Journal of Alloys and Compounds 536S (2012) S456–S459

Contents lists available at SciVerse ScienceDirect

Journal of Alloys and Compounds
journal homepage: www.elsevier.com/locate/jallcom

Characterization of Kevlar-29 fibers by tensile tests and nanoindentation
J.A. Bencomo-Cisneros a , A. Tejeda-Ochoa a,b , J.A. García-Estrada b , C.A. Herrera-Ramírez c ,
A. Hurtado-Macías a , R. Martínez-Sánchez a , J.M. Herrera-Ramírez a,∗
a
b
c

Centro de Investigación en Materiales Avanzados (CIMAV), Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, 31109 Chihuahua, Chih., Mexico
Instituto Tecnológico de Chihuahua (ITCH), Av. Tecnológico No. 2909, 31310 Chihuahua, Chih., Mexico
Escuela Superior de Ingeniería Mecánica y Eléctrica (ESIME)-Unidad Culhuacán, Av. Santa Ana No. 1000, Col. San Francisco Culhuacán, Del. Coyoacán, 04430 México, 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 fibers
Tensile tests
Nanoindentation
Mechanical properties

a b s t r a c t
Kevlar-29 fibers are being used in different applications due of their exceptional mechanical properties. More mechanical information on these fibers is needed for better understanding of their complex
mechanical behavior. This article presents results from tensile tests on single Kevlar-29 filaments, 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
fiber cross-section is lower than that obtained in the longitudinal direction due to the high anisotropy of
the fibers.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction
Aramid fibers, 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 fibers [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 fiber axis
leading to a highly ordered structure with a high degree of crystallinity [2]. Kevlar fibers 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 fibers are related to
their particular microstructure characterized by several features
such as fibrils, radial pleated sheets and skin–core differentiation
[3–5]. A variety of techniques have been used to elucidate the
microstructure of the aramid fibers 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. García-Estrada), cahr21@yahoo.com.mx (C.A. Herrera-Ramírez),
abel.hurtado@cimav.edu.mx (A. Hurtado-Macías), roberto.martinez@cimav.edu.mx
(R. Martínez-Sánchez), martin.herrera@cimav.edu.mx (J.M. Herrera-Ramírez).
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 fiber [6]. Although there
is some confusion in the literature, it is generally accepted that
the core is less well aligned than the skin [7–9] but that this difference disappears during tensile loading due to alignment of the
molecular structure. It is clear that the molecular morphology of
the fibers is responsible for the favorable properties of aramid fibers
and it would prove extremely valuable to evaluate the mechanical
properties of the individual regions.
The longitudinal behavior of single fibers has been studied for a
long time, including Kevlar fibers [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 fiber response
to mechanical loads in other directions, such as the cross-section.
An understanding of a material’s 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 films 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 fiber 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.

SEM observations revealed that the polished Kevlar-29 fibers have a quasi-circular cross-section. 2). However the method used was the CSM. equipped with a load cell of 250 g calibrated from 0 to 100 g.10] and is attributed to the fibrillar nature of the fiber structure. Untested Kevlar-29 fibers. No differences in properties between the skin and the core were found. the diameter of each fiber was systematically measured before each test by using a Mitutoyo LSM-500S laser apparatus. Results and discussion Fig. as it is done traditionally. Prior to the tests the equipment was calibrated using a standard fused silica sample. 3. Results indicate that the stress-strain curves of Kevlar-29 fibers remain practically linear until failure (Fig. Work by Phoenix and Skelton [19] directly measured the radial properties of Kevlar fibers using the Brazilian test and revealed the high anisotropy of the fiber.J. The effects of the anisotropy of the fiber structure were clearly demonstrated by Greenwood and Rose [17] who subjected unidirectional Kevlar composites to compressive loads and reported yielding at about 0. the fibers were hand polished in order to provide a smooth exposed surface and measurements were performed in their cross-section. micrographs were taken with the AFM NanoVision G200 (Fig. A beam voltage of 1–2 kV and a working distance of 8–15 mm were used for the observations. strain rate target of 0. The fiber specimens were extracted manually from the bundles and glued to card supports so as to give a gauge length (Lo ) of 30 mm. roughness. and even swarf on the surface (Fig. for Kevlar KM2 tested in tension [16] or by Rebouillat for Kevlar-29. The tensile fracture morphology of the Kevlar-29 fibers is shown in Fig. The splitting may be the result of stress concentrators due to defects on the surface or inside the fibers. depth limit of 100 nm. The card protected the fibers from the machine grips. The nanoindentation tests were carried out by an Agilent Nano Indenter G200. of the Kevlar-29 fibers cross-section. 3. Materials and methods 1 0 0 1 2 ε (%) 3 Fig. (a) Smooth surface and (b) swarf on the surface. A field emission scanning electron microscope (JEOL JSM-7401F) was used for all observations of the fibers. In order to normalize the stress. The measurements were made radially across the cross-section of the Kevlar-29 fibers. 1b). The fibers were vertically embedded in an epoxy resin and cured in a plastic mold. These imperfections seem to come from the fiber manufacturing process. . The Young’s modulus of Kevlar-29 is about half that of Kevlar-49 [5. harmonic displacement target of 1 nm and a frequency target of 75 Hz. Young’s modulus (E).7 GPa 3 2 σ (GPa) 2. was found to be less ordered than the latter due to poorer alignment of the molecular morphology induced during manufacture. with a precision of 0. the shape of the curve almost perfectly straight is in agreement with those presented by Cheng et al. [18] revealed that the fibers were made up of radial pleated sheets superimposed on the fibrillar structure. Secondary electron emissions were used to obtain the images. This morphology will have direct effects on the physical properties of the fiber both radially and longitudinally.1 × 10−3 s−1 . [14]. hardness and Young’s modulus. After curing.3 ± 0. We used the nanoindenter to directly determine the nanomechanical properties. Stress–strain curve of a Kevlar-29 fiber showing a linear stress–strain behavior. In order to show the residual footprints of the nanoindentations. The calibration of this apparatus was performed by scanning electron microscopy (SEM). Other studies by Dobb et al. 4 the curves of the experimental nanoindentation tests for load–displacement display that the highest load reached was close to 0.2 mN. using the continuous stiffness measurement (CSM) method with a Berkovich diamond indenter with radius of 30 nm. resulting in an average value of hardness of H = 1. The tests were conducted at a strain rate of 4. 49 and 149 tested in bending [15]. Single fibers were subjected to tensile tests at room temperature using a Universal Fiber Tester developed originally by Bunsell et al. The poly(p-phenylene terephthalamide) (PPTA) fibers analyzed in this work were Kevlar-29 from DuPont de Nemours. Fibers appear essentially as smooth cylinders (Fig. with an accuracy of 0. 1a) although some of them present flaws. which was the object of this study.01 g. and failure strain (ε) are close to those reported by the supplier [1]. being highly anisotropic with a low transverse strength leading to splitting upon failure under tensile loading condition. Tensile test results carried out in this work are summarized in Table 1. / Journal of Alloys and Compounds 536S (2012) S456–S459 S457 Fig. The standard deviation shown with the results indicates that there is considerable variability in the mechanical properties of these fibers. 1 shows micrographs of the as-received Kevlar-29 fibers. 5). 1.7% strain.01 ␮m.05 s−1 . It can be seen that the values of failure stress ( R ). previously coated with gold. 2.A.2 software from Sysma. In Fig. meaning that the stiffness (S) was calculated during loading and not in the unloading.15] and therefore it is not surprising that the former fiber. which would correspond to a displacement within the surface of h = 100 nm. striations. This complex morphology is well reported elsewhere [5. they are the average of thirty measurements. Data acquisition used a PC linked to the fiber tester via a National Instrument interface card and WinATS 6. Bencomo-Cisneros et al.

A. finding also low values. 4. / Journal of Alloys and Compounds 536S (2012) S456–S459 Table 1 Tensile mechanical properties of the Kevlar-29 fibers.2 3 84. 5.7 12 2. Load–displacement curves of the nanoindentation test measurements in a Kevlar-29 fiber.7 ± 0.0 83 3.3 3. they consider that the technique underestimates the mechanical properties of the fibers. compared with the supplier’s data. compared to that reported for the modulus in compression of the fibers (63 GPa).2 ± 0.6 GPa. Yu et al. Graham et al.1 × 10−3 – and modulus of E = 20.4 GPa). whereas by nanoindentation. Bencomo-Cisneros et al. the hydrogen bonds are disrupted and not the covalent bonds. reported that the polishing procedure disrupted the surface and a no radially anisotropic structure could be observed. However. coherent results Fig. It can be noted that the elastic modulus measured by this technique is much lower than that obtained by tensile tests (Table 1).8 ± 0.5 ± 5. . Fig. 3. This damage caused the microstructure became non-crystalline and an elastic modulus too low was measured (13. The difference between these results again reflects the anisotropy of the fiber structure and could Fig. respectively.30 ± 1. SEM fractographs of Kevlar-29 fibers showing (a) and (b) severe splitting and (c) markings parallel and perpendicular to the axial direction. [6]. Sample Measured values Supplier’s data [1] Lo (mm) 30 – Diameter (␮m)  R (GPa) E (GPa) ε (%) Strain rate (s−1 ) 12. AFM image of a Kevlar-29 fiber.6 4. which applies an ultra-low load. taken by the NanoVision system coupled to the Nanoindenter G200. [20] and Gindl and Schöberl [21] used the nanoindentation technique to evaluate the modulus of bamboo and wood fibers. be attributed to the fact that under tension loads the breaking of covalent bonds occurs.S458 J. who made use of an interfacial force microscope to evaluate the mechanical properties of the core and skin regions of the Kevlar-49.

P. Janotta. 1989. W. http://www.J. A. W. J. C. Graham. T.). G. Skelton. Text Res. Mater. Young. Antúnez-Flores and O. [8] S. [4] R. P. Mater. Vincze. ATO is grateful to CONACYT-Red Temática de Nanociencias y Nanotecnología for his scholarship. R. Yu. Phys. [19] S. Amsterdam.). 127 (2005) 197–203. P. Greenwood. Saville.G.A.F. Sci. Phys. Knoff. [12] ASTM D3379-75e1. Bunsell (Ed. E 4 (1971) 868–872. R. J. in order to determine whether the nanoindentation technique underestimates the mechanical properties or the polishing procedure induces the amorphization of the fiber microstructure. 2009. Cheng. The technical assistance S459 of K. D. Riekel. They have high strength and modulus but show considerable scatter in these properties. Bunsell. [17] J. Weerasooriya.H. Lu. Roth.R. / Journal of Alloys and Compounds 536S (2012) S456–S459 (60.8 GPa) were found when they cut the samples with a microtome. 246–329. Hearle (Ed. Mater.J. H. Sci. L. J. Rebouillat.J. Handbook of Tensile Properties of Textile and Technical Fibres. J. G. Burghammer.M. O. 2011.H. M. High-Performance Fibres. pp. [20] Y. Lafitte. Rose. Conclusions Tensile test and nanoindentation technique have been used to determine the mechanical properties of single Kevlar-29 fibers. J. Yang. 354–436. References [1] Kevlar Aramid Fiber. M. Burghammer. C.R. This difference between the longitudinal and radial direction is due to the high anisotropy of the fibers. Dobb. Polym. H. Bunsell. Wang. Hunter. Cambridge. Sci. Bunsell (Ed. McCague. [7] C. J.W. Fei. A.J. T.R. Ed. C. A. Polym. but four times lower than that obtained in the longitudinal direction by tensile tests. Chen. Macromolecules 32 (1999) 7859–7865. Hearle. Mahendrasingam. Campos-Venegas. [5] A. Eng. Tian. [10] A. pp. W.O. Warren. Polymer 41 (2000) 4761–4764. P. Technical Guide. Sci. J. C. Macromolecules 39 (2006) 4834–4840. The samples tested exhibited a stress–strain behavior almost perfectly straight. Cambridge. Sci. B. Standard Test Method for Tensile Strength and Young’s Modulus for High-Modulus Single-Filament Materials. in: J.com. 9 (1974) 1809–1814. Woodhead Publishing Limited. Woodhead Publishing Limited.). 2001. 27 (1992) 5431–5440. J. [16] M.G. Phoenix. Acknowledgements This research was supported by CONACYT FOMIX-Chihuahua (147982). Mater. Traina. 1988. Therefore. 4. Technol. Solís-Canto is greatly appreciated.W. [11] ASTM D3822-01. [3] H. Holzforschung 65 (2011) 113–119. JABC was supported as a graduate student by CONACYT (239769). J. Eng. [2] M. The elastic modulus of the fibers evaluated by nanoindentation was homogeneous in all the fiber cross-section. pp. Pharr. [18] M. 44 (1974) 934–940. The fracture morphology under quasi-static loading condition presents severe splitting of the structure. M. [9] R. [14] A. Pregoretti. Dieing. Schöberl. Mater. T. Engström.S.dupont. A 253 (1998) 151–159. further studies using a microtome to prepare our Kevlar-29 fibers are needed. in: A. [6] J. Macromolecules 36 (2003) 1585–1593.F.H. J. Norton. Wang. Fibre Reinforcements for Composite Materials. [21] W. Gindl.L. Martin.A. which is induced during the drawing process. 23–61. Sci. B. Davis. Johnson. Bencomo-Cisneros et al. Elsevier.L.R. Bunsell. Mater. [13] G. Composites A 35 (2004) 1345–1349.J. Riekel. [15] S. Standard Test Method for Tensile Properties of Single Textile Fibers. D. Riekel. Davies. 15 (1977) 2201–2211. 10 (1975) 1300–1308.R. Day. .S. in: A. 17 (1982) 2391–2397.R.