Materials and Design 31 (2010) 4244–4250

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Materials and Design

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Tensile behavior contrast of basalt and glass fibers after chemical treatment
Bin Wei b, Hailin Cao a,c,*, Shenhua Song b
a
Harbin Institute of Technology, Harbin 150001, China
b
Shenzhen Graduate School, Harbin Institute of Technology, Xili, Shenzhen 518055, China
c
Shenzhen Aerospace Tech-Innovation Institute, Shenzhen Key, Laboratory of Composite Materials, Shenzhen 518057, China

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

Article history: Basalt and glass fibers were treated with sodium hydroxide and hydrochloric acid solutions respectively
Received 12 January 2010 for different periods of time. Both the mass loss ratio and the strength maintenance ratio of the fibers
Accepted 5 April 2010 were examined after the treatment. The morphologies of the fiber surfaces were characterized using
Available online 9 April 2010
scanning electron microscopy and their compositions were analyzed using energy dispersive X-ray spec-
troscopy. For the basalt fibers, the acid resistance was much better than the alkali resistance. Neverthe-
Keywords: less, for the glass fibers, the acid resistance was nearly the same as the alkali resistance. Based on the
B. Fibers and filaments
experimental results, possible corrosion mechanisms are addressed.
E. Corrosion
F. Microstructure
Ó 2010 Elsevier Ltd. All rights reserved.

1. Introduction is very sensitive to a corrosive environment [8,9]. Many attempts

High performance filaments are frequently used as the rein-
forcement of the composites, such as carbon fibers, glass fibers
and ceramic fibers. Fibers in the composites are known to confer
strength and rigidity to the weak matrix. Most of the external load
is undertaken by the reinforcement filaments when the materials
are in service [1,2]. Chemical corrosion on the composites is
unavoidable in some applications. For example, some containers,
vessels, tubes, off-shore platforms and equipments in marine
applications may be corroded after long-term service in an alkali
environment. It is believed that one of the obstacles preventing
the extensive use of composites is the lack of long-term durability
and performance data when servicing in critical environments.
Consequently, it is necessary to understand how the materials be-
have during long-term applications [3,4].
Most of the previous studies on the degradation of the rein-
forcement fibers in chemical environments are focused on the fab-
ricated materials in which the fibers are covered by the matrix. As
shown in Refs. [5–7], the resistance of the filament to corrosion is
mainly dependant on the resin’s corrosion-resistance, and the cor-
rosion crack propagation is also related to the resin toughness. The
lack of complete understanding of the basic mechanisms of dam-
age and degradation of the fiber is obvious. Damage on the fiber
surface may be noticed after a prolonged exposure in the critical
environment. It is also indicated that the glass fiber under stress
* Corresponding author at: Harbin Institute of Technology, Harbin 150001, China.
Tel./fax: +86 0755 26996829.
E-mail address: caohl@hit.edu.cn (H. Cao).
have been made to investigate the response of the glass fiber rein-
forced products to the critical environment [10–17]; but only a lit-
tle attention has been paid to the fiber itself [18,19].
Basalt fiber is a novel fiber appearing in recent years. It has high
strength, excellent fiber/resin adhesion and ability to be easily pro-
cessed using conventional processes and equipments. In addition,
the basalt fibers do not contain any other additives in a single pro-
ducing process. This makes them have an additional advantage in
cost. As known, the basalt fibers have higher tensile strength than
the E-glass fibers and their strain to failure is larger than the car-
bon fibers. In addition, they have high chemical stability and sound
mechanical properties as well as being non-toxic and non-combus-
tible [20]. For these reasons, the basalt fibers could be widely ap-
plied to many fields, such as corrosion-resistance stuff in the
chemical industry, wear and friction stuff in the automobile indus-
try, target area of anti-low velocity impact, reinforcing material in
construction, and high temperature-insulation of automobile cata-
lysts [21–25]. The basic properties of basalt and E-glass fibers are
shown in Table 1.
Because the long-term chemical resistance of mineral fibers
cannot be explicitly measured or determined, they are generally
compared to each other after accelerated aging at fixed experi-
ment conditions. The corrosion rate is decided by numerous
parameters such as temperature, aging time, composition of the
fibers, the component of the aging solution, and also the fiber siz-
ing [26]. The aim of the present work was to investigate the di-
rect effects of NaOH and HCl on the performance filaments of
basalt and glass fibers, excluding the influence of the matrix
and revealing clear and accurate response of the fibers to the
chemical corrosion.

0261-3069/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2010.04.009
 B. Wei et al. / Materials and Design 31 (2010) 4244–4250 4245

Table 1 50
Mechanical property of basalt fibers. basalt fiber
Property Basalt Glass (E-glass) glasa fiber
Tensile strength (MPa) 2600 2500
40
Filament diameter (lm) 13 12

Mass loss ratio/ %

Yarn fineness (tex) 800 1200
Elastic modulus (MPa) 90 75 30
Elongation at failure (%) 3.1 4.7
Sizing content (%) 0.1 0.2

20

2. Experimental procedures
Basalt fibers (produced by Shenzhen Academy of Aerospace
Technology, China, one bundle has 2400 fibers) and glass fibers
(Type E, produced by PPG Company, US, one bundle has 4000 fi-
bers) were used. The specific mass of the fibers was 800 tex for ba-
salt fibers with an average diameter of 13 lm and 1200 tex for
glass fibers with an average diameter of 12 lm. Their compositions
are listed in Table 2.
The two kinds of fiber were treated in NaOH and HCl solutions
with a concentration of 2 mol/l, respectively. Before the treatment,
all the filaments were washed using the acetone in order to clean
the fiber surface. The treating time ranged from 0.5 to 3 h and
the experimental solution maintained at boiling point during the
whole process. After treatment, the filaments were immersed in
distilled water for 24 h, removing the residual chemical softly.
The mass losses of fibers after the treatment were examined using
an electronic analytical balance with a precision of 0.001 g. Assum-
ing the mass of initial state fibers is m0; the mass of treated state
fibers is m1, then mass loss ratio equals to (m0  m1)/m0. Both be-
fore and after the treatment, the specimens were dried in an oven
at 105 °C for 3 h in order to make the metage accurate.
Tensile strength of the filaments before and after the treatment
was measured. Since a single fiber was too delicate to handle espe-
cially after treated, the bundle strength was measured. The fiber
multifilament strength was measured according to GB/T 7690.1-
7690.6-2001 using a multiple mechanical tester manufactured by
SANS, China. The distance between the two collets of the specimen
was kept 500 mm and the crosshead speed was 200 mm/min. All
the samples were maintained under an environment of relative
humidity 65% and 25 °C for 24 h before the test. Ten specimens
were tested for each condition and the mean value of the data
points obtained was taken as the measured result.
The surface morphologies of the basalt and glass fibers before
and after the treatment were characterized using a Hitachi S-
4700 field emission gun scanning electron microscope (FEGSEM)
equipped with an energy dispersive X-ray spectrometer (EDS,
manufactured by EDAX Inc., US).
3. Results and discussion
3.1. Hydrochloric acid aqueous solution treatment
Fig. 1 shows the mass loss ratio as a function of treating time for
the two types of fiber. As seen, the mass loss ratio increases sharply
before 0.5 h for both types of fiber. After that, it rises slowly until
1 h and keeps stable with further increasing treating time for the
10
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Treating time/ h
Fig. 1. Mass loss ratio-treating time behavior (acid treatment). The error bars
represent the standard deviation for the estimate of the mean mass loss of ten
samples.
basalt fibers, while it increases continuously and slowly until the
maximum treating time (3 h) for the glass fibers. In addition, the
mass loss ratio is much lower for the basalt fibers than that for
the glass fibers (3 times lower). As a result, the basalt fibers are
much more resistant to acid corrosion as compared with the glass
fibers.
The tensile behavior of the two types of fibers after acid treat-
ment is represented in Fig. 2. Apparently, compared with the origi-
nal value, the strength drops dramatically for both types of fiber
until 0.5 h. After that, the strength of the glass fibers falls slowly
with further increasing treating time until the maximum treating
time (3 h). However, for the basalt fibers, after 0.5 h the strength
decreases slowly until 1 h and then increases a little with further
extending treating time.
The surface morphologies of acid-treated and untreated glass fi-
bers are shown in Fig. 3. Seemingly, there is little change in the sur-
face morphology after acid treatment. But it may be seen that there
are local amplificatory cracks with a size in a range of a few hun-
dred nanometers on the fiber surfaces (see Fig. 3c, the arrowed
position).
Fig. 4 shows SEM images and EDS spectra of the basalt fibers be-
fore and after acid treatment. The surfaces of the basalt fibers are
seriously damaged after the treatment for 1 h (see Fig. 4b). The
cracks extend along the axial direction, and also extend into the
interiors of the fibers at the same time. After 3 h treatment, the
damaged surfaces are partially healed (see Fig. 4c). Probably the
cracks are filled with some chemical reaction products. This could
account for the increase in the tensile strength test of the basalt fi-
bers with further treatment after 1 h. Of course, the tensile
strength loss cannot be totally offset by the healing effect. The
EDS spectra are presented here to indicate the composition change
of the basalt fiber surface after acid treatment, and the microanal-
ysis results are shown in Table 3. As seen, the concentrations of the
elements in the fiber are decreased due to the treatment except Si
and Ti, and the decrease becomes severer with increasing treating
time. This phenomenon is totally different from the work of Majb-

Table 2
Chemical compositions of the basalt and glass fibers (wt%).

Composition SiO2 Al2O3 CaO MgO K2O Na2O FexOy TiO2 B2O3
Basalt fiber 48.39 14.7 7.7 4.7 1.6 3.0 15.3 3.8 –
Glass fiber 52.1–53.4 13.5–14.5 18.5–19.5 3.6–4.4 0–1 0–0.6 0–0.5 8.0–9.0
4246
100
Strength maintenance ratio/%
80
60
40
20
0 Fig. 5 shows the SEM images of the basalt fiber cross-sections.
0.0 0.5 1.0 1.5 2.0
Treating time/ h
Fig. 2. Strength maintenance ratio-treating time behavior (acid treatment).
ritt D. Lund and Yuan-Zheng Yue. They measured the aging behav-
ior of basalt fibers under water medium and found water aged fi-
bers show a decrease of the relative amount the elements Na,
Mg, Al and K compared to Si qualitatively [27]. The concentration
of Si is increased substantially with increasing treating time and
becomes about 52.5 wt% after 3 h treatment. The concentration
of Ti does not change apparently due probably to its stable chem-
ical properties. It is interesting to note that the strength of the ba-
salt fiber does not decrease with further increasing treating time
after 1 h treatment. This may be because the content of SiO2 in
the fiber surface layer increases with treating time (see Table 3).
The SiO2 may be beneficial to corrosion-resistance and partially
offset the damaging effect of the acid solution. In the silicate glass
b c
Fig. 3. SEM images of glass fibers before and after treatment in HCl solution (a – original fiber; b – after 1 h treatment; c – after 3 h treatment).
B. Wei et al. / Materials and Design 31 (2010) 4244–4250
structure, the silicon dioxide plays a role of the net former and the
basalt fiber alumina plays a dual role of the net former and modifier. This case
glass fiber also applies to the basalt fibers [28]. During the first 1 h treatment,
the constituents of the basalt fiber, such as Ca, Mg, Al, Fe, Na and K,
are dissolved into the solution. It makes the framework damaged,
especially by the framework former elements (Al and Fe). After
that, the whole chemical reaction of the basalt fibers with acid
may be over. And then the subsequent 2 h treatment is an absorb-
ing/transferring process that some elements migrate from solution
onto the basalt fiber surface including the surface of cracks under
the driving force of chemical gradient. Consequently, the surface
flaws of the basalt fibers are partially healed and the crack tips
are passivated. Edith Mäder has proved the fact [29] that the glass
fiber defects (flaws) can be healed by the nanometer-scale rein-
forcement (nanotubes, nanoclays).
2.5 3.0
As seen, after 1 h treatment a corrosion layer appeared around
the basalt fibers, and the corrosion layer became even thicker with
a thickness of 2–3 lm after 3 h treatment. From Fig. 5 with refer-
ence to Table 3, we could guess SiO2 is dominant in the corrosion
layer. Therefore, there may be another reason concluded that
causes the strength increase after 3 h treatment in hydrochloric
acid solution: that is the formation of like high silica glass fiber
organization.
It may be concluded from the above that the strength loss due
to acid corrosion is less for the basalt fibers than for the glass fibers,
i.e., the basalt fibers are more resistant to acid corrosion than the
glass fibers.
3.2. Sodium hydroxide aqueous solution treatment
The mass loss ratio is represented in Fig. 6 as a function of treat-
ing time for the two types of fibers in alkali environment. As
 B. Wei et al. / Materials and Design 31 (2010) 4244–4250 4247

a
Spectrum1 Spectrum1

b
Spectrum 2

c
Spectrum 3 Spectrum 3

Fig. 4. SEM images and EDS spectra of the basalt fiber surfaces before and after treatment in HCl solution (a – original fiber; b – after 1 h treatment; c – after 3 h treatment).

Table 3 a little until 3 h. Compared with the glass fibers, the mass loss ratio
Surface concentrations of elements in the basalt fibers before and after acid treatment of the basalt fibers are much larger.
(wt%). Tensile strength maintenance ratio of the two types of fibers
Element O Si Na Mg Al K Ca Ti Fe treated by NaOH is presented in Fig. 7. The ratio decreases sharply
Untreated 41.8 26.9 2.6 2.9 8.2 1.3 5.3 2.6 8.4 and almost reaches below 20% after 0.5 h treatment. Then with
1h 38.9 32.9 1.7 2.2 7.7 1.1 4.9 2.5 8.1 increasing treatment time, the tensile strength of the fibers contin-
3h 35.4 52.5 0.2 0.7 3.4 0.4 1.9 2.2 3.3 ues to fall until non-strength. It is also seen from Fig. 7 that the de-
crease rate of the tensile strength for the glass fibers is a little
lower than that for the basalt fibers. This may be because the
framework (mainly composed of Si and Al) in the glass fibers is
shown, the mass loss ratio increases sharply before 2 h for the ba- more compact than that in the basalt fibers. The Ca element is
salt fibers. After that, it keeps stable with further increasing treat- more in the glass fibers than in the basalt fibers and the reaction
ing time. The mass loss rate of the basalt fibers is somewhat larger products (compound containing a plentiful of Ca element) on the
than that presented in the literature (5%) [30,31]. However, for fiber surface could effectively prevent the reaction further develop-
the glass fibers, the mass loss rate becomes slower after 0.5 h ing [32].
and the mass loss ratio reaches a maximum value after treating Fig. 8 shows the surface morphologies of the two types of fibers
for 1 h. Then it keeps stable until 2 h, and subsequently decreases after 3 h treatment in a 2 mol/l NaOH solution. There is a flake
4248 B. Wei et al. / Materials and Design 31 (2010) 4244–4250

Fiber

Matrix

b c

Corrosion layer
Corrosion layer

Fig. 5. SEM images of the basalt fiber cross-sections before and after treatment in HCl solution (a – original fiber; b – after 1 h treatment; c – after 3 h treatment).

8 100

basalt fiber
Strength maintenance ratio/ %

glass fiber
80
6
Mass loss ratio/ %

basalt fiber
glass fiber
60
4

40

2
20

0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Treating time/ h
Treating time/ h
Fig. 6. Mass loss ratio-treating time behavior (alkali treatment).
Fig. 7. Strength maintenance ratio-treating time behavior (alkali treatment).

structure present on the fiber surfaces, indicating that some chem-
ical reactions have occurred during the treatment. Seemingly, both
the basalt and glass fibers appear to have similar deterioration
characteristics and to lose strength and volumetric stability under
severe alkali conditions. Water and NaOH reagents may penetrate
into the net structure of the glass fiber and cause some reactions to
destroy the original structure. Meanwhile, some constituents in-
side the glass fiber could migrate outside and dissolve in the solu-
tion. On the other hand, hydrolytic action may exist on the alkali
silicate of the fiber [19]. It is also believed that the alkaline metal
oxides in the fiber would cause their chemical stability weaker
when meeting with the alkali molecules. Edith Mäder’s research
group has proved that using nanometer-scale coating based
copolymer with nanoclays could obviously increase alkali resis-
tance of the glass fibers [29].
The main component in the glass and basalt fibers is SiO2. Dur-
ing chemical treatment in the alkali solution, the ASiAOA bond
which is the main framework of the fiber will be broken by the hy-
droxyl ion:
½ASiAOASiA þ OH ! ½ASiAOH þ ½ASiO ð1Þ
Hence the strength of the fibers after treatment in alkali solu-
tion is decreased considerably. Their acid corrosion-resistance is
relatively better as compared to alkali corrosion-resistance proba-
bly because the ASiAOA structure is inert to the acid except for
hydrofluoric acid and phosphorous acid.
 B. Wei et al. / Materials and Design 31 (2010) 4244–4250
a b
Fig. 8. SEM images of the glass and basalt fiber surfaces after treatment in NaOH solution (a – glass fiber, b – basalt fiber).
The behavior of the glass fiber reinforced materials in sodium
hydroxide environment has been investigated. Now the applicabil-
ity of the basalt fiber as a structural strengthening material is
highly expected. Brik investigated fundamental properties of the
basalt fiber as a reinforcing steel replacement in the concrete struc-
tures, and proved the feasibility of basalt fibers in the construction
application [33,34]. It is the filaments in the FRP that are responsi-
ble in bearing the foreign load, and the corrosive behavior of the
fibers is always the basic concern. Since the fibers are wrapped
completely by the matrix materials in the fiber reinforced polymer
(FRP), it is difficult to judge how the fibers are affected by the so-
dium hydroxide. This research focused on the fibers themselves
and obtained direct response behaviors of the fibers to the external
chemical environment.
4. Conclusions
The glass and basalt fibers may be damaged greatly in the HCl
and NaOH solutions with a concentration of 2 mol/l. The tensile
strength of the fibers decreases with increasing treatment time.
It seems that in the same acid environment the effect of the treat-
ment time on the strength reduction of the basalt fibers is not as
obvious as that for the glass fibers. As for alkali environment, the
variation of the strength with treating time is almost similar to
each other for both the basalt and glass fibers.
The acid resistance of the basalt fibers is much better than
the alkali resistance. But for the glass fibers, the acid resistance
is similar to the alkali resistance. The surface morphologies of
the basalt and glass fibers after acid treatment do not change
as much as those after alkali treatment. Deterioration of both
the glass and basalt fibers occurs if they are contacted with
NaOH solution. On the whole, the chemical stability of the basalt
fibers is better than the glass fibers, especially in an acidic
environment.
Finally, for the equipment used in a corrosive environment,
both high strength and high corrosion-resistance are required.
The basalt fiber may be a good alternative material compared with
the traditional fibers in manufacturing the fiber reinforced com-
posites. The basalt fiber reinforced composite could be used in a
chemical environment for long-term service.
Acknowledgement
The authors would like to thank the National Nature Science
Foundation of China (Grant No. 50503007) for financial support.
4249
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