Corrosion Science 64 (2012) 1–7

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Corrosion Science
journal homepage: www.elsevier.com/locate/corsci

Corrosion behaviour and crack formation mechanism of basalt fibre in

sulphuric acid
V. Nasir, H. Karimipour, F. Taheri-Behrooz ⇑, M.M. Shokrieh
Composites Research Laboratory, Mechanical Engineering Department, Iran University of Science and Technology, Tehran 16846-13114, Iran

a r t i c l e i n f o a b s t r a c t

Article history: In this investigation, the corrosion behaviour and crack formation mechanism of the basalt fibre exposed
Received 16 November 2011 to sulphuric acid were studied. For this purpose, different points of the fibre surface were examined by
Accepted 12 June 2012 SEM and EDX methods to explain the corrosion behaviour and leaching of non-siliceous ions from the
Available online 16 July 2012
fibre surface. The fracture mechanism of the basalt fibre showed that the spiral and axial cracks were gen-
erated at the higher exposure times in comparison with the E-glass fibre. The study on the strength
Keywords: behaviour of the basalt fibre also revealed that the strength degradation of the E-glass fibre was more
A. Sulphuric acid
severe than that of the basalt fibre.
B. SEM
C. Acid corrosion
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction Shokrieh et al. [16] studied longitudinal strength of fibrous com-

Polymer composites are widely used in many industries. Brittle
fracture resulting from corrosion or stress corrosion is very current
phenomenon of these materials. In other words, corrosion causes
strength degradation in the polymer composites which in return
lead them to failure in very lower mechanical stresses than their
ultimate strength. Tubes and gratings used in the chemical and
pipeline industries [1–4] and high voltage composite insulators
[5–10] made by polymer composites are current examples of com-
ponents which are degraded in the corrosive environments. As a
result, industries suffer many damages and high maintenance
prices. Due to the importance of this issue, many investigations
were carried out on the parameters affecting the corrosion of poly-
mer composites such as type of resin and fibre [10], matrix tough-
ness [11,12], concentration and temperature of corrosive
environment [13], external loads [3] and manufacturing processes
[9]. Since the main failure cause of polymer composites in the
acidic media is fibre degradation, many studies focused on this
subject such as using ECR glass fibre instead of E-glass fibre [8],
corrosion of E-glass fibre in the different acidic medias [14,15]
and corrosion behaviour and crack formation mechanism of E-glass
fibre in sulphuric acid environment [15]. Due to the sound
mechanical and chemical properties of glass fibre, this material is
well known to be utilised as reinforcement of polymer composites.
Thus, many studies were performed on the glass/polymer compos-
ites and glass fibre to evaluate their mechanical and chemical
behaviours under different corrosive environments. For instance,
⇑ Corresponding author. Tel.: +98 21 77491228; fax: +98 21 77240488.
E-mail address: taheri@iust.ac.ir (F. Taheri-Behrooz).
posites exposed to acidic environment. As a reinforcement of poly-
mer composites, basalt fibre is a novel fibre emerging in recent
years. Basalt fibre is virtually similar to the glass fibre from various
points of view like chemical composition, mechanical properties
and industrial application. Moreover, the basalt fibre has higher
tensile strength than the E-glass fibre [17]. Mentioned characteris-
tics of basalt fibres make them an appropriate replacement of the
glass fibre. Thus, the basalt fibre can be widely applied to many
industrial fields and different properties of this fibre have been
widely studied [18,19].
Nevertheless, corrosion mechanism of basalt fibre and basalt fi-
bre reinforced composites has hardly been studied. Liu et al. [20]
studied the corrosion behaviour of basalt/epoxy composites in a
salt medium. Shokrieh and Memar [21] worked on the stress cor-
rosion of basalt/epoxy composites under the bending loading in
sulphuric acid environment. Wei et al. [17] studied the effects of
NaOH and HCl environments on the corrosion behaviour of basalt
fibre. Moreover, they compared the results with corrosion behav-
iour of glass fibre. The results showed that the acid resistance of
basalt fibre was much better than its alkali resistance. Corrosion
behaviour of basalt/epoxy composites in the seawater was also
studied by Wei et al. [22]. They indicated that the anti-seawater
corrosion property of the basalt fibre reinforced composites was al-
most the same as that of the glass fibre reinforced ones. To the best
knowledge of authors, the corrosion and crack formation mecha-
nism of basalt fibre in sulphuric acid have not been studied yet.
The investigations only studied the corrosion behaviour of basalt
fibre in terms of strength degradation and mass losing.
In this research, corrosion behaviour and crack formation mech-
anism of basalt fibre exposed to sulphuric acid environment were

0010-938X/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.corsci.2012.06.028
2 V. Nasir et al. / Corrosion Science 64 (2012) 1–7

studied for the first time. The EDX (Energy Dispersive X-ray Micro-
analysis) and SEM (Scanning Electron Microscope) methods were
used to explain the role of Al3+, Ca2+ and Fe3+ ions in the corrosion
mechanism of basalt fibre. These methods were also used to ex-
plain the relation between the leaching of Fe3+ ions and damages
generated on the fibre surface. In addition, crack formation mech-
anism of basalt fibre was studied. The EDX and SEM results along
with ion depletion depth model were employed to investigate
the causes of axial and spiral cracks generated on the fibre surface.
Tensile tests were also performed on the intact and degraded fibres
to determine the strength behaviour of basalt fibre. Furthermore, a Fig. 1. Normalised strength of basalt fibre vs. immersion time (normalised standard
comparison was made between the corrosion, strength behaviour deviation (±SDV) of tests are 2.25%, 3.21%, 2.97%, 2.41%, 2.83% respectively).
and crack formation mechanism of basalt and E-glass fibre.

2. Experimental procedure

In this research, basalt fibre bundles were kept in 5 wt.% sul-

phuric acid solution for different immersion times. Thereafter, they
were removed from the solution and rinsed with de-ionised water
and finally were dried in the air. In order to study the corrosion
behaviour and crack formation mechanism of basalt fibre, some in-
tact and degraded fibre bundles were examined by quantitative
XRF based on the ASTM C982-97 standard. After that, some intact
and degraded fibre bundles were examined by SEM and EDX
analyses to investigate the element changes and crack formation
mechanism of fibres. The tensile tests were performed on the bun-
dles based on the ASTM D 3379-75 Standard. It should be noted Fig. 2. Normalised modulus of basalt fibre vs. immersion time (normalised
standard deviation (±SDV) of tests are 2.01%, 2.42%, 2.65%, 1.88%, 2.07%
that all the experiments of this paper are in accordance with those
respectively).
of Ref. [16].

3. Results and discussion

3.1. Strength behaviour of basalt fibre

The mechanical properties of intact basalt fibre are given in Ta-

ble 1 based on the tensile test results on seven specimens. The
strength, modulus and strain to failure of degraded fibres were
normalised relative to the properties of intact basalt fibres. In
Figs. 1–3, each experimental point is the normalised mean value
of seven tests. The normalised strength and modulus of basalt fibre
versus different immersion times are illustrated in Figs. 1 and 2. It
can be seen that after 720 h of immersion time, the strength and
modulus of fibre reduce 58.5% and 31.5%, respectively. Compared
to the strength behaviour of E- glass fibre in the same media for Fig. 3. Normalised strain to failure of basalt fibre vs. immersion time (normalised
192 h [16], the strength and modulus of glass fibre reduce 44% standard deviation (±SDV) of tests are 2.92%, 2.46%, 3.17%, 2.12%, 2.65%
and 37%, respectively. The strain to failure of basalt fibre is illus- respectively).
trated in Fig. 3. It is seen that after 720 h, it reduces 37% and this
reduction is 32% for E-glass fibre for the same time. It can be con-
cluded that the strain to failure of basalt fibre and E-glass fibre are ever, the modulus falls dramatically until the maximum exposure
approximately the same but strength degradation of E-glass fibre is time.
more severe than that of basalt fibre. As a result, basalt fibre can be
used as a replacement for E-glass fibre in the corrosive environ-
3.2. Corrosion mechanism
ments. Furthermore, as depicted in Figs. 1–3, strength and strain
to failure values show a rapid reduction rate during early 250 h
In order to study the corrosion behaviour of basalt fibre, the ele-
which is followed with slower reduction rate after this time. How-
ments changes of basalt fibre in sulphuric acid environment should
be determined. Thus, intact and degraded fibres exposed to acid for
200 h were examined by quantitative XRF analysis. Main chemical
Table 1
composition of intact and degraded basalt fibres are given in Ta-
The mechanical properties of intact basalt fibre.
ble 2. The results indicated that the Ca2+, Al3+ and Fe3+ ions were
Parameter Strength Modulus of elasticity Strain to failure the main non-siliceous ions involving in the corrosion of basalt fi-
(MPa) (GPa) (%)
bre. The SEM image of intact basalt fibre before exposure to acid is
Magnitude (Mean 2260 84 2.46 illustrated in Fig. 4. In this case, there is no crack and deposit on the
value)
basalt fibre surface. The EDX results of the intact basalt fibre sur-
Standard deviation 100.23 7.46 0.16
face (Fig. 4) are given in Table 3.
 V. Nasir et al. / Corrosion Science 64 (2012) 1–7 3

Table 2 3.2.1. The corrosion behaviour after 150 h immersion time

Quantitative XRF results of intact and degraded basalt fibre in sulphuric acid after The SEM images of basalt fibres exposed to sulphuric acid for
200 h.
150 h are shown in Figs. 5–7. It was seen that there was no crack
Component Na2O MgO Al2O3 SiO2 CaO Fe2O3 K2O TiO2 on the fibre and only some amount of deposits were seen on the
percentage surface. The EDX results of different marked points of fibre surface
Intact basalt fibre 1.80 4.90 16.40 49.10 8.40 14.80 1.20 3.40 showed the chemical reaction between the basalt fibres and sul-
(wt.%) phuric acid environment along with ion depletion of basalt fibres.
Degraded basalt fibre 1.60 4.50 14.20 55.80 6.80 12.60 1.40 3.10
(wt.%)
The EDX results of marked points of Figs. 5–7 are given in Table 4.
The marked points of Figs. 5a, 6a and 7a are related to those areas
which are far from the deposit regions. The results of these points
indicated the similarity between their elements composition.
Moreover, compared to the EDX results of intact basalt fibres, the
contents of Fe3+ and Ca2+ ions slightly changed and the content
of Al3+ ion reduced. It should be mentioned that Al3+ ion cannot re-
act with SO24 .The decrease of Al3+ ion of basalt fibre in the pres-
ence of HCl was also studied by Wei et al. [17]. The cause of Al3+
depletion during the basalt fibre corrosion in acidic environment
is not clear. Moreover, this behaviour was seen in the corrosion
of glass fibre in sulphuric acid but the cause of this phenomenon
was not given [14] and just some speculations were proposed.
One of them was that Ca2+ and Al3+ depletion might be two depen-
dent processes. The high amount of Ca2+ depletion might reduce
the stability of the glass structure and thus facilitating the Al3+
Fig. 4. The SEM image of intact basalt fibre. No deposits and cracks are seen on the
depletion [14]. This mechanism would be used to describe the
fibres surface. Al3+ depletion of basalt fibre. The EDX results of marked point of
Fig. 5b showed that Fe3+ and Ca2+ ions were leached out from the
fibre surface and entered in sulphuric acid environment. The Fe3+
Table 3 deposits generated on the basalt fibre surface are shown in
The EDX results of the intact basalt fibre surface. Fig. 7b. The results of marked point of this image indicated the in-
Related Element content (wt.%) crease of contents of Fe3+ and Ca2+ ions on the fibre surface and
Fig. number Na Mg Al Si K Ca Fe Ti those of Figs. 5c and 6b showed the high amount of Ca2+ deposits
4 2.37 3.65 12.94 50.33 3.31 9.45 15.73 2.22 on the basalt fibre surface. It would be concluded that after
150 h, Ca2+ and Fe3+ ions were leached out from the fibre surface.

Fig. 5. SEM image of basalt fibres after 150 h. The marked point of (a) is related to the area which is far from the deposit regions. The marked point of (b) shows the leaching of
Fe3+ and Ca2+ ions and that of (c) shows the high amount of Ca2+ deposits.
4 V. Nasir et al. / Corrosion Science 64 (2012) 1–7

Fig. 6. SEM image of basalt fibres after 150 h. The marked point of (a) shows the areas without the deposit and marked point of (b) shows the Ca2+ deposits.

Fig. 7. The marked point of (a) shows the intact area on the basalt fibre surface and that of (b) shows the Fe3+ deposits generated on the fibre surface after 150 h.

that the shape of Ca2+ deposits for different immersion times was
Table 4
almost the same but it was different with that of Fe3+ deposits.
The EDX results of marked points of Figs. 5–7.

Related Element content (wt.%)

3.2.3. The corrosion behaviour after 500 h immersion time
Fig. number
Na Mg Al Si K Ca Fe Ti 3.2.3.1. The role of Fe3+. After 500 h immersion time, SEM observa-
5a 1.63 2.80 10.38 55.23 3.14 9.91 15.01 1.90 tions showed that the some parts of the fibre were separated from
5b 2.48 3.55 11.20 59.81 4.21 6.38 10.27 2.10 the surface. The EDX results of marked points of Fig. 10 are given in
5c 0.85 0.61 6.10 38.37 1.53 44.30 7.20 1.04
Table 6. The marked layer shown in Fig. 10b which was taken apart
6a 1.31 1.91 10.66 55.98 2.61 8.96 16.24 2.33
6b 0.00 1.35 5.24 27.35 1.68 58.15 5.48 0.75
from the surface contained 22.08% Fe3+ that indicated the leaching
7a 1.92 3.61 11.50 53.27 3.26 8.58 15.72 2.14 of Fe3+ ions from the core to the fibre surface. One of the main dif-
7b 2.79 2.48 9.32 44.66 5.99 11.30 21.82 1.64 ferences between the corrosion mechanisms of E-glass and basalt
fibres could be the role of Fe3+ depletion. In the E-glass fibre, the
high content of Fe3+ is seen around the micro-cracks generated
on the fibre surface [16]. However, the EDX results revealed that
Some amounts of these ions were entered in the solution and some some parts taken apart from the basalt fibre surface have a high
of them were deposited on the basalt fibre surface. content of Fe3+. Therefore, it could be only speculated that there
is a relationship between the leaching of Fe3+ ions and the separa-
tion of some parts from the basalt fibre surface. However, it is not
3.2.2. The corrosion behaviour after 250 h immersion time
still clear that the depletion of Fe3+ can directly cause the separa-
The images of basalt fibres exposed to sulphuric acid environ-
tion of some parts from the basalt fibre surface.
ment for 250 h are illustrated in Figs. 8 and 9. It was seen that
the amount of deposits generated on the surfaces was increased.
The EDX results of marked points of these images are presented 3.2.3.2. The role of Ca2+. High content of Ca2+ deposits was also seen
in Table 5. The results of marked point of Fig. 8a, showed the high at this time (Fig. 11). High depletion of Ca2+ ions from the fibre sur-
amount of Fe3+ deposits on the fibre surface. It indicated that Fe3+ face caused some surface layers were flaked. Some kind of these
ions were leached out from the interior layers of basalt fibre to its flaking shape deposits are shown in Fig. 12. These deposits only
exterior layers. A part of the fibre taken apart from the surface is had Ca2+ content of 1.96%.
shown in Fig. 8b. The EDX results of this part revealed the high
amount of Fe3+ ions and low amount of Ca2+ ions. The Fig. 9 showed 3.3. Fracture mechanism
that the surfaces of some fibres contained higher amount of Ca2+
deposits like those fibres exposed to acid environment for 150 h. Corrosion behaviour and fracture mechanism of basalt fibre and
The difference was that the amount of deposits for 250 h was in- E-glass fibre are almost the same. Similar to corrosion mechanism
creased and the deposits spread all over the fibre surface. The of E-glass fibre, the Al3+, Ca2+ and Fe3+ ions were leached out from
EDX analysis of Fig. 9 showed the high amount of Ca2+ deposits the basalt fibre surface during different immersion times which re-
on the fibres surfaces. The surface morphologies of fibre revealed sulted in the formation of a rich Si layer at the fibre surface. The
 V. Nasir et al. / Corrosion Science 64 (2012) 1–7 5

Fig. 8. The marked point of (a) shows the high amount of Fe3+ deposits and (b) shows that a part of fibre is taken apart from the surface after 250 h.

Table 6
The EDX results of marked points of Figs. 10–12.

Related Element content (wt.%)

Fig. number
Na Mg Al Si K Ca Fe Ti
10a 3.52 6.70 26.52 33.91 3.86 3.67 17.96 3.86
10b 0.00 1.27 11.43 56.25 3.71 3.96 22.08 1.30
11 1.10 0.52 0.00 5.67 1.92 82.51 7.7 0.58
12 3.87 6.60 26.00 35.54 4.13 1.96 17.40 4.50

Fig. 9. The marked point shows the high amount of Ca2+ deposits after 250 h.

Table 5
The EDX results of marked points of Figs. 8 and 9.

Related Fig. number Element content (wt.%)

Na Mg Al Si K Ca Fe
8a 1.32 1.58 0.00 53.27 2.56 9.70 30.72
8b 0.42 1.14 12.51 59.17 3.26 2.24 20.14
9 1.60 1.02 0.00 5.67 1.92 81.20 7.72

Fig. 11. The marked point shows the Ca2+ deposit on the fibre surface after 500 h.

most apparent difference between the corrosion mechanism of ba-

salt and E-glass fibre was the role of Fe3+ ion depletion from the ba-
salt fibre surface after a specific immersion time. As mentioned
earlier, The EDX results of some layers taken apart from the fibre
surface (Fig. 10) showed the high content of Fe3+ ions at these
parts. Thus, it could be speculated that the leaching of Fe3+ ions
from the interior layers of the fibre to its exterior layer causes
formation of higher amount of Fe3+ ions in some part of the fibre
surface.
From the separation of some parts of the basalt fibre surface, it
could be concluded that the strength degradation of basalt fibre is
more severe than that of E-glass fibre. However, the strength deg-
radation results contradict this issue. In fact, it should be noted

Fig. 10. SEM image of basalt fibres after 500 h. The marked point of (a) shows the damaged part of the fibre surface and that of (b) shows a part of fibre taking apart from the
surface with high content of Fe3+.
6 V. Nasir et al. / Corrosion Science 64 (2012) 1–7

Fig. 12. Flaking shape deposits after 500 h. Fig. 15. Damaged fibres after 500 h.

Two known models were employed to describe the crack for-

that these damages on the basalt fibre surface were seen after
500 h and there was no crack and damage on the fibre surface until
this time. In contrast, after 192 h immersion of glass fibre, many
micro-cracks were generated on the E-glass fibre surface [16]. In
other words, the crack formation of the basalt fibre was generated
at the higher exposure times in comparison with the E-glass fibre.
In fact, the corrosion process is a time dependent phenomenon and
strength degradation of fibres should be studied over the time.
Moreover, after 500 h immersion time of basalt fibre, spiral cracks
(Figs. 13 and 15) and axial cracks (Fig. 14) were seen. The crack for-
mation mechanism of basalt fibre in sulphuric acid has not been
studied up to now. In this study, a scenario was developed for crack
formation of basalt fibre based on the images generated by SEM
and similarity of the fracture mechanism between the basalt and
E-glass fibre.
mation mechanism of glass fibre in acidic environment. The first
model was proposed by Metcalfe et al. [23]. The second one was
the ion depletion depth model [14]. The main problem of the first
model was that it could not give a reasonable explanation for the
formation of surface axial cracks. In addition, this model did not
consider the effects of the residual stresses generated at the fibre
surface during the fabrication process. Since axial cracks (Fig. 13)
were generated on the basalt fibre surface after 500 h exposure
time, the Metcalfe’s model was not able to describe the crack for-
mation mechanism of basalt fibre in acidic media. Based on the
ion depletion depth model, cracks generated on the basalt fibre
surface could be caused by residual stresses of fibre induced during
the fibre fabrication. They could also be formed by the shrinkage
stress initiated between the basalt fibre surface and its core. The
ion transfer between acid and fibre during fibre corrosion caused

Fig. 13. Spiral cracks on the basalt fibre surface after 500 h.

Fig. 14. Axial cracks on the basalt fibre surface after 500 h.
 V. Nasir et al. / Corrosion Science 64 (2012) 1–7
shrinkage of the outer surface of the fibre. Due to the difference in
the mechanical properties between the degraded outer surface and
the intact inner core, three-dimensional stresses were generated
all inside the fibre. Stresses caused by shrinkage of outer surface
had three axial, radial and spiral components. Unlike the residual
stresses, the shrinkage stresses were dynamic in nature and in-
creased as ion-depletion-depth of the fibre increased [14].
When the ion-depletion-depth was small, axial residual stresses
were considerable. In this case, a crack started at a point on the fi-
bre surface and tended to turn around the fibre with specific pitch
angle. However, when the ion-depletion-depth was high, hoop
stresses induced by shrinkage of outer surface was more remark-
able. In this case, because of a smaller strength of degraded surface
in the hoop direction than in the axial direction, cracks were
formed in the axial direction of the fibre. In most cases, there were
combinations of axial, hoop and spiral stresses. The SEM results
show that after 500 h, the dominant cracks are still spiral (Figs. 13
and 15). In other words, after 500 h of corrosion time, the ion
depletion depth is not high enough to generate the axial cracks.
In this case, axial cracks are only seen on a few fibre surfaces
(Fig. 14), while spiral cracks are dominantly seen in most of the fi-
bre surfaces. Thus, it can be concluded that fracture mechanism of
basalt fibre can result from combination of crack formation caused
by ion depletion depth and separation of some parts from the ba-
salt fibre surface.
4. Conclusion
(1) The comparison between the mechanical behaviour of basalt
and E-glass fibres after corrosion tests showed that strain to
failure of the basalt and E-glass fibre were approximately the
same but strength degradation of the E-glass fibre was more
severe than that of the basalt fibre. Therefore, basalt fibre
would be a suitable replacement for the E-glass fibre in the
corrosive environments.
(2) The results revealed that the fracture mechanisms of the
basalt and E-glass fibres are almost the same except in the
role of Fe3+ ions. In the E-glass fibre, the high content of
Fe3+ is seen around the areas surrounded by the micro-
cracks generated on the fibre surface. However, the EDX
analysis performed on the basalt fibre revealed that some
parts separated from the fibre surface have a high content
of Fe3+.
(3) Crack formation mechanism of the basalt and E-glass fibres
are virtually the same and they are in accordance with ion
depletion depth model. The important difference is that
the spiral and axial cracks in basalt fibre are initiated at
the higher exposure times. This is another advantage of
the basalt fibre to the E-glass fibre.
(4) Similar to the corrosion mechanism of the E-glass fibre, the
Al3+ and Ca2+ ions were leached out from the basalt fibre sur-
face during different immersion times which resulted in the
formation of a rich Si layer at the fibre surface.
7
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