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Article history: In the last decades, eco-friendly materials are playing an increasingly important role in the building
Received 24 July 2015 industry. Particularly, many studies deal with the use of natural fibers as replacement to synthetic fibers
Received in revised form 15 September in reinforced composites. Natural fibers are already employed in many building materials, due to their
2015
attractive features, such as good mechanical properties, low cost, low density, low thermal conductibility
Accepted 18 September 2015
Available online 25 September 2015
and recyclability.
In this research, the interaction between abaca fibers and gypsum matrix was studied, in order to
produce fiber-reinforced plasterboards with enhanced toughness performances.
Keywords:
Abaca fiber
Firstly, the influence of some parameters (i.e. fibers dimensions, amount of fiber addition, water to
Gypsum gypsum ratio) on physical and mechanical behavior of the plasters was evaluated.
Pullout In order to improve the composite performances, the fibers were subjected to different chemical
Chemical treatments treatments (with distilled water, NaOH solution and EDTA solution) to modify the surface characteristics
Surface modification and to improve the adhesion with the gypsum matrix. Their effects were explored by scanning electron
microscope and mechanical tests, such as pull-out and flexural strength tests.
The treatments with NaOH and EDTA solutions resulted in a worsening of the mechanical behavior of
the composites, while the fibers treated with distilled water gave a better adhesion with the inorganic
matrix.
Ó 2015 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2015.09.020
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
F. Iucolano et al. / Construction and Building Materials 99 (2015) 184–191 185
coupled with a high water solubility, hindering outdoor X-ray diffraction analysis was performed to evaluate the mineralogical compo-
sition of the binder, using a XRD Philips PW 1730 apparatus (rad. CuKa1). The den-
application.
sity of the abaca fibers was evaluated with a helium pycnometer (MultiVolume
Generally adding fibers to a binder materials can improve its Pycnometer 1305, Micromeritics).
mechanical properties, especially to the post-cracking behavior Morphology and size of the natural fibers was evaluated by means of scanning
[3–7]. In particular, brittleness may be appreciably reduced by electron microscope analysis (SEM, Cambridge S440).
combining gypsum with mineral particles or natural fibers [8]. Mechanical characterization was performed by Tensometer 2020 testing
machine (Alpha Technologies), equipped with a 100N load cell equal and a deflec-
The competition in the industrial field, looking for materials
tion rate equal to 10 mm/min, according to the Standard ASTM-D3822 [22]. Tensile
that meet both socioeconomic expectations and environment strength, Young’s modulus and failure elongation were evaluated as average on
preservation, drives toward the utilization of natural fibers thirty samples.
[9,10]. Advantages of natural fibers, such as good mechanical prop-
erties, low cost, low density, low thermal conductibility and recy- 2.3. Chemical treatments of the fibers
clability make them a good potential replacement for synthetic
In order to modify the surface characteristics and to improve the adhesion with
fibers in composite materials [11,12]. Many applications of natural the gypsum matrix, abaca fibers were subjected to different chemical treatments.
fiber-reinforced composites can be found in building, packaging Short (10 mm) and long fibers (150 mm) were treated with: (a) distilled water for
industries, furniture and auto-motive fields [13]. 24 h at 20 °C, (b) sodium hydroxide (NaOH) and (c) ethylene diamine tetraacetic
Natural fibers are mainly composed of hemicellulose, lignin and acid (EDTA).
The treatment with distilled water allows to softly clean fiber surface by remov-
pectin [14], moreover the composition can more or less change
ing all the water-soluble organic compounds (e.g. the weakly linked pectin, extre-
according to the growing conditions, the location and the age of mely soluble in water due to a high methyl esterification coefficient [15,25]). This
the plant. treatment enhances the surface roughness, improving the fiber–matrix adhesion
In the last years, many studies tried to estimate the influence of and increases the amount of cellulose exposed on the fiber surface, thus increasing
adding natural fibers in gypsum matrix, mainly in terms of the number of possible reaction sites.
Alkaline treatment is one of the most common chemical treatment of natural
mechanical properties of the composite material [15–17]. Abaca, fibers when they are used as reinforce in composite materials; it involves the break
a particular variety of banana-tree native to the Philippines, has of hydrogen bonding in the network structure, increasing fiber surface roughness
been recently studied for the flexible and very resistant fibers and improving mechanical interlocking with the matrix [15,21]. In addition, this
extracted from its trunk [18]. treatment could enhance the rigidity of the fiber itself [27].
Fibers were immersed in sodium hydroxide solution (0.5 M; pH = 13.7) for 2 h
The main drawback in the use of natural fibers as reinforcement
and then washed with distilled water. In order to neutralize the alkalinity of the
in composite materials is the weak interaction between fibers and treated fibers an additional washing step with acetic acid was performed.
matrix. Therefore, many studies were carried out on suitable chem- Last treatment was carried out with EDTA on fibers pretreated with NaOH solu-
ical treatments on fibers to improve the adhesion between fiber and tion. The EDTA, a strong chelating agent, could potentially react with calcium ions
matrix, in order to increase the composite strength [19,20]. and solubilize a great fraction of pectin, bringing to the separation of fiber bundles
and so enhancing the fiber–matrix adhesion [26,28,29]. Abaca fibers were first
In the present paper, the effect of abaca fibers on the mechani- soaked in NaOH solution as above reported and then they were immersed for 2 h
cal properties of gypsum based composite was investigated. In par- in a 13.5103 M EDTA solution. The pH was adjusted at 11 with sodium hydroxide).
ticular, the role of different treatments on fibers and the Fibers were washed with distilled water, to neutralize the alkalinity of the treated
consequent morphologic surface modification were evaluated, fibers. For each treatment the fiber-to-solution ratio was fixed at 30 g/l, and after
the treatments the fibers were dried at 40° C for 24 h. Finally, the weight loss of
with the aim to obtain preliminary indications about the use of
the fibers due to the soluble fraction was evaluated after each treatment. All the
abaca fibers as a sustainable opportunity to manufacture plaster- treatment conditions were summarizes in Table 1.
boards with enhanced toughness performances.
2.4. Fiber reinforced plasters characterization
2. Experimental
2.4.1. Chemical characterization (SEM–FTIR)
2.1. Materials In order to evaluate the effects of different surface treatment on the morphol-
ogy of the fibers, scanning electron microscopy (SEM) was performed. Characteriza-
Gyproc Saint Gobain (Termoli, Italy) kindly provided the gypsum used in the tion was carried out on both treated and untreated fibers. Moreover, the adhesion
present research. As reported in the technical sheet, it was obtained by calcination between fiber and matrix was verified controlling the microstructure of the fracture
of natural gypsum (calcium sulfate dehydrate, CaSO4 2H2O) at T = 120–150 °C, in surfaces of the hardened compacts. Abaca fibers and fracture surfaces were coated
order to obtain a mixture mainly consisting of hemihydrate, with some amount with gold and then analyzed using a SEM Cambridge S440 equipment.
of anhydrous gypsum (anhydrite). The chemical surface modifications were also evaluated by means of Fourier
Fiber Industry Development Authority of the Department of Agriculture, Repub- Transform Infrared Spectroscopy (FT-IR) [30], using a Nicolet apparatus (Thermo
lic of the Philippines, supplied the abaca fibers. An average chemical composition of Scientific, Italy) and a standard KBr pellet technique. For each sample 64 scan were
abaca fibers was reported by Li et al. [21]. acquired between 4000 and 400 cm1 with a wavenumber resolution of 4 cm1.
After preliminary runs, 10 mm length fibers, obtained by means of an automatic Abaca fibers were chopped to a length less than 1 mm and mixed with 200 mg of
cutter, were selected both to give a ‘‘bridge action” effect during the flexural failure KBr. The resulting powder was then pressed into a pellet with a diameter equal
and to be consistent with the dimensions of typical plasterboard panels commer- to 16 mm and subjected to FTIR analysis.
cially available. In addition, 150 mm length fibers were used for pull-out test.
Moreover the influence of the fibers addition on the setting time of the pastes 2.4.2. Mechanical characterization
was preliminarily evaluated. In fact a recent research on gypsum products rein- 2.4.2.1. Pull-out test. The pull-out test is a method used for the characterization of
forced with hemp and flax fibers showed that this addition could considerably delay the fiber–matrix interphase. It allows measuring the tensile load necessary to
the setting time of the pastes. The reason of this phenomenon is to be found in the extract a single reinforcing fiber by the matrix in which it is immersed, and there-
chemical composition of the natural fibers. They contain a considerable fraction of fore lets to estimate the quality of fiber–matrix adhesion [31].
pectin, soluble in water, and capable of trapping the calcium ions present in
solution, so preventing the hydration of the hemihydrate [15]. Therefore, the setting
time of two different pastes, with 2 wt.% of short fibers or without fibers, were Table 1
evaluated according to the Vicat test [33]. Treatments conditions.
Sodium hydroxide (NaOH) and ethylene diamine tetraacetic acid (EDTA) used
for the chemical treatments of the abaca fibers were Carlo Erba reagents. Fiber Treatment Residence Molarity Soluble
typology agent time fraction [%]
2.2. Characterization of the raw materials F – – – –
FW H2O 24 h – 6
The chemical composition of the binder was evaluated by simultaneous thermal FS NaOH 2h 0.5 M 10
analysis (DSC-TGA), using a Netzsch STA409 PCLuxx apparatus. In particular, FSE NaOH 2h+2h 0.5 M 10
weighted samples were heated on alumina pans from 20 to 1000 °C with heating + EDTA + 1.35103 M
rate of 10 °C/min under N2 atmosphere.
186 F. Iucolano et al. / Construction and Building Materials 99 (2015) 184–191
For each type of treatment, two abaca long fibers were arranged longitudinally peak was detected around T = 350 °C, and was attributed to the
into a polystyrene mold of 100 25 25 mm, as shown in Fig. 1, and subsequently
polymorphic transition CaSO4 (a) ? CaSO4 (b).
gypsum plaster (water to gypsum ratio = 0.7) was placed into the molds and
compacted with a conventional vibration table for about 30 s.
The mineralogical composition performed with XRD confirmed
The specimens were cured for 24 h under controlled conditions (T = 20 ± 2 °C the above results. In fact, the pattern reported in Fig. 3b, showed
and RH = 65 ± 5%), then they were de-molded and dried for 48 h at T = 40 °C. peaks ascribed to hemihydrate (ICDS#081-1848), anhydrite
The specimens were finally cut in half, to obtain a total of four tensile load mea- (ICDS#070-0909) and calcite (ICDS#072-1651); whereas no peaks
surements for each one (A1, A2, B1, B2, see Fig. 1) and then stored in a climatic cham-
related to dehydrate gypsum was revealed.
ber (MSL Humichamber, mod. EC 125) at 20 °C and RH = 60%, until the time of
testing. Specimens were manufactured in triplicate in order to get twelve measure- SEM analysis showed that the fibers have a diameter in the
ments for each type of treatment of the fiber surface. Pull-out test was performed range 0.15–0.40 mm, and each fiber is itself constituted by a com-
with a Tensometer 2020 testing machine (Alpha Technologies), with load cell equal bination of thinner filaments (d 5–15 lm), as shown in Fig. 4.
to 100 N and a speed displacement equal to 1.0 mm/min. Tensile load was con-
The density of the abaca fibers was evaluated by means of
stantly applied at the free end of the fiber (see Fig. 2). Known the maximum tensile
load T at which the fiber is extracted from the matrix, it is possible to estimate the
helium pycnometry, and resulted to be equal to 1.28 gcm3. Thirty
related mean stress su,m by the following Eq. (1), where d is the fiber diameter and l fibers were mechanically tested and the following average values
is the anchorage depth: as well as the standard deviations were evaluated: the tensile
T strength was equal to 760 ± 160 MPa, the Young’s modulus was
su;m ¼ ½N=mm2 ð1Þ
pdl equal to 28.9 ± 5.8 GPa and the failure elongation was equal to
2.64 ± 0.68%. These calculated parameters agree, on the whole,
2.4.2.2. Three point flexural test. In order to estimate the real efficacy of the rein-
with those related to other natural fibers [21,23,24].
forcement, in terms of ultimate strength and toughness, three point flexural tests The results of Vicat test did not show any significant influence
were conducted on 160 40 20 mm specimens, according to the Standard UNI of the fibers on the setting time of the samples, probably due to
EN 1015-11 [32]. Short abaca fibers, both raw and treated, were added to the binder the chemical composition of abaca fibers used in the experimental,
at different percentages (1%, 2% and 3% by weight respect to binder). The dry mix-
not so rich in pectin fraction. In addition it should be considered
ture was firstly homogenized and then the compound was slowly added to the
water (water to gypsum ratio = 0.7) and mixed in a blender for about 30 s. The mix- that a delay in setting time may happen if the extractable materials
ture was casted into mold and compacted with a conventional vibration table for (e.g. pectins) contained in the fibers dissolves when immersed in
about 30 s. The specimens were cured following the same procedures described water. In the above-cited paper [15], Dalmay et al. used a high
above. For each fiber typology, specimens were manufactured and measurements water to gypsum ratio (1.0), while in the present study a lower
were performed in triplicate.
The flexural test was performed with a Tensometer 2020 testing machine
ratio was used (0.7). Therefore, the lower water amount, coupled
(Alpha Technologies), with load cell equal to 5 kN and deflection rate equal to to the rapidity of the gypsum setting process, probably involved
0.6 mm/min. in a negligible amount of dissolved fraction, with a consequent
Known the maximum load F reported by testing machine, it is possible to eval- any significant delay on the setting time.
uate the flexural strength of the specimen ru,max, using the following equation (Eq.
Lastly, the effect of the treatments on the abaca fiber morphology
(2)), where l is the span distance, b and d are respectively the width and the thick-
ness of the specimen: and the mechanical behavior of the composites materials are
hereafter reported.
Fl
ru; max ¼ 1:5 2
½N=mm2 ð2Þ
bd
Fig. 1. Long fibers arranged into the mold (a); specimen dimensions and cross section (b).
Fig. 3. Characterization of the starting binder: (a) thermogravimetric (continuous line) and differential scanning calorimetry (dotted line) analysis; (b) XRD pattern
(H = CaSO40.5H2O; A = CaSO4; C = CaCO3).
188 F. Iucolano et al. / Construction and Building Materials 99 (2015) 184–191
(±0.26) and the behavior of the FW pull-out curve, the only one representative of the 3% addition was reported (FW3). The reason
similar to the pull-out ideal curve (see Fig. 7) [31]. of these behavior could be due to the scarce workability, related
The treatments with soda and soda + EDTA resulted, respec- to the fiber excess, observed during the manufacturing of F3 and
tively, in pull-out tensile loads lower than (1.89 ± 0.45 N) or com- FW3 specimens. The loss of workability leads to a heterogeneous
parable (2.39 ± 0.67 N) with those obtained with raw fibers, so distribution of the fibers, as showed in Fig. 9c, with a consequent
proving to be too aggressive toward the fibers and decidedly worsening of both flexural strength and load transfer capacity from
ineffective. matrix to fibers. The analysis of the fracture surfaces also confirms
In accordance with the SEM and FTIR analyses, and with the that 1 wt.% of fibers are too few to ensure a bridging action (Fig. 9a)
preliminary mechanical results obtained from the pull-out tests, while 2 wt.% of fibers give rise to a homogeneous and effective
the flexural behavior was just evaluated on specimens manufac- fibers distribution (Fig. 9b).
tured with raw (Fx) and distilled water treated (FWx) fibers, where
‘‘x” represents the amount (wt.%) of fibers added respect to the bin-
der. Moreover, reference samples (REF), manufactured without
adding fibers, were realized as reference material, and tested. The
curves relative to the three points flexural tests are showed in
the Fig. 8, and the resulting mechanical features were summarized
in Table 3. By inspecting Fig. 8a it appears evident that both F1 and
FW1 specimens present the same catastrophic failure typical of a
brittle material (REF), thus proving that the addition of 1% of fibers
is ineffective to enhance the toughness.
Conversely, when fibers were added to gypsum at 2% by weight,
the flexural behavior of composites changed, and the fibrous rein-
forcement resulted to be effective to provide a good toughness. In
fact the curves shown in Fig. 8b indicate that, after the maximum
flexural load is reached, the fibrous reinforcement bridges the
macro crack and reduces the defects propagations, so to ensure
the structural continuity of the specimen [3]. Moreover, the speci-
men FW2 presents a better post-cracking behavior compared with
the F2 specimen, with a better gain of load due to a better load
transfer from the matrix to the fibers.
Finally, a further increase of fibers amount from 2 to 3 wt.% does
not involve neither in a further gain of load nor in an enhanced
toughness, as shown in Fig. 6b, where only one curve Fig. 6. FT-IR spectra of untreated (F) and treated (FW, FS, FSE) abaca fibers.
Fig. 5. SEM micrograph of untreated (F) and treated (FW, FS, FSE) abaca fibers.
F. Iucolano et al. / Construction and Building Materials 99 (2015) 184–191 189
Table 2 Table 3
Pull-out test results. Three point flexural test results.
Sample Maximum tensile load T Shear stress su,m Sample Fiber amount Flexural load, F Flexural strength, rf
[N] [MPa] [wt.%] [N] [MPa]
F 2.40 ± 0.67 0.10 ± 0.03 REF – 278.6 ± 15.3 2.61 ± 0.14
FW 4.42 ± 0.26 0.19 ± 0.01 F1 1 288.1 ± 24.4 2.70 ± 0.23
FS 1.89 ± 0.45 0.08 ± 0.02 FW1 1 283.8 ± 25.5 2.66 ± 0.24
FSE 2.39 ± 0.67 0.10 ± 0.02 F2 2 291.1 ± 20.4 2.73 ± 0.19
FW2 2 315.0 ± 19.6 2.95 ± 0.18
F3 3 267.5 ± 28.1 2.51 ± 0.26
FW3 3 262.5 ± 29.9 2.46 ± 0.28
Further information about the role of the fibers inside the gyp-
sum matrix can be obtained from the morphological analysis of
matrix–fiber interface after a three point flexural test (Fig. 10).
SEM micrograph of F2 sample exhibit a fiber surface quite neat, of the addition of the natural fibers on the setting time of the mix-
with a scarce presence of gypsum crystals, whereas the fiber sur- ture was preliminary investigated and no significant delay on the
face in FW2 sample appears almost covered by gypsum crystal, setting time was observed.
so confirming the above-mentioned better adhesion matrix–fibers. Both the morphological analysis and the pull-out tests demon-
strated that the treatments with soda and EDTA resulted to be too
4. Conclusion aggressive toward the fiber’s surface, leading to a worsening of
mechanical features. On the contrary, the treatment of raw fibers
The effect of abaca fibers on the mechanical properties of gyp- with distilled water resulted in a slight enhance in surface rough-
sum based composite was investigated in this paper. Furthermore, ness, with a consequent improved fiber/matrix adhesion.
the effect of different treatments on fibers and the consequent Moreover, three point flexural tests showed that the addition of
morphologic surface modification were analyzed. The influence 2 wt.% of FW fibers to gypsum leads to an enhanced toughness of
Fig. 9. Fracture surfaces of FW1 (a), FW2 (b) and FW3 (c) specimens.
Fig. 10. SEM micrographs of raw (F2) and water-treated (FW2) fibers after the flexural test.
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