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Composite Structures
journal homepage: www.elsevier.com/locate/compstruct
a
Shanghai Center for High Performance Fibers and Composites, and Center for Civil Aviation Composites of Donghua University, Donghua University, Shanghai 201620,
China
b
Key Laboratory of Textile Science & Technology of Ministry of Education, College of Textiles, Donghua University, Shanghai 201620, China
c
Innovation Center for Textile Science and Technology, Donghua University, Shanghai 201620, China
Keywords: To improve the stab resistance but decrease the weight of the stab-resistant clothing, coated stab-resistant
Stab-resistant composites composites have been prepared by coating aramid fabric with boron carbide (B4C)/epoxy resin. At first, B4C
B4C particles dispersion was prepared and a three-factor, four-level orthogonal experiment was designed to determine the
Quasi-static puncture optimal dispersion combination. It was shown that when the particle diameter is 2.5 μm, mass fraction is 49%
Mechanism
and stirring temperature is 30 °C, the particle dispersion is the most uniform, with the highest relative sedi-
mentation height. Then, the B4C dispersion was mixed with the expoxy resin and coated onto the aramid fabric,
after which, stiffness, pulling-out, tearing and quasi-static puncture tests were conducted on the coated fabric.
The results showed that the stab resistance increases with the decrease in particle diameter as well as the
increase in particle mass fraction. For coated composites, the ultimate puncture load per weight reached 486 N/
g, 428% higher than that of uncoated samples. The anti-stinging mechanism of the coated composites has also
been investigated by analyzing the surface and fracture morphologies and the load-displacement curves.
⁎
Corresponding author at: Key Laboratory of Textile Science & Technology of Ministry of Education, College of Textiles, Donghua University, Shanghai 201620,
China.
E-mail address: quan@dhu.edu.cn (Z. Quan).
https://doi.org/10.1016/j.compstruct.2019.111370
Received 13 May 2019; Received in revised form 2 August 2019; Accepted 4 September 2019
Available online 05 September 2019
0263-8223/ © 2019 Elsevier Ltd. All rights reserved.
M. Xia, et al. Composite Structures 228 (2019) 111370
results showed that the addition of B4C particles improved the stab
resistance of the coated fabric significantly. Furthermore, the anti-
together in the weight proportion of 1:0.85 and heated in an oven at
stinging mechanism of the coated composites was investigated by
60 °C for 30 min to improve the fluidity. The B4C dispersion was added
analyzing the surface and fracture morphologies and the load-dis-
into the resin/curing agent mixture in a certain predetermined amount
placement curves.
and stirred evenly. Then the coating liquid was coated onto the aramid
fabric by screen printing and the thickness of the coating was controlled
2. Materials and methods
between 80 μm and 150 μm [26]. The coated samples were heated at
80 °C for 15 min, to get rid of excess ethanol, and at 120 °C for 1 h, to
2.1. Materials and instruments
obtain B4C particle coated stab-resistant composites.
Materials: B4C particles with four different diameter (2.5, 5, 10, and
20 μm) (Mudanjiang Diamond Carbide Co., Ltd., Mudanjiang, China),
2.3. Characterization of coated stab-resistant composites
ethylene glycol (Hongsheng Chemical Fine Co., Ltd., Xingtai, China),
ethanol (Shanghai Ling Feng Chemical Reagent Co., Ltd. Shanghai,
2.3.1. Flexibility test
China), epoxy resin (Changshu Jiafa Chemical Co., Ltd., Changshu,
To test the effects of B4C fillers on the flexibility of coated compo-
China), curing agent (Changshu Jiafa Chemical Co., Ltd., Changshu,
sites, coated composites samples were evaluated by cantilever beam
China), aramid 1414 fabric (Guangxi Wanwei New Material Co., Ltd.,
method, with the coated and uncoated side as the bottom side, re-
Nanning, China) with thickness of 0.22 mm and areal density of 200 g/
spectively. The tests were accord with the GB/T 18318-2001 standard
m2.
(Fig. 1). The sample was cut into 150 mm × 25 mm slim bar, where
Instrument: DF-101S magnetic stirrer (Shanghai Lingke Industrial
a:b = 1:3 and one end was fixed while the other end hanged a weight of
Development Co., Ltd., Shanghai, China), DHG-9145A oven (Shanghai
5 g. The sagging height (h) of the sample was measured to evaluate the
Yiheng Scientific Instrument Co., Ltd., Shanghai, China), HD026N+
flexibility of coated composites. Larger the h, more flexible the sample;
electronic fabric strength meter (Beijing Weixin Yiao Technology
and vice versa.
Development Co., Ltd., Shanghai, China), KM-SY3050 screen printer
(Kai Trade Machinery Equipment Factory, Shenzhen, China), lab-built
quasi-static puncture machine, BTY-506 USB digital microscope
2.3.2. Single-bundle pulling-out test
(Shenzhen Youpin Zhishang Technology Co., Ltd., Shenzhen, China).
Among puncture damages, fiber pulling-out in the fabric is a
common one, i.e., the fiber pulling-out behavior is closely related to the
2.2. Preparation of coated stab-resistant composites
puncture resistance. Here, the single-bundle pulling-out tests were
conducted according to the Ref. [27].
2.2.1. Preparation of B4C dispersion
A three-factor, four-level orthogonal test was designed by taking
B4C particle diameter, mass fraction and mix temperature as the in-
fluencing factors and relative sedimentation height as the index, as
shown in Table 1. First, an appropriate amount of B4C particles were
added into the mixture of ethylene glycol and ethanol (ethylene gly-
col:ethanol = 1:1 in weight). Then, the mixture was magnetically
stirred for 30 min to obtain a uniform B4C dispersion. Finally, the dis-
persion was transferred into a measuring cylinder, standing for 90 min
to measure the relative sedimentation height (the ratio of turbid section
height /dispersion total height), based on which the optimal combi-
nation of factors for dispersion was determined.
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M. Xia, et al. Composite Structures 228 (2019) 111370
Smaller the B4C particle diameter, more uniform the dispersion is,
2.3.3. Tearing test and easier it is for the particles to diffuse into the aramid fabric, fa-
In the process of puncture, a triangle area is generated around the cilitating the local slippage of fibers and, thus, improving the total
cut edge, which has a significant influence on the stab-resistance per- flexibility of the coated composites. As a result, with the increase in
formance. Therefore, tearing tests were carried out, according to British particle diameter, the sagging height of coated composites decreased.
industrial standard BS3424 method 7A [28]. Sagging height for particle diameter 2.5 μm increased by14% compared
to that of uncoated composites, while the height for particle diameter
2.3.4. Quasi-static puncture test 20 μm is almost the same as that of the blank sample (Fig. 3a). Also, the
To conduct the quasi-static puncture tests, a lab-built tester was particles play an important role in hindering the propagation of cracks
developed based on HD026N+ electronic fabric strength tester, of in resin matrix and improving the toughness of the resin matrix. As
which the head for bursting was replaced by a standard knife as shown shown in Fig. 3b, the sagging height gradually increased with the in-
in Fig. 2. During tests, circular specimens of 80 mm in diameter were crease in B4C mass fraction, reached the maximum value when the mass
fixed and the knife was moved upward at a constant speed of 5.1 mm/s fraction was 30%, and then fell down. It can also be seen that the
(0.2 in./s). The load-displacement curve was recorded by the sensor. sagging height of coated side is higher than that of the uncoated side,
indicating that the coating improved the rigidity of sample.
2.3.5. Surface and fracture morphology observation
To further analyze the anti-stinging mechanism of the hard particles 3.3. Pulling-out load and elongation of coated composites
coated composites, the surface and fracture morphology of the coated
composites was observed with a magnification of 500× using the BTY- As mentioned before, B4C particles could promote the local slippage
506 digital microscope. of fibers and yarns. As the particle diameter decreased and the mass
fraction increased, a larger number of B4C particles were dispersed
3. Results and discussions between the yarns. As shown in Fig. 4, the pulling-out load and elon-
gation of coated composites increased as the B4C particle diameter
3.1. Uniformity of B4C dispersion decreased and the mass fraction of B4C increased. With the particle
diameter of 2.5 μm and mass fraction of 40%, the pulling-out load and
To disperse B4C particles in the solution evenly and ensure the elongation of coated composites increased by 227% and 237%, re-
uniformity of the subsequent coating solution, the relative sedimenta- spectively, compared to those of uncoated samples.
tion height of B4C particles in the dispersion solution was measured
(Table 2), based on which, the optimal combination of the factors for 3.4. Tearing load of coated composites
preparing dispersion solution has been determined. Larger the relative
sedimentation height, more uniform the dispersion is. Tear failure is very common and typical in stab-resistant fabric. As
It can be seen that RA > RB > RC, i.e., particle diameter has the shown in Fig. 5, the coated composites without B4C particles showed a
largest influence on the uniformity of B4C dispersion, followed by mass “brittle” failure behavior under single tongue tear test, breaking along a
fraction and stirring temperature. With the increase in particle certain angle to the direction of pre-cut crack without any obvious
stretching or slippage of fibers. In contrast, for the coated composites
Table 2 with B4C particles, an obvious triangle zone was formed at the tearing
Relative sedimentation height. tip, which was attributed to the fiber pulling-out and slippages under
Number A – Diameter B – Mass fraction (wt C – Stirring temperature tearing load.
(μm) %) (°C) As shown in Fig. 6, with the decrease in B4C particle size and the
increase in mass fraction, more particles were filled between the yarns,
K1 3.88 3.11 3.65
which improved the slippage of yarns, and more yarns were involved in
K2 3.69 3.48 3.71
K3 3.09 3.72 3.29 the triangle zone to share the tearing load. Thus, the tearing load of
K4 3.38 3.73 3.39 coated composites was enhanced.
k1 0.97 0.78 0.91
k2 0.92 0.87 0.93 3.5. Composites surface and fracture morphology
k3 0.77 0.93 0.82
k4 0.85 0.93 0.85
R 0.2 0.15 0.11 3.5.1. Composites surface morphology
The surface morphology of coated composites with different particle
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M. Xia, et al. Composite Structures 228 (2019) 111370
diameters was given in Fig. 7a, where the mass fraction was 40%. With 3.6. Ultimate puncture load and displacement
the diameter of B4C particles decreasing, more and more particles were
observed covering on the fabric surface evenly, which is beneficial to As shown in Fig. 9a, when the B4C diameter was not too large, the
the stab resistance. Especially, when the particle diameter was 2.5 μm, ultimate puncture load per weight and corresponding puncture dis-
the hard particles not only covered on the surface of the fabric, but also placement of the coated composites could be enhanced significantly.
diffused into the inter-yarn and inter-fiber gaps. During puncture tests, The maximum puncture load per weight reached 486 N/g, 428% higher
the blade would be passivated by hard particles. Fig. 7b presents the than that of the composites without B4C particles. As the particle dia-
surface morphology of coated composites with different mass fractions meter increased, the loads and displacements reduced. When the par-
of B4C particles, when the particle diameter was 2.5 μm. As the mass ticle diameter got as large as 20 μm, due to the poor diffusion of particle
fraction increased, more particles were observed on the surface of in fabric, the load per weight and displacement were lower than those
aramid fabric and between the fibers compactly, which would improve of the blank samples. As shown in Fig. 9b, the ultimate puncture loads
the stab resistance. per weight and the corresponding puncture displacements of the coated
composites increased gradually with the increase in B4C mass fraction,
until the mass fraction reached 40%, that could be attributed to the
3.5.2. Composites fracture morphology increased number of particles and the decreased gaps between adjacent
Fracture morphology of the coated composites was shown in Fig. 8. particles.
While almost none fiber was pulled-out for the composites without B4C A typical load-displacement curve of puncture test was shown in
particle, typical fiber pull-out phenomena were observed on both the Fig. 10. In section a–b, the knife began to touch the composite sample
coated and uncoated sides of the coated composites with B4C particles, and the sample deformed elastically, so the puncture load remained
indicating that the addition of B4C particles weakens the fiber-matrix low. With the continuous increase of the displacement, the load began
adhesion and, thus, makes the slippage of fibers easier. Besides, due to to increase rapidly until reached the ultimate value (section b–c). With
the lack of coating, more fibers were pulled-out on the uncoated side load increasing, at point c, the knife started to penetrate into the sample
than on coated side. As the particle diameter decreased and the mass and the puncture load dropped dramatically (section c–d). During the
fraction increased, more particles were filled between the fibers, facil- knife penetrating through the sample, puncture load fluctuated with the
itating the fiber slippage and pull-out even more, so that more energy puncture displacement, due to the local deformation and fracture of the
could be absorbed. With the mass fraction of 40% and diameter of composite sample, through which the puncture energy was absorbed
2.5 μm, B4C particles distributed between the fibers were in continuous gradually.
strip shape, indicating that smaller particle diameter and larger mass
fraction lead to denser and more uniform coating.
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M. Xia, et al. Composite Structures 228 (2019) 111370
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M. Xia, et al. Composite Structures 228 (2019) 111370
Fig. 7. Surface morphology of coated composites: (a) different particle diameters, (b) different mass fractions. (500×, scale bar: 100 μm).
Fig. 8. Fracture morphology of coated composites: (a) different particle diameters, (b) different mass fractions. (500×, scale bar: 100 μm).
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M. Xia, et al. Composite Structures 228 (2019) 111370
Fig. 9. Ultimate puncture load per weight and corresponding puncture displacement of coated composites.