Journal of Alloys and Compounds 536S (2012) S456S459

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Journal of Alloys and Compounds

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

Characterization of Kevlar-29 bers by tensile tests and nanoindentation

J.A. Bencomo-Cisneros a , A. Tejeda-Ochoa a,b , J.A. Garca-Estrada b , C.A. Herrera-Ramrez c ,
A. Hurtado-Macas a , R. Martnez-Snchez a , J.M. Herrera-Ramrez a,
a
b
c

Centro de Investigacin en Materiales Avanzados (CIMAV), Laboratorio Nacional de Nanotecnologa, Miguel de Cervantes No. 120, 31109 Chihuahua, Chih., Mexico
Instituto Tecnolgico de Chihuahua (ITCH), Av. Tecnolgico No. 2909, 31310 Chihuahua, Chih., Mexico
Escuela Superior de Ingeniera Mecnica y Elctrica (ESIME)-Unidad Culhuacn, Av. Santa Ana No. 1000, Col. San Francisco Culhuacn, Del. Coyoacn, 04430 Mxico, D.F., Mexico

a r t i c l e

i n f o

Article history:
Received 26 June 2011
Received in revised form 20 October 2011
Accepted 7 November 2011
Available online 16 November 2011
Keywords:
Kevlar
Single bers
Tensile tests
Nanoindentation
Mechanical properties

a b s t r a c t
Kevlar-29 bers are being used in different applications due of their exceptional mechanical properties. More mechanical information on these bers is needed for better understanding of their complex
mechanical behavior. This article presents results from tensile tests on single Kevlar-29 laments, to
characterize their intrinsic behavior under quasi-static loading, and nanoindentation tests, to investigate
their cross-section mechanical properties. The results reveal that the elastic modulus measured in the
ber cross-section is lower than that obtained in the longitudinal direction due to the high anisotropy of
the bers.
2011 Elsevier B.V. All rights reserved.

1. Introduction
Aramid bers, produced under the commercial name of Kevlar
by DuPont de Nemours, have a remarkable combination of high
strength, high modulus, toughness and thermal stability compared
to many other organic bers [1]. These impressive properties are
due to their molecular structure, developed during their production process which is based on liquid crystal technology, as the
rigid molecular chains form a mesophase in solution. The spinning process aligns the molecular chains parallel to the ber axis
leading to a highly ordered structure with a high degree of crystallinity [2]. Kevlar bers were developed for demanding industrial
and advanced-technology applications, such as ballistic protection
armor, helicopter blades, pneumatic reinforcement, and sporting
goods. The mechanical properties of aramid bers are related to
their particular microstructure characterized by several features
such as brils, radial pleated sheets and skincore differentiation
[35]. A variety of techniques have been used to elucidate the
microstructure of the aramid bers and several models have been

Corresponding author. Tel.: +52 614 439 48 27; fax: +52 614 439 48 23.
E-mail addresses: antonio.bencomo@cimav.edu.mx (J.A. Bencomo-Cisneros),
tejedaarmando@hotmail.com (A. Tejeda-Ochoa), jagestrada@hotmail.com
(J.A. Garca-Estrada), cahr21@yahoo.com.mx (C.A. Herrera-Ramrez),
abel.hurtado@cimav.edu.mx (A. Hurtado-Macas), roberto.martinez@cimav.edu.mx
(R. Martnez-Snchez), martin.herrera@cimav.edu.mx (J.M. Herrera-Ramrez).
0925-8388/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2011.11.031

proposed with a common feature being the differentiation of a core

and skin region within each individual ber [6]. Although there
is some confusion in the literature, it is generally accepted that
the core is less well aligned than the skin [79] but that this difference disappears during tensile loading due to alignment of the
molecular structure. It is clear that the molecular morphology of
the bers is responsible for the favorable properties of aramid bers
and it would prove extremely valuable to evaluate the mechanical
properties of the individual regions.
The longitudinal behavior of single bers has been studied for a
long time, including Kevlar bers [2,10], and some test standards
have been formulated for this intention [11,12]. In addition to the
longitudinal direction, it is necessary to study the ber response
to mechanical loads in other directions, such as the cross-section.
An understanding of a materials properties on a nanometer-scale
provides insight and understanding into that material performance
on a macroscopic scale. Ultra-low load indentation, also known as
nanoindentation, is a widely used tool for measuring the mechanical properties of thin lms and small volumes of material [13].
One of the great advantages of the technique is its ability to probe
a surface and map its properties on a spatially resolved basis,
sometimes with a resolution of better than 1 m. On the contrary,
nanoindentation does not permit the calculation of the ultimate
tensile strength. In the present paper the ber tested was Kevlar-29,
and to obtain a better and more comprehensive understanding of
its mechanical behavior, nanoindentation and longitudinal tensile
testing were jointly investigated.

J.A. Bencomo-Cisneros et al. / Journal of Alloys and Compounds 536S (2012) S456S459

S457

Fig. 1. Untested Kevlar-29 bers. (a) Smooth surface and (b) swarf on the surface.

The poly(p-phenylene terephthalamide) (PPTA) bers analyzed in this work

were Kevlar-29 from DuPont de Nemours. Single bers were subjected to tensile
tests at room temperature using a Universal Fiber Tester developed originally by
Bunsell et al. [14], equipped with a load cell of 250 g calibrated from 0 to 100 g, with
a precision of 0.01 g. The ber specimens were extracted manually from the bundles
and glued to card supports so as to give a gauge length (Lo ) of 30 mm. The card protected the bers from the machine grips. The tests were conducted at a strain rate
of 4.1 103 s1 . Data acquisition used a PC linked to the ber tester via a National
Instrument interface card and WinATS 6.2 software from Sysma. In order to normalize the stress, the diameter of each ber was systematically measured before each
test by using a Mitutoyo LSM-500S laser apparatus, with an accuracy of 0.01 m.
The calibration of this apparatus was performed by scanning electron microscopy
(SEM). The nanoindentation tests were carried out by an Agilent Nano Indenter
G200, using the continuous stiffness measurement (CSM) method with a Berkovich
diamond indenter with radius of 30 nm, depth limit of 100 nm, strain rate target of
0.05 s1 , harmonic displacement target of 1 nm and a frequency target of 75 Hz. The
bers were vertically embedded in an epoxy resin and cured in a plastic mold. After
curing, the bers were hand polished in order to provide a smooth exposed surface
and measurements were performed in their cross-section. We used the nanoindenter to directly determine the nanomechanical properties, hardness and Youngs
modulus, of the Kevlar-29 bers cross-section. Prior to the tests the equipment was
calibrated using a standard fused silica sample. A eld emission scanning electron
microscope (JEOL JSM-7401F) was used for all observations of the bers, previously
coated with gold. A beam voltage of 12 kV and a working distance of 815 mm
were used for the observations. Secondary electron emissions were used to obtain
the images.

3. Results and discussion

Fig. 1 shows micrographs of the as-received Kevlar-29 bers.
Fibers appear essentially as smooth cylinders (Fig. 1a) although
some of them present aws, roughness, striations, and even swarf
on the surface (Fig. 1b). These imperfections seem to come from
the ber manufacturing process. Tensile test results carried out
in this work are summarized in Table 1; they are the average of
thirty measurements. It can be seen that the values of failure stress
( R ), Youngs modulus (E), and failure strain () are close to those
reported by the supplier [1]. The Youngs modulus of Kevlar-29
is about half that of Kevlar-49 [5,15] and therefore it is not surprising that the former ber, which was the object of this study,
was found to be less ordered than the latter due to poorer alignment of the molecular morphology induced during manufacture.
The standard deviation shown with the results indicates that there
is considerable variability in the mechanical properties of these
bers. Results indicate that the stress-strain curves of Kevlar-29
bers remain practically linear until failure (Fig. 2); the shape of
the curve almost perfectly straight is in agreement with those presented by Cheng et al. for Kevlar KM2 tested in tension [16] or by
Rebouillat for Kevlar-29, 49 and 149 tested in bending [15]. The tensile fracture morphology of the Kevlar-29 bers is shown in Fig. 3.
This complex morphology is well reported elsewhere [5,10] and is

attributed to the brillar nature of the ber structure, being highly

anisotropic with a low transverse strength leading to splitting upon
failure under tensile loading condition. The splitting may be the
result of stress concentrators due to defects on the surface or inside
the bers.
SEM observations revealed that the polished Kevlar-29 bers
have a quasi-circular cross-section. The effects of the anisotropy of
the ber structure were clearly demonstrated by Greenwood and
Rose [17] who subjected unidirectional Kevlar composites to compressive loads and reported yielding at about 0.7% strain. Other
studies by Dobb et al. [18] revealed that the bers were made up of
radial pleated sheets superimposed on the brillar structure. This
morphology will have direct effects on the physical properties of
the ber both radially and longitudinally. Work by Phoenix and
Skelton [19] directly measured the radial properties of Kevlar bers
using the Brazilian test and revealed the high anisotropy of the ber.
In Fig. 4 the curves of the experimental nanoindentation tests
for loaddisplacement display that the highest load reached was
close to 0.2 mN, which would correspond to a displacement within
the surface of h = 100 nm. However the method used was the CSM,
meaning that the stiffness (S) was calculated during loading and
not in the unloading, as it is done traditionally. In order to show
the residual footprints of the nanoindentations, micrographs were
taken with the AFM NanoVision G200 (Fig. 5). The measurements
were made radially across the cross-section of the Kevlar-29 bers.
No differences in properties between the skin and the core were
found, resulting in an average value of hardness of H = 1.3 0.7 GPa

(GPa)

2. Materials and methods

(%)

Fig. 2. Stressstrain curve of a Kevlar-29 ber showing a linear stressstrain behavior.

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J.A. Bencomo-Cisneros et al. / Journal of Alloys and Compounds 536S (2012) S456S459

Table 1
Tensile mechanical properties of the Kevlar-29 bers, compared with the suppliers data.
Sample
Measured values
Suppliers data [1]

Lo (mm)
30

Diameter (m)

 R (GPa)

E (GPa)

(%)

Strain rate (s1 )

12.8 0.7
12

2.7 0.2
3

84.5 5.0
83

3.2 0.3
3.6

4.1 103

and modulus of E = 20.30 1.6 GPa. It can be noted that the elastic modulus measured by this technique is much lower than that
obtained by tensile tests (Table 1). The difference between these
results again reects the anisotropy of the ber structure and could

Fig. 4. Loaddisplacement curves of the nanoindentation test measurements in a

Kevlar-29 ber.

be attributed to the fact that under tension loads the breaking of

covalent bonds occurs, whereas by nanoindentation, which applies
an ultra-low load, the hydrogen bonds are disrupted and not the
covalent bonds. Yu et al. [20] and Gindl and Schberl [21] used
the nanoindentation technique to evaluate the modulus of bamboo and wood bers, respectively, nding also low values; they
consider that the technique underestimates the mechanical properties of the bers. Graham et al. [6], who made use of an interfacial
force microscope to evaluate the mechanical properties of the
core and skin regions of the Kevlar-49, reported that the polishing procedure disrupted the surface and a no radially anisotropic
structure could be observed. This damage caused the microstructure became non-crystalline and an elastic modulus too low was
measured (13.4 GPa), compared to that reported for the modulus
in compression of the bers (63 GPa). However, coherent results

Fig. 3. SEM fractographs of Kevlar-29 bers showing (a) and (b) severe splitting and
(c) markings parallel and perpendicular to the axial direction.

Fig. 5. AFM image of a Kevlar-29 ber, taken by the NanoVision system coupled to
the Nanoindenter G200.

J.A. Bencomo-Cisneros et al. / Journal of Alloys and Compounds 536S (2012) S456S459

(60.8 GPa) were found when they cut the samples with a microtome. Therefore, further studies using a microtome to prepare our
Kevlar-29 bers are needed, in order to determine whether the
nanoindentation technique underestimates the mechanical properties or the polishing procedure induces the amorphization of the
ber microstructure.

4. Conclusions
Tensile test and nanoindentation technique have been used to
determine the mechanical properties of single Kevlar-29 bers.
The samples tested exhibited a stressstrain behavior almost perfectly straight. They have high strength and modulus but show
considerable scatter in these properties. The fracture morphology
under quasi-static loading condition presents severe splitting of the
structure. The elastic modulus of the bers evaluated by nanoindentation was homogeneous in all the ber cross-section, but four
times lower than that obtained in the longitudinal direction by
tensile tests. This difference between the longitudinal and radial
direction is due to the high anisotropy of the bers, which is induced
during the drawing process.

Acknowledgements
This research was supported by CONACYT FOMIX-Chihuahua
(147982). JABC was supported as a graduate student by CONACYT
(239769). ATO is grateful to CONACYT-Red Temtica de Nanociencias y Nanotecnologa for his scholarship. The technical assistance

S459

of K. Campos-Venegas, W. Antnez-Flores and O.O. Sols-Canto is

greatly appreciated.
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