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Sofiene In
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Journal of Advanced Ceramics

2015, 4(4): 272–281 ISSN 2226-4108


DOI: 10.1007/s40145-015-0161-1 CN 10-1154/TQ
Research Article 

Characterisation of mechanical and thermal properties in flax fabric 
reinforced geopolymer composites 
Hasan ASSAEDIa, Thamer ALOMAYRIa, Faiz U. A. SHAIKHb, It-Meng LOWa,c,*
a
Department of Imaging & Applied Physics, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
b
Department of Civil Engineering, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
c
Department of Engineering, Curtin College, Building 205, Curtin University Bentley Campus, Kent Street, Perth,
Western Australia 6102, Australia

Received: February 19, 2015; Revised: June 17, 2015; Accepted: June 18, 2015
© The Author(s) 2015. This article is published with open access at Springerlink.com

Abstract: This paper presents the mechanical and thermal properties of flax fabric reinforced fly ash
based geopolymer composites. Geopolymer composites reinforced with 2.4, 3.0 and 4.1 wt% woven
flax fabric in various layers were fabricated using a hand lay-up technique and tested for mechanical
properties such as flexural strength, flexural modulus, compressive strength, hardness, and fracture
toughness. All mechanical properties were improved by increasing the flax fibre contents, and showed
superior mechanical properties over a pure geopolymer matrix. Fourier transform infrared
spectroscopy (FTIR) and scanning electron microscopy (SEM) studies were carried out to evaluate the
composition and fracture surfaces of geopolymer and geopolymer/flax composites. The thermal
behaviour of composites was studied by thermogravimetric analysis (TGA) and the results showed
significant degradation of flax fibres at 300 ℃.
Keywords: geopolymer composites; flax fibre; mechanical properties; thermal properties

1    Introduction  cement [1–5].


Despite their desirable characteristics, geopolymer
Ordinary Portland cements are used in many matrices suffer from brittle failure under applied force
construction applications because of their good and demonstrate low flexural strength ranging between
mechanical and durability properties. However, the 1.7 and 16.8 MPa [6,7]. Improving their flexural and
greenhouse emissions caused by cement based tensile strengths will significantly increase the
materials have made it necessary to find an eco-friendly application of these materials in the construction and
alternative. A new group of promising construction building industries; and this may be accomplished by
material is geopolymer, first introduced and named by dispersing inorganic or organic fibres throughout the
Davidovits in 1989, exhibiting good mechanical matrices. Hitherto, the most common fibre
performance, durability, and fire and acid resistance. reinforcements used in geopolymer composites are
It can be cured and hardened at room temperature based on carbon, basalt, and glass fibres [8–12], but
with 80%–90% fewer CO2 emissions than Portland concerns over the environment and
 non-biodegradability have made renewed interest
* Corresponding author. recently in replacing the synthetic fibres used in
E-mail: j.low@curtin.edu.au geopolymer or other brittle matrices with natural plant

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J Adv Ceram 2015, 4(4): 272–281 273

fibres. These include flax, hemp, jute, pineapple, straw,


switch grass, kenaf, coir, and bamboo [13,14]. These
plant fibres cost less, have low density, and display
good mechanical properties when compared with
industrial fibres [15]. For example, natural fibres have
lower densities than synthetic fibres generally, with
many almost 30%–50% less dense than their synthetic
counterparts [16]. They are also renewable, recyclable,
and biodegradable, and demonstrate excellent
mechanical characteristics like flexibility, high specific
strength, and high specific modulus [17,18]. For
example, wood-derived cellulose can be used for
Fig. 1 Structure of the flax fabric.
toughening epoxy and other polymers [19–22], and
bamboo fibres improve the flexural strength of concrete Australia, was used as reinforcement in the fabrication
[23]; the same desirable effect has been observed in of geopolymer composites. The structure and physical
wood fibre reinforced concrete [24]. Cotton fabrics also properties of the flax fabric are shown in Table 1. Low
enhance the strength and toughness of geopolymer [25], calcium fly ash (ASTM class F) collected from the
and wool and flax fibres have been successfully used to Eraring power station in New South Wales, Australia,
reinforce geopolymer composites, with improvements was used as the source material for the geopolymer
in mechanical and fracture properties [26,27]. However, matrix. The chemical composition of fly ash is shown in
no study so far has reported the mechanical properties Table 2. The alkaline activator for geopolymerisation
of flax fabric (FF) reinforced fly ash based geopolymer was a combination of sodium hydroxide and sodium
composites despite their advantages of cheapness, ready silicate grade D solution. Sodium hydroxide flakes of
availability, lack of toxicity, biodegradability, and good 98% purity were used to prepare the solution. The
tensile strength. The present report describes the chemical composition of sodium silicate used was
development and mechanical properties of new 14.7% Na2O, 29.4% SiO2, and 55.9% water by mass.
environmentally friendly geopolymer composites To prepare the geopolymer composites, an alkaline
reinforced with the readily-available natural flax fibres solution to fly ash ratio of 0.75 was used, and the ratio
of Australia, to produce materials with excellent of sodium silicate solution to sodium hydroxide
flexural strength and graceful failure properties. solution was fixed at 2.5. The concentration of sodium
This study considers the viability of developing a hydroxide
(a) solution was 8 M, and was prepared and
green composite material that uses fly ash geopolymer combined with the sodium silicate solution one day
as the matrix and FF as the reinforcement. Fourier before mixing.
transform infrared spectroscopy (FTIR), scanning The alkaline solution was added to the fly ash in a
electron microscopy (SEM), and thermogravimetric Hobart mixer at low speed until the mix became
analysis (TGA) are used to investigate the morphology, homogeneous, then mixed for another 10 min on high
microstructure, failure mechanisms, and thermal speed with an additional 50 mL of water to improve the
behaviour of geopolymer/flax composites. The effect of workability. This produced a geopolymer matrix of
different FF contents of 2.4, 3.0, and 4.1 wt% on molar composition of SiO2/Al2O3 = 4.16, Na2O/SiO2 =
mechanical properties of the composites such as 0.37, and H2O/Na2O = 11.43.
flexural strength, flexural modulus, compressive
Table 1 Structure and physical properties of the flax fabric
strength, hardness, and fracture toughness is also
Fabric thickness (mm) 0.6
presented in this paper. Fabric geometry Woven (plain weave)
Yarn nature Bundle
Bundle diameter (mm) 0.6 (see Fig. 2(a))
Filament size (mm) 0.01–0.02 (see Fig. 2(b))
2    Experimental procedures  Opening size (mm) 2–4
Fabric density (g/cm3) 1.5
2. 1    Materials  Modulus of elasticity (GPa) 39.5
Tensile strength (MPa) 660
Flax fabric shown in Fig. 1, supplied by Pure Linen

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274 J Adv Ceram 2015, 4(4): 272–281

Table 2 Chemical composition of fly ash (Unit: wt%)


SiO2 Al2O3 CaO Fe2O3 K2O MgO Na2O P2O5 SO3 TiO2 MnO BaO LOI
63.13 24.88 2.58 3.07 2.01 0.61 0.71 0.17 0.18 0.96 0.05 0.07 1.45

(a) (b)

Fig. 2 Diameters of the (a) flax bundle and (b) flax fibres.

Three samples of geopolymer composites reinforced were aligned horizontally to the applied load in all
with 2.4, 3.0, and 4.1 wt% FF were prepared by mechanical tests. Ten samples of each composite were
spreading a thin layer of geopolymer paste in a well used to evaluate the flexural strength and the flexural
greased wooden mould and carefully laying the first modulus according to the standard ASTM D790 [28].
layer of FF on top. The fabric was fully saturated with The values were recorded and analysed with the
paste by a roller, and the process repeated for the desired machine software (NEXYGENPlus) and average values
number of layers; each specimen contained a different were calculated. The flexural strength (  F ) was
number of layers of FF (see Table 3). For each specimen, determined using the equation:
the final layer was geopolymer paste. The wooden 3 pm S
moulds were then placed on a vibration table for 2 min, F  (1)
2 WD 2
then covered with plastic film and cured at 80 ℃ for
24 h in an oven before demoulding. They were then where pm is the maximum load; S is the span of the
dried under ambient conditions for 28 days. This sample; D is the specimen width; and W is the specimen
procedure of preparing geopolymer composites is thickness.
reported by Alomayri et al. [25]. Flexural modulus ( EF ) values were computed using
the initial slope of the load displacement curve
2. 2    Mechanical properties  ( P / X ) using the equation [29]:
S 3  P 
A LLOYD material testing machine (50 kN capacity) EF    (2)
with a displacement rate of 0.5 mm/min was used to 4WD 3  X 
perform the mechanical tests. Rectangular bars of A crack with a length to width ratio (a/W) of 0.4
60 mm × 18 mm × 15 mm with a span of 40 mm were was introduced into the specimen using a 0.4 mm
cut from the fully cured samples for three-point bend diamond blade, to evaluate fracture toughness. The
tests to evaluate the mechanical properties. All samples fracture toughness ( K IC ) was calculated using the
equation [29]:
Table 3 Formulation of samples
p S a
Fly NaOH Na2SiO3 FF K IC  m 2/3 f   (3)
Fabric WD W 
Sample ash solution solution content
layers
(g) (g) (g) (wt%) where a is the crack length, and f (a/W) is the
1 1000 214.5 535.5 0 0
2 1000 214.5 535.5 5 2.4
polynomial geometrical correction factor given by [29]:
3 1000 214.5 535.5 7 3.0 a
4 1000 214.5 535.5 10 4.1 f    3(a / W )1/2 [1.99  (a / W )(1  a / W ) 
W 

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J Adv Ceram 2015, 4(4): 272–281 275

(2.15  3.93a / W  2.7a 2 / W 2 )] /


[2(1  2a / W )(1  a / W )2/3 ] (4)
The compressive strength of the geopolymer
composites was tested according to ASTM C109 [30],
but instead of using the recommended 50 mm cube
specimens, 20 mm cubes were used. The compressive
strength (C) of the sample was calculated using the
following formula:
CP/ A (5)
where P is maximum load on the sample at failure and A
is the surface area of the specimen. Wavenumber (cm1)
Fig. 3 FTIR spectra of pure geopolymer and
The hardness of geopolymer composites was flax/geopolymer composite.
measured on the Rockwell H scale using an Avery
Rockwell hardness tester. Before measurement, five the absorbance peak around 1653 cm1 is attributed to
samples were polished with emery paper to achieve flat, the bending vibration of absorbed water [34,35]. The
smooth surfaces. presence of bands in the regions 1440–1490 cm1 is an
indicator of the atmospheric carbonation on the surface
2. 3    Characterisation   
of the matrix where it reacts with carbon dioxide [34].
An FTIR spectrum was performed on a Perkin Elmer The presence of flax fibres in the composites can be
Spectrum 100 FTIR spectrometer in the range of recognised by the peak at 1418 cm1, which is attributed
4000–500 cm1 at room temperature. The spectrum was to the CH3 bending vibration of cellulose [32]. The
an average of 10 scans at a resolution of 2 cm1, intensity of the bands at 3385 and 1653 cm1 increases
corrected for background. in response to the existence of absorbed water in the
The microstructures of geopolymer composites were cellulose fibres.
examined using a Zeiss Neon focused ion beam
scanning electron microscope (FIB–SEM). The 3. 2    Flexural strength and modulus 
specimens were mounted on aluminium stubs using Generally, flexural tests are used to characterise the
carbon tape and then coated with a thin layer of mechanical properties of layered composites as they
platinum to prevent charging before the observation. provide a simple means of determining the bending
A thermogravimetric analyser (TGA) was used to response. This provides useful information on the
examine the thermal behaviours of the composites. performance of layered fabric based composites [36].
Solid samples of 25 mg were placed in an alumina The effect of FF contents on the flexural stress–strain
crucible and tests were carried out in an argon curves of the geopolymer composites is presented in
atmosphere with a heating rate of 10 ℃/min from 25 to Fig. 4.
800 ℃.

3    Results and discussion 

3. 1    FTIR observation 
FTIR spectra of both pure geopolymer and
flax/geopolymer composite are shown in Fig. 3. The
strong peak at ~1000 cm1 is associated with Al–O and
Si–O asymmetric stretching vibrations and is the
fingerprint of the geopolymerisation [31]. The FTIR
spectra show a broad peak in the region at 3466 cm1
corresponding to the hydroxyl (OH) stretching vibration Fig. 4 Typical stress–strain curves of pure geopolymer
of free and hydrogen bonded –OH groups [32,33], and and geopolymer composites with various FF contents.

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276 J Adv Ceram 2015, 4(4): 272–281

It can be seen that, the composite containing 4.1 wt%


FF shows the highest flexural strength among all
composites. The flexural strength of the composites
improves from 4.5 MPa in the pure geopolymer to
about 23 MPa with 4.1 wt% FF. This result is
comparable with that of short flax fibre reinforced
geopolymer composites reported by Alzeer and
MacKenzie [27]. Both studies show that increasing the
content of flax fibres leads to a significant improvement
in the flexural strength of the composite. This can be
explained by the fact that the number of reinforcement
layers controls the flexural strength. The lower weight
Fig. 6 Compressive strength of geopolymer composites
of flax fabrics allows multiple layers of fabric in the as a function of fabric content.
composite to resist the shear failure and contribute
in sustaining the applied load to the composites. increases with increase in fibre contents. The increase in
This permits greater stress transfer between the matrix compressive strength with fibre loading may be due to
and the flax fibres, resulting in improved flexural the ability of the flax fibres to absorb stress transferred
strength [37]. from the matrix. The compressive strength of the neat
The flexural modulus of geopolymer composites, geopolymer paste increases from 19.4 to 91 MPa after
shown in Fig. 5, also indicates that the addition of FF to the addition of 4.1 wt% flax fibres. This significant
the matrix improves the flexural modulus over that of a enhancement of compressive strength is due to the fact
pure geopolymer matrix. Flexural modulus is the that the interface between the fabric and the matrix is
measure of resistance to deformation of the composite not exposed to any shear loading, which in turn reduces
in bending. It was observed that none of the reinforced the possibility of fabric detachments or delamination
specimens were completely broken at peak load. This from the matrix at high loads. Similar remarkable
could be attributed to crack bridging of the long improvements in compressive strength have also been
continuous flax fibres under load, which makes the reported by Alomayri et al. [38] in the case of cotton
flexural modulus higher than that of pure geopolymer. fibre reinforced geopolymer composites. They
Long fibres are able to withstand a higher load and are concluded that the increase is due to the ability of
capable of supporting multiple cracks throughout the horizontally laid cotton fabric to directly absorb and
loading process, consequently preventing brittle failure distribute a load uniformly throughout the
of the geopolymer. cross-section.

3. 3    Compressive strength  3. 4    Hardness 


The results presented in Fig. 6 show that the Hardness measurement enables the ability of a material
compressive strength of the composites containing FF to resist plastic deformation under indentation to be
determined. The hardness values of FF reinforced
geopolymer composites are shown in Fig. 7. The results
show that the hardness of composites increases with the
addition of high number of flax fabrics to the
geopolymer composite. This enhancement in hardness
is due to the uniform distribution of the load on the flax
fibres, which reduces the penetration of the test ball at
the surface of the composite. A similar increase has
been reported by other researchers studying natural
fibre reinforced geopolymer composites: for instance,
Alomayri et al. [25] reported that with increasing
cotton fibre content, the hardness value of cotton fibre
Fig. 5 Flexural modulus of geopolymer composites as a reinforced geopolymer composites increases.
function of fabric content.

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J Adv Ceram 2015, 4(4): 272–281 277

matrix. It was observed that the composites with fibres


do not completely break into pieces, as the close
spacing of woven FF leads to crack-bridging by fibres
and enhancing the resistance to their propagation. The
effect of fibre content on the fracture surface can be
seen by observing the difference between the matrix
region and the fibre region. In Figs. 10(a) and 10(b),
composites filled with lower fibre contents (2.4 and
3.0 wt%) show an increase in matrix-rich regions,
which means there are insufficient fibres to transfer the
load from the matrix. Due to this reason, the
Fig. 7 Hardness of geopolymer composites as a function geopolymer composites with low fibre content exhibit
of fabric content. low fracture toughness and mechanical properties.
However, Fig. 10(c) illustrates the fracture surfaces of
3. 5    Fracture toughness  the geopolymer composites with higher fibre content,
Generally, fibres’ ability to resist crack deflection, which means higher fibre-rich regions of composites
debonding, and to bridge cracks, slows down crack with 4.1 wt% of FF. An increase in fibre-rich regions
propagation in fibre reinforced composites and leads to greater stress-transfer from the matrix to the FF
increases the fracture energy [39–42]. Figure 8 shows thereby resulting in improvement of fracture toughness.
the influence of FF content on the fracture toughness of
geopolymer composites. It can be seen that the 3. 6    Thermal stability 
composites containing FF show significantly higher The thermal stability of samples was determined using
fracture toughness than pure geopolymer matrix, and thermogravimetric analysis (TGA). In this test, thermal
the higher the FF content, the higher is the fracture stability was studied in terms of the weight loss
toughness. The greatest improvement in fracture percentage as a function of temperature in argon
toughness was obtained from about 0.4 MPa·m1/2 in the atmosphere. The thermograms (TGA) of FF, neat
pure matrix to about 1.8 MPa·m1/2 with 4.1 wt% geopolymer, and FF reinforced geopolymer composite
FF reinforcement. This extraordinary enhancement are shown in Fig. 11.
is due to the unique ability of flax fibre to resist The thermogram of flax fibres shows degradation in
fracture resulted in increased energy dissipation three steps. The first transition occurs from 25 to
from crack-deflection at the fibre–matrix interface, approximately 240 ℃, with the release of free water
fibre-debonding, fibre-bridging, fibre pull-out and evaporation. Then, the largest weight loss occurred
fracture, clearly shown in the SEM images (see Figs. between 240 and 365 ℃ is due to the decomposition of
9(a)–9(f)). It can be seen in these images that small cellulose. This result is in agreement with Alzeer and
pieces of geopolymer paste attached to the fibre surface MacKenzie [27], where the highest weight loss of short
of the composites: such retention of the matrix on the flax fibres under flowing air is in the range of
fibre surfaces shows good adhesion between fibres and 240–340 ℃. The final stage occurs above 365 ℃, when
the fibres start to decompose but display a lower rate of
weight loss, and all volatile substances are dispelled.
The pure geopolymer shows weight loss occurring
from 25 to 300 ℃ , caused by the evaporation of
physically adsorbed water. Above 300 ℃, weight loss is
attributed to the dehydroxylation of the chemically
bound water. The FF reinforced geopolymer composite
shows a weight loss of 10.5% up to about 260 ℃, which
is due to the evaporation of physically absorbed water.
Above 260 ℃, the composite shows further weight loss
because of the degradation of the fibre content in the
Fig. 8 Fracture toughness of geopolymer composites as a
function of fabric content.
sample. The porosity of geopolymer matrix allows the

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278 J Adv Ceram 2015, 4(4): 272–281

Fig. 9 SEM images of the fracture surface for geopolymer composites reinforced with flax fibres show (a) fibre debonding, (b)
fibre imprint and pull-out, (c) fibre bridging cracks ((d) and (e) show the adhesion between fibre and matrix), and (f) fibre fracture.

oxygen to enter and cause degradation of the flax fibres whole composite sample because the distribution of flax
at high temperatures. The composite shows a total fibres is not uniform within the geopolymer matrix.
weight loss of ~15% at 300 ℃ which indicates further Therefore, the fibre content of the TGA micro-sample
degradation of fibres inside the composite. At this will be highly dependent on the position it is taken from
temperature a substantial amount of fibre degradation the composite sample. However, TGA test can provide a
has occurred. Therefore, it could be concluded that this good estimation of the thermal stability of a composite
composite system is only suitable for service below when compared to the thermal stability of its
250 ℃. It is worth mentioning here that the TGA components.
micro-sample is not necessarily representative of the

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J Adv Ceram 2015, 4(4): 272–281 279

Fig. 10 Low magnification SEM images of the fracture surface for geopolymer composites reinforced with (a) 2.4, (b) 3.0, and (c)
4.1 wt% of flax fibres.

4    Conclusions 

This paper presents the mechanical and thermal


properties and microstructural characterisation of FF
reinforced geopolymer composites. It shows that the
presence of FF in geopolymer composites remarkably
increases flexural and compressive strength, hardness,
and fracture toughness compared to neat geopolymer.
These significant enhancements are due to the unique
properties of flax fibres in resisting greater bending and
fracture forces than the more brittle geopolymer. SEM
micrographs show a number of toughening mechanisms
Fig. 11 TGA curves of the flax reinforced geopolymer that include crack bridging, fibre pull-out, and fibre
composite, the matrix, and the flax fibres. fracture; these are the major factors contributing to the

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280 J Adv Ceram 2015, 4(4): 272–281

enhanced mechanical properties of FF reinforced reinforced geopolymer composites. In Strategic Materials


geopolymer composites. Thermogravimetric analysis and Computational Design: Ceramic Engineering and
Science Proceedings, Volume 31. Kriven WM, Zhou Y,
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