite plies, Allix et al. [10]
reported 𝛼 ′ of 24 for an IM carbon fibre, IM6. IM2C is similar to IM6,
so the 𝛼 ′ value of 8 ± 3 and the 𝛽 ′ value of 14 ± 4, obtained in our
study, are therefore very different from previous results. However, the
values found in [10] are determined over the entire range of strains Fig. 9. Evolution of axial modulus for IM2C and HR40 carbon fibres as well EC14
up to failure (at around 1.5%), which is very different from the range glass fibre in an unidirectional epoxy/fibre ply as given by the non-local numerical
model.
considered here (0.1–0.5%). Indeed over the entire range of strains up
to failure, Keryvin et al. [6] reported an 𝛼 ′ of 22 ± 2, consistent with
the literature [10]. Yet, Murphey et al. [7] reported 𝛼 ′ and 𝛽 ′ values
of the misalignment angle 𝜃 = 2◦ . Assuming a more relevant value of
of 11 and 12 for IM7 as well as 12 and 13, respectively, for IM10.
1◦ for this angle (see [20,22,36,37]), the increase and the decrease
The authors observed very high failure strains on thin composites in
are limited to ∼0.2 and 0.35%, respectively, so that geometry can
bending. This comparison with IM fibres is a classic example of the
explain 1/14th and 1/11th of the changes in stiffness in tension and in
need to pay special attention when comparing raw results: the fibres
compression, respectively.
may differ even if they are made from IM type; the range of maximum
For HR40 carbon fibre, geometry can explain up to 1/10th of the
strains differ and the assumption of a linear variation of elastic moduli
increase and up to 1/6th of the decrease, by taking an extreme value
may have an influence; the method used for the direct extraction of
of the misalignment angle 𝜃 = 2◦ . For a more relevant value of 1◦ for
parameters (as in this study) for the two coefficients or the use of
this angle, the increase and the decrease are limited to ∼0.25 and 0.5%,
different tests (and therefore different maximum strains) [7] has a clear respectively, in which case geometry can explain 1/50th and 1/20th of
impact on the values. the changes in stiffness in tension and in compression, respectively.
All these comparisons, as well as the numerous different epoxy Therefore, for a reasonable value of the misalignment angle, and
matrices studied (see Section 3), lead us to infer that the method used for a maximum strain of 0.5%, the (extrinsic) contribution of geometry
for the extraction of the non-linear parameters 𝛼 ′ and 𝛽 ′ is well-founded is of second order, but not negligible, with respect to the (intrinsic)
and that these properties are not resin-based. contribution of the carbon fibre.
The differences in response between the carbon and glass fibres are
4.2. Possible origins of elastic non linearity very marked. We might consider that the large diameter of the glass
fibres is the main cause of this difference, but a simulation with 7 μm
We attempt to discriminate here between possible contributions to in diameter fibres (see Tables 1 and 2) leads to the same linear response
elastic non-linearity due to the carbon fibre itself and its misalignment. (see Fig. 10). Consequently these differences cannot be attributed to the
Table 6 shows the relative contribution of geometry (misalignment diameter of the reinforcement, which is not the only parameter that
angle 𝜃) obtained with the BNL (Beam Non Local) model vis-à-vis defines the behaviour in tension and compression. While it is true that
experimental results in compression and in tension obtained by 4PB. the section contributes to the microbending stiffness of the fibres, it is
For IM2C carbon fibre, geometry can explain up to 1/10th of the essential to take into account of the non-linear geometric destabilising
𝐼
increase and up to 1/4th of the decrease, by taking an extreme value term 𝑉𝑓 𝐸𝑓 𝑆𝑓 (see Eq. (8)) in the analysis. If this term depends on
𝑓

7
V. Keryvin et al. Composites Part B 247 (2022) 110329

5. Conclusion

To understand the origins of elastic non-linearity of continuous fibre


composites in tension and compression, we have performed four-point
bending experiments and numerical simulations. The former allows us
to extract the quantitative parameters of this non-linearity. Compared
to other experiments and literature results, we have shown that this
procedure is well-founded. The latter allows us to quantify the contri-
bution of fibre waviness to this non-linearity. Considering the interplay
between glass and carbon fibres on the one hand, and, the diameter of
these fibres, along with their initial waviness, on the other hand, we
can address the initial question on the origins of elastic non-linearity.
For the range of strains considered here (less than 0.5%):

1. The initial moduli are equal in tension and in compression


2. GFRP as well as single glass fibres are linear elastic
Fig. 10. Evolution of axial modulus for EC7 glass fibre in an unidirectional epoxy/fibre 3. CFRP with IM or HM fibres as well as single fibres are non-linear
ply as given by the non-local numerical model.
elastic
4. The non-linearity for HM carbon fibre in tension and compres-
sion is more pronounced than for IM carbon fibre
the initial defect as detailed in [26], it is also a function of the stress 5. The non-linearity arising from fibre misalignment is almost nil
applied in the direction of the fibres. However, for glass fibres, this in GFRP and much larger for CFRP. The difference is shown to
stress level is much lower than for carbon fibres at the same level of be derived from the lower stress levels in glass fibres and not
deformation imposed on the ply. Consequently, the geometric nonlinear from the larger diameter of glass fibres
term that generates the evolution of the stiffness in tension as well 6. Geometry can contribute to the global elastic non linearity,
as in compression will only be quantifiable at much higher levels of using misalignment levels reported in the literature (∼ 1◦ ), with
deformation for glass fibres. These levels would be above the local changes up to 1/14th in tension and 1/11th in compression for
micro-plastic buckling instability. For the two types of carbon fibre, the IM carbon fibres
differences arise not only from the geometrical stiffness of the fibres, 7. The non-linearity of carbon fibres in tension and compression is
but also from the stiffnesses in the other directions (differentiated predominantly intrinsic to their nature
stiffnesses given in Tables 1 and 2).
Besides, the non-local numerical model, used in this study, opens
some interesting perspectives. For instance, after accounting for the
4.3. Impact and relevance of this study nonlinearities in compression, it will finally be possible to understand
much more precisely the failure stress in compression with all the
It might be strange to state that the non-linear elasticity of CFRP, potential to account for the material variabilities (defects, volume
the very first behaviour required for design, is still either unknown fraction) at the mesostructure scale.
or not properly addressed by composite scientists and engineers. This
study is clearly an attempt to reappraise this topic, which is not yet CRediT authorship contribution statement
solidly grounded. If this non-linearity is not taken into account in
numerical simulations, stress-based approaches become meaningless. If V. Keryvin: Resources, Data curation, Conceptualization, Method-
it is taken into account, one may be interested in knowing the levels of ology, Validation, Writing – original draft, Supervision, Formal anal-
non-linearity, in tension and compression, for a given composite ply. ysis. A. Marchandise: Writing – review & editing, Resources, In-
This justifies, by the way, to compare our results to that of literature, vestigation. J.-C. Grandidier: Software, Writing – review & editing,
highlighting possible traps for a fast reader who could quickly pick Conceptualization, Investigation.
numbers without reading in details a given study. Besides, for force-
imposed boundary value problems, dimensioning in terms of deflection
Declaration of competing interest
or strength requires the elastic behaviour to be known. It is also the
case when comparing test results on composite parts or structures
The authors declare that they have no known competing finan-
with instrumentation, recording only kinematical data (displacements
cial interests or personal relationships that could have appeared to
or strains), to numerical simulations. Moreover, since the compressive
influence the work reported in this paper.
strength is often the key design parameter for composite structures,
the questions of its measurement and its estimation are at stake. In
both situations, one needs to calculate a stress, based on a modulus. Data availability
Untangling the possible contributions of this nonlinear elasticity is both
scientifically and pragmatically of interest. For the former, it permits Data will be made available on request.
to study the mechanisms of nonlinearity at different scales, identifying
the ultramicrostructure of carbon fibres as the main contributor. For Acknowledgements
the latter, it allows one to separate possible effects of matter (carbon
fibre) from that of manufacturing. Indeed, fibre waviness comes mostly We would like to thank the French ANRT for partial funding of the
from the curing step in thermosets-based composites. For example, PhD grant of A. Marchandise (#2016/0114) as well as A. Boyer, P.-
the estimation of compressive strength proposed by Budiansky and Y. Méchin, I. Pillin, H. Bellegou (IRDL), F. Portanguen (UBS) and R.
Fleck [38] separates the behaviour of the plies from that of the fibre Le Borgne (Avel Robotics) for their experimental assistance. Dr M.S.N
waviness. Carpenter post-edited the English style and grammar.

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