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Plastics, Rubber and Composites

Macromolecular Engineering

ISSN: 1465-8011 (Print) 1743-2898 (Online) Journal homepage: https://www.tandfonline.com/loi/yprc20

Experimental study on mechanical properties


of aramid fibres reinforced natural rubber/SBR
composite for large deformation – quasi-static
mechanical properties

Jianhong Gao, Xiaoxiang Yang, LiHong Huang & Yaohong Suo

To cite this article: Jianhong Gao, Xiaoxiang Yang, LiHong Huang & Yaohong Suo (2018)
Experimental study on mechanical properties of aramid fibres reinforced natural rubber/SBR
composite for large deformation – quasi-static mechanical properties, Plastics, Rubber and
Composites, 47:9, 381-390, DOI: 10.1080/14658011.2018.1514480

To link to this article: https://doi.org/10.1080/14658011.2018.1514480

Published online: 01 Sep 2018.

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PLASTICS, RUBBER AND COMPOSITES
2018, VOL. 47, NO. 9, 381–390
https://doi.org/10.1080/14658011.2018.1514480

Experimental study on mechanical properties of aramid fibres reinforced


natural rubber/SBR composite for large deformation – quasi-static mechanical
properties
Jianhong Gaoa,b, Xiaoxiang Yanga,b, LiHong Huanga and Yaohong Suoc
a
College of Chemical Engineering, Fuzhou University, Fuzhou, People’s Republic of China; bQuanzhou Normal University, Quanzhou,
People’s Republic of China; cCollege of Mechanical Engineering & Automation, Fuzhou University, Fuzhou, People’s Republic of China

ABSTRACT ARTICLE HISTORY


Quasi-static mechanical properties of aramid fibres reinforced natural rubber/SBR composites Received 25 December 2017
are comprehensively investigated via scanning electron microscopy (SEM), uniaxial tensile Revised 14 August 2018
tests, multi-step stress relaxation, and the Mullins experiment. The strength, stiffness, Accepted 17 August 2018
viscoelasticity, and Mullins effect of composites are analysed, and the micro failure
KEYWORDS
mechanism is also explored. It is shown that the samples appear similar to a laminate plate Rubber; aramid; fibres;
with random short fibres in a plane. The results of the uniaxial tensile tests indicate that the experiment; mechanical
tensile strength and elongation at failure decrease, while the stiffness increases following the property; composites;
addition of a small amount of aramid fibres into the rubber matrix. The multi-step relaxation Mullins; relaxation
and Mullins experiments reveal that the aramid-short-fibres weaken the viscoelasticity of
rubber composites. Finally, the strain energy of the composite is divided into four parts, and
one part is considered with respect to its application to the study of interface destruction
between the matrix and fibre.

Introduction
investigations, there is a paucity of studies on proper-
A recent research topic that is rapidly gaining attention ties including stress relaxation, viscoelasticity, and
involves reducing the weight and rolling resistance of a Mullins damage of AFRC, and this is seemingly impor-
tyre, thus improving the global environment and sav- tant for rubber composites with short fibres.
ing automobile fuel. Aramid pulp is widely used as a With respect to composites reinforced by short
reinforcement material in the rubber matrix used for fibres, a few classical theories that describe mechanical
tyres [1,2]. During the process of rubber mixing at behaviour include Eshelby’s equivalent inclusion the-
high temperatures, a chemical reaction occurs between ory [9], Mori–Tanaka modified theory [10], the self-
aramid pulp and carbon black. This results in consistent method [11], and the Hashin–Shtrikman
decreased friction energy between fillers, and improve- bound method [12]. Additionally, several theoretical
ments in the hysteresis characteristics [1,3]. Addition- and numerical studies focused on short fibre-
ally, it results in a higher modulus and improves the reinforced composites [13–15]. However, given the
characteristics of the cutting and stab resistance for limitation of the application with respect to small
rubber composites [4,5]. Furthermore, the tyre weight deformations, it is not possible to apply most of the
is reduced by adjusting the mass ratio of carbon aforementioned methods on rubber composites that
black to aramid short fibres. exhibit the characteristics of hyper elasticity and large
Therefore, recent research attention focused on the deformation directly. During large deformation, there
mechanical properties of aramid fibre-reinforced are still several internal structure mechanisms, such
rubber composites (AFRC). Pitchapa et al. [6] exam- as the interaction between fibres and matrix and
ined the effects of aramid fibre and carbon black con- fibres and fibres, which should be explored. It is necess-
tent on the mechanical properties of natural rubber ary to develop an effective method to predict the failure
and acrylonitrile rubber composites. Shirazi and Noor- behaviour of AFRC.
dermeer [7] discussed the main factors that influence In the study, four types of experiments are adopted:
the mechanical properties of aramid-short-fibre- scanning electron microscopy (SEM), uniaxial tensile
reinforced rubber composite. Mehdi [8] investigated test, multi-step stress relaxation, and Mullins exper-
the effect of aramid fibres on the static and dynamic iment. The experimental study of quasi-static properties
mechanical properties of tyres, such as rolling resist- aids in examining the effect of aramid fibres on the
ance and traction force. Despite the aforementioned mechanical properties of aramid pulp reinforced natural

CONTACT Xiaoxiang Yang yangxx@fzu.edu.cn College of Chemical Engineering, Fuzhou University, Fuzhou 350108, People’s Republic of China;
Quanzhou Normal University, Quanzhou 362000, People’s Republic of China
© 2018 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
382 J. GAO ET AL.

rubber/SBR composites under large deformations. This interface between fibre and matrix, and orientation dis-
constitutes the framework of subsequent studies on tribution of fibres (among others) are obtained. This is
the micromechanical properties of the AFRC. achieved by scanning the fracture surface, transverse
section of the stretched sample (that is perpendicular
to the x-direction in Figure 1), longitudinal section
Experimental study (that is perpendicular to the y-direction in Figure 1),
The samples used in the study were provided by a tyre and the section perpendicular to the thickness direction.
manufacturer. A small amount of aramid fibres The experimental results indicate the following: (1)
improved the overall performance of rubber products, Mutual entanglement between fibres is scarce, as
given that the aramid fibre exhibited mechanical proper- shown in Figure 2(A). This is because the stiffness of ara-
ties corresponding to high strength and modulus as well mid-short-fibre is relatively higher, and the fibre length
as the internal chemical reaction caused by aramid pulp. is short. (2) As shown in Figure 2(B), almost all the inter-
To investigate the mechanical properties of aramid fibres faces between the fibre and matrix exhibit small voids
reinforced natural rubber/SBR composites, samples with and low fibre breakage, which indicates that the failure
eight different recipes were prepared, as listed in Table 1. of the samples under tensile load mainly corresponds
The reference rubber compound (that corresponds to interface debonding and matrix tearing. (3) Given
to F0 sample in Table 1) consists of natural rubber the shear force of mechanical stirring in the mixing pro-
(Thailand SriTrangAgro), styrene butadiene rubber cess, a few fibrils of the aramid pulp are separated from
(Sinopec), carbon black N220 (Cabot), and other the main fibres, and it is easy to bond the fibrils with the
compounding agents. With respect to the AFRC, matrix due to their small diameter, thereby leading to
the mass of aramid pulp (Teijin) was valued from increases in the matrix stiffness. (4) To understand the
0 to 7 phr, while the contents of rubber matrix, car- fibre orientation, the fibre distribution in the transverse
bon black, and other compounding agents were the section (perpendicular to the x-direction), longitudinal
same. Two stages of mixing (that were completed section (perpendicular to the y-direction), and section
in the internal mixer and opening mixer) were perpendicular to the thickness direction are observed,
employed, and both the parking times were longer as shown in Figure 2(C–E), respectively. It is observed
than 8 h. All the rubber compounds were vulcanised that several fibres emerge from the face in Figure 2 (C,
in the plate vulcanising press machine under 143°C
for 45 min. The length of aramid fibre Lf was
1 mm, short fibre diameter Df was 12 μm, and the
tensile modulus Ef was 20 GPa. The constitutive par-
ameters of the rubber matrix were obtained via the
uniaxial tensile test.
Based on the China national standard GB/T2941, a
dumbbell-shaped sample of I-type is adopted, as shown
in Figure 1. A scanning electron microscope exper- Figure 1. Shape and size of the dumbbell-shaped sample.
iment, uniaxial ‘tension to fracture’ test, multi-step
stress relaxation test, and Mullins cycle experiment
were performed. Table 2 shows the details of the Table 2. Equipment and their manufacturers employed in the
main experimental equipment. current study.
Manufacturers of
Experiment type Equipment equipment
Discussion Unidirectional tensile Microcomputer control MTS Industrial
test, Mullins and electron universal Systems
Scanning electron microscope stress relaxation test testing machines (China)CO.,LTD
CMT4104
Scanning electron Scanning electron FEI America
To investigate the internal structure of composites, the microscope microscope Quanta 250
damage mode of the samples, bonding state of the experiment

Table 1. Recipes of the AFRC (phr).


Ingredients (part per 100 rubber) F0 F1 F2 F3 F4 F5 F6 F7
Natural rubber 80 80 80 80 80 80 80 80
Styrene butadiene rubber 1502 20 20 20 20 20 20 20 20
Aramid pulp 0 1 2 3 4 5 6 7
Carbon black, N220 50 50 50 50 50 50 50 50
Other ingredients 18.4 18.4 18.4 18.4 18.4 18.4 18.4 18.4
Total 168.4 169.4 170.4 171.4 172.4 173.4 174.4 175.4
Mass fraction of Aramid pulp (%) 0 0.59 1.17 1.75 2.32 2.88 3.44 3.99
Vulcanisation characteristics: Curing conditions of rubber compound 143°C × 45 min.
PLASTICS, RUBBER AND COMPOSITES 383

D), although most fibres coming out from the face in comparing the experimental results and fitting results
Figure 2(E) are absent. This indicates that the fibre is of the constitutive models, and this indicates that the
not oriented along the thickness direction of samples. large deformation constitutive model of rubber is still
Rather, it is randomly distributed in the x–y plane and applicable to the AFRC with the isotropic assumption,
is thereby perpendicular to the thickness direction (see because the fibre content is low. Specifically, both the
Figure 1). Therefore, it is concluded that it is easy for OgdenN3 and PolyN2 models [16] exhibit higher
the fibre to be oriented along the flowing direction of fitting degrees for all the samples.
the rubber compound during the processing, because The Halpin–Tsai equation [13] predicts the elastic
the stiffness of aramid-short-fibre is relatively high. modulus of short fibre reinforced composites. With
The morphology allows the sample to be considered respect to the composites with randomly distributed
as a laminate plate with randomly distributed short fibres in a plane, the empirical formula [17] of elastic
fibre, as shown in Figure 3. modulus derived from the Halpin–Tsai equation is as
follows:

Uniaxial tensile test 3 5


E = EL + ET (1)
8 8
In the uniaxial tensile tests, the loading rate is set as
1 mm min−1 for the quasi-static state of the tensile where EL denotes the longitudinal elastic modulus, and
sample. A force sensor rated at 500 N is used to ensure ET denotes the transverse elastic modulus of the com-
test accuracy. To avoid slippage of samples while posite. The empirical formula is widely used, and thus
clamping, an eccentric wheel fixture PA103A that it is continuously revised for several different materials.
tightens when the sample thickness decreases during In the study, the experimental stress–strain curve is
straining is selected. In the experiment, the sample is compared with the results from the empirical formula,
stretched until fracture, and the number of specimens as shown in Figure 5. The specific steps are as follows:
in a sample corresponds to three. the tangent modulus Etg of F0 samples at different
strain is calculated based on the test data, and they
3 Stress–strain curve are then substituted into the Halpin–Tsai empirical
To verify whether it is possible to apply the constitutive
model of rubber for large deformation to rubber com-
posites with randomly distributed short fibres, the
stress–strain curves of each sample are fitted by
PolyN2, OgdenN3, and Yeoh constitutive models.
The rubber matrix is treated as incompressible. As Figure 3. Random distribution of the short fibres in the AFRC
shown in Figure 4, good agreements are obtained by sample.

Figure 2. SEM micrographs of (A, B) fracture morphology, (C) transverse section, (D) longitudinal section, and (E) section perpen-
dicular to the thickness direction of the stretched sample.
384 J. GAO ET AL.

Figure 4. Comparison of the experimental stress–strain curves


for sample F1, F3, F5, and F7 with respect to their fitting curves
of the constitutive model.

formula to achieve the tangent modulus of AFRC at


different strains. Hence, the relationship between stress
and strain is obtained. The curves in Figure 5(A) corre-
spond to samples F1, F3, F5, and F7 samples. It is
observed that with the exception of sample F1, the
experimental results are significantly closer to that of
the empirical formula for small deformation that is
within the strain limit of approximately 0.20–0.25,
while they gradually deviate for the high fibre content
and large deformation.
Figure 5. Stress–strain curves of experimental results vs. the
Figure 5(B) shows the stress–strain curves of results of the Halpin–Tsai equation for samples F1, F3, F5,
samples F5, F6, and F7 at the initial deformation. It and F7.
is observed that increases in the sample stiffness
increase the fibre content at the beginning of loading. strength of composite increases. Evidently, the overall
This is because most of the loads are shared by the performance of a composite is closely related to the
fibres, wherein the stiffness significantly exceeds that interfacial adhesion between the fibre and matrix.
of the rubber matrix, and this leads to the high rigidity The effect of the short fibre content on tensile
of the composite materials at the beginning of loading. strength σb of the samples is shown in Figure 6. It is
observed that σb decreases with increasing fibre con-
Strength of composites tent. This result is consistent with other studies [6].
It is reported that given the fibre dilution effect within a With the exception of the error from the manufactur-
certain range of fibre content, the strength of rubber ing and test process, the main reason for the high dis-
composite reinforced by short fibres initially decreases, persion degree of the experimental data corresponds to
and then increases with increasing fibre content irre- the lower fibre content that leads to the non-uniform
spective of whether the fibre is continuous or short. distribution of the fibre in the composites, and the
This is because decreases in the fibre content decrease composites fail to realise complete isotropy. Therefore,
the fibre’s capacity to limit the overall deformation of the modulus of AFRC is potentially high in one direc-
the sample, and thus the interface between fibre and tion, although relatively low in another direction if the
matrix is destroyed under small loads. Subsequently, fibre content is low.
rubber matrix bears most of the load after the interface Figure 7 shows the effect of short fibre content on
destruction. The destruction of the interface is equival- the elongation at break δ. The elongation at break δ
ent to a void in the matrix, which results in earlier decreases if the short fibre is added to the rubber
damage to the sample. Therefore, the tensile strength matrix, and tends to steady state when the fibre content
is smaller than that in the sample without the fibre increases. With respect to the F0 sample, δ is approxi-
[18]. However, the strength of fibre dominates if the mately 510%. With respect to the F1 sample, δ corre-
fibre content is relatively high. Additionally, with sponds to 420%. However, δ is maintained at 380%
increases in the fibre content, the strength distribution when more than 4 phr of fibre is added. The main
is gradually uniform in each region of the sample. reason for the decrease in δ is that the fibre restricts
Given both the aforementioned reasons, the tensile the deformation of the sample. A potential reason for
PLASTICS, RUBBER AND COMPOSITES 385

Figure 6. Tensile strength vs. mass fraction of the fibre. Figure 9. Test for the stress relaxation and Mullins damage for
sample F2.

increasing fibre content at a fixed strain, and this indi-


cates the reinforced effect of fibre on the rubber matrix.
However, with respect to high strains (100% strain), an
upward trend is not evident, and this is because the
damage to a few interfaces between the fibre and matrix
reduces the reinforcement of the fibre at a high
deformation.

Stress relaxation test


Stress relaxation is an important characteristic of
rubber that belongs to the static viscoelastic behaviour
of materials. The rubber molecular chain is stretched
Figure 7. Elongation at break vs. mass fraction of the fibre.
along the loading direction under the external tensile
load. The thermal motion of the polymer segments
leads to molecular chain unwrapping and relative
slip, and thus the internal stress decreases. However,
given the friction between molecular chains, the change
in internal stress lags behind the change in the external
force, thereby leading to stress relaxation. To examine
the effect of fibre on stress relaxation, samples with
different mass fraction are investigated by multi-step
relaxation in conjunction with Mullins cycle tests, as
shown in Figure 9. The four curves in Figure 9 denote
the stress relaxation and Mullins cycle characteristics of
sample F2 in the case of the maximum strains corre-
sponding to 60, 128, 176, and 229%.

Viscoelasticity
Figure 8. Stress at different strain vs. mass fraction of the fibre. The classical viscoelastic model corresponds to the
Maxwell model that describes the stress variation in
the materials during the process of the stress relaxation.
the steady δ is that the increased fibre content leads to The relationship between stress and time is expressed
increases in the probability of interface failure. When as follows:
the interface is destroyed, the load is mainly under- q1 −t/p1
taken by the rubber matrix that weakens the ability s(t) = 1e (2)
p1
of the fibre to limit the sample deformation.
The four curves in Figure 8 show the effect of short where 1 denotes the step strain, and q1 and p1 denote
fibre content on the elongation stress at different viscoelastic material parameters. Figure 10 shows the
strains. It is observed that the stress increases with relationship between stress and time during the process
386 J. GAO ET AL.

Figure 11. dσ vs. nominal strain for the stress relaxation of


Figure 10. Stress vs. time at the 52% strain for samples F0, F1, each sample.
and F7.

of the stress relaxation at a strain of 52% for samples Stress drop


F0, F1, and F7. As shown in Figure 10, the stress After the Mullins cycling, the internal structure of the
value tends to be stable when the relaxation continues, rubber is increasingly steady, and this leads to steady
which satisfies the exponential function as well as the material characteristics. The deformation history of a
Maxwell model. sample significantly affects stress relaxation [19].
To investigate the effect of fibre on the stress relax- After the Mullins damage, the AFRC sample (when
ation properties of materials, the stress change is intro- reloaded) exhibits subtle stress relaxation until the
duced to evaluate the viscoelasticity of materials as strain exceeds the experienced maximum value, the
follows: stress–strain relationship returns to the primary load-
ing curve, and the stress relaxation recovers, as
smin
ds = (3) shown in Figure 9.
smax
The stress drop at a given strain is defined as follows:
in which smin and smax denote the highest and lowest Ds = smax − smin (5)
points during the process of stress relaxation, respect-
ively, as shown in Figure 9. To investigate the viscoelas- in which the meaning of smax and smin are shown in
ticity of AFRC, the relationships between ds(t) and 1 Figure 9. The stress drop of curves 1 and 2 in Figure 9
are shown in Figure 11, where the scatter points denote are shown in Figures 12 and 13, respectively. As
the experimental data, and solid and dashed lines shown in Figure 12, Ds is proportional to the strain
denote the fitting curve for the experimental data of and fibre content. Figure 13 shows the stress relaxation
samples F1 and F7, respectively. It is observed that characteristics of samples when reloading after Mullins
ds(t) increases rapidly, then tends to a constant damage, indicating the relationship between Ds and
value ds(t)′ when 1 increases. With respect to all the 1/1′max , where 1 denotes the strain of curve 2 and 1′max
samples, ds(t)′ is approximately in the range of 0.85– denotes the experienced maximum strain of curve
0.88 and is extremely close. As shown in Figure 10, 1. Given the Mullins damage, when 1/1′max is less than
the fibre content affects ds(t)′ . Thus, with increasing 0.8, the rubber chain arrangement and damages to the
fibre content, ds(t)′ decreases, indicating that the rubber matrix, fibre, and interface between the fibre
fibre weakens the viscoelasticity of composites and and matrix are almost stable. Thus Ds is constant, as
the stress relaxation. This is because the viscoelasticity shown in Figure 13. Given that the viscoelasticity is
of a composite material is caused by the rubber matrix. mainly manifested by the rubber matrix, Ds of samples
The load undertaken by the rubber matrix decreases with different fibre content only exhibit a few differ-
when the fibre content increases. Furthermore, in ences. When 1/1′max exceeds 0.8, the stress–strain
Figure 11, the strain 1′ is approximately 35% when curve gradually returns to the primary loading curve
ds(t)′ of all the samples approaches the steady state, (Figure 9). Thus, the viscoelasticity recovers, because
indicating that 1′ mainly depends on the property of the rubber molecular chain is rearranged, thereby result-
the rubber matrix, and not the fibre content. By ing in new microscopic damage.
fitting the experimental data, the relationship between
ds(t) and 1 is described as the exponential function:
Mullins damage
s(t) = AeB1 + CeD1 (4)
The Mullins effect [20] corresponds to the static soft-
where A, B, C, and D denote the material parameters. ening characteristic of the filled rubber material.
PLASTICS, RUBBER AND COMPOSITES 387

Figure 14. Strain energy distribution of rubber.


Figure 12. Maximal strain 60%, Stress drop vs. strain.

Table 3. η and permanent set of samples with different fibre


content.
F0 F2 F4 F5 F7
η (ε = 0.1) 1.153 1.460 1.626 2.066 1.733
η (ε = 0.2) 1.086 1.272 1.406 1.795 1.600
η (ε = 0.3) 1.038 1.285 1.351 1.767 1.600
η (ε = 0.4) 1.083 1.255 1.326 1.715 1.605
η (ε = 0.5) 1.076 1.229 1.338 1.490 1.603
Permanent set 5.58 × 10−5 0.063 0.028 0.034 0.028

Stress softening and permanent set


Generally, stress softening is expressed by variable η.
This variable denotes the ratio between the reloading
stress and loading stress at the same strain (h = s′ /s),
Figure 13. Maximal strain 128%, Stress drop vs. ε/ε ,max. where s′ denotes the loading stress of the virgin
sample, and s denotes the reloading stress, as shown
Given Mullins damage, the unloading stress and in Figure 14. The permanent set denotes the residual
reloading stress are significantly lower than that of extension that remains after a material sample is
primary loading at the same strain, as shown in stretched and released [20]. In this study, the perma-
Figure 9. With respect to the rubber composites nent set refers to the residual strain of the sample after
reinforced by carbon black, the microscopic Mullins unloaded. With respect to carbon black filled rubber
damage generally includes molecular chain unwrap- composites, permanent set increases with increasing
ping, short chain fracture, molecular chain slippage carbon black content [23]. With respect to the aramid
from carbon black surface, and rupture of fillers clus- short fibre-reinforced rubber composites, based on
ters. Macroscopically, we observe effects such as the experimental result, η and permanent set for
stress softening, permanent set, energy loss, and Mul- samples F0, F2, F4, F5, and F7 are listed in Table 3.
lins induced anisotropy. Given the complex micro- It is observed that for each strain, η of sample F0 is
structure in the rubber, it is still challenging to lower than that of the other samples. Furthermore,
explain the mechanism of Mullins damage and estab- increases in fibre content increase η with the excep-
lish a mechanical model given all the Mullins effects, tion of sample F7. Given that the fibre content of
and agreement is absent with respect to the origin sample F7 corresponds to largest in the study, it is
of the effect at the microscopic or mesoscopic scales not possible to ensure whether η increases if the
[20]. fibre content exceeds that of sample F7. However,
Most existing studies mainly focused on rubber the data in Table 3 indicates that the fibre intensifies
composites reinforced by carbon black or silicon the stress softening. With respect to the permanent
filler [21,22]. In this study, based on the Mullins set, sample F0 is several orders of magnitude less
experimental results, we attempt to investigate the than that of the other samples. Regularity of the per-
effect of short fibre on the Mullins stress softening, manent set for samples with different fibre contents is
permanent set, energy loss of AFRC, and microstruc- absent, owing to the low fibre content. Evidently, the
ture of composites to interpret the Mullins damage for bonding state of the interface between the rubber
AFRC. matrix and fibre is also a key factor.
388 J. GAO ET AL.

Figure 15. Comparison of the Mullins curve for F0, F2, F4, and F5 samples.

Energy loss the stiffness of the rubber are extremely rare. However,
With respect to the carbon black filled rubber, when with respect to the other three samples (F2, F4, and F5),
the sample is subjected to uniaxial tensile loading and the reloading curve does not fall at the stress equili-
unloading, the energy loss lies in the middle of the brium point. With increasing fibre content, the distance
loading and unloading curves. This is expressed as between the reloading curve and the stress equilibrium
Wdis = W1 + W2, where W1 denotes the energy dissipa- point also increases, and this implies that the stress soft-
tion during the internal reconfiguration such as frac- ening intensifies. This is because the internal damage
ture, friction, unwrapping of rubber molecular chain, with fibre is more complicated, and the fibre matrix
and rupture of fillers clusters. Additionally, W2 is interface debonding denotes the main failure mode
attributed to the friction of the rubber molecular that causes severe stress softening. Based on Figure 15,
chain motion and is considered as energy lag loss the strain energy is divided into four parts. Thus, W =
caused by rubber viscoelasticity, as shown in Figure Wela + Wdis = W’1 + W’2 + W’3 + W’4 as shown in Figure
14. However, with respect to the short fibre-reinforced 16, where W’1 (the circular scatter point part) denotes
rubber composites, the energy loss of the Mullins effect the energy loss caused by the rubber viscoelasticity,
is related to the carbon black and rubber molecular W’2 (the shaded part) denotes the energy loss caused
chains and to the fibre breakage and friction between by the friction between rubber chains and interface fric-
fibres and matrix on interfaces during debonding. tion of fibre, and matrix W’3 (the triangular scattered
Figure 15 shows the Mullins cycle experiment in con- point part) is caused by the interaction between rubber
junction with multi-step relaxation. It is observed that and fibre and mainly includes interfacial debonding and
when reloaded, the strain–stress curve of F0 simply fibre breakage. Specifically, it also includes matrix
passes through the lowest point of the stress relaxation damage caused by the effect of fibre on the matrix. Fur-
process of the primary loading curve where the stress thermore, W’4 (Unfilled part under the curve) denotes
attains a balance. Therefore, it is concluded that if the the elastic energy of the rubber molecular chain and
maximal strain of F0 is less than 60%, then only chain fibre while the molecular chain returns to the coiled
segment unwrapping or chain slippage exist in the conformation from extensional conformation.
rubber matrix, although a large amount of molecular In the aforementioned four parts of strain energy,
chains fracture and filler clusters rupture that influence W’3 directly reflects the material internal damage
PLASTICS, RUBBER AND COMPOSITES 389

failure mode, the interface debonding between


the matrix and fibre (and matrix tearing) was
dominant, while fibre fracture was rarely
observed.
(ii) The large deformation constitutive model of
rubber material was still suitable for rubber
composites with low fibre content, and the
PolyN2 model exhibited a high fitting degree
to the composites. With respect to the case of
the small fibre content and small deformation
of the sample, the stress–strain curve from the
experiment was close to the empirical formula,
while the two gradually deviated with respect
to the large content and large deformation.
Figure 16. Four parts of strain energy of short fibre-reinforced (iii) When compared with that of the sample without
rubber composites. the aramid fibre, the tensile strength and
elongation at the break of AFRC reduced,
while the stiffness increased similar to the stress
at a given strain.
(iv) The experimental results of stress relaxation
indicated that increases in the content of short
fibre decreased the load undertaken by the
rubber matrix, and this decreased the viscoelas-
ticity of the composites. This is because the vis-
coelasticity was caused by the rubber matrix as
opposed to the fibre.
(v) After the Mullins damage, the rubber chain
arrangement, matrix damage, and interface fail-
ure fibre were almost stable while the samples
were loaded within the maximum deformation
of history. Therefore, when the sample was
Figure 17. Effect of short fibre content on W’3. reloaded, the stress relaxation characteristic
was extremely weak until the stress–strain
caused by the fibre. The effect of fibre content on W’3 is relationship returned to the primary loading
shown in Figure 17. The value of W’3 increases with curve, and the original viscoelasticity sub-
increasing fibre content, and thus it is interpreted sequently recovered.
that increases in the fibre content increase the failure (vi) The existence of short fibre intensified the stress
probability of the interface. softening characteristics and increased the per-
manent set of AFRC.
(vii) The strain energy of short fibre-reinforced
Conclusion
rubber composites was divided into four parts.
In this study, SEM, tensile test, multi-step relaxation, In a future study, W’3 is a part of the strain
and Mullins experiments were performed to investigate energy that will be considered for application
the quasi-static mechanical properties of AFRCs. The in the examination of interface debonding.
strength, stiffness, viscoelasticity, and Mullins effect
of composites were investigated, and the micro-
damage mechanism was also explored. The following Disclosure statement
conclusions were obtained:
No potential conflict of interest was reported by the authors.
(i) The SEM image indicated that intertwined fibres
seldom existed, given that the aramid fibre
Funding
exhibited relatively large stiffness. The aramid
fibre was easily orientated along the flowing This work was supported by National Natural Science Foun-
dation of China: [Grant Number 11372074]; the Natural
direction of the rubber compound as opposed
Science Foundation Projects of the Fujian Province of
to the thickness direction during the moulding, China: [Grant Number 2018J01427]; Education and Scien-
and thus the sample was equivalent to laminates tific Research Program of Educational Commission of Fujian
with random fibres in a plane. In terms of the Province of China: [Grant Number JA170491]. Natural
390 J. GAO ET AL.

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