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Characterisation of "One-Part" Ambient Cured Engineered Geopolymer Composites

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Journal of Advanced Concrete Technology Vol.

21, 204-217, April 2023 / Copyright © 2023 Japan Concrete Institute 204

Scientific paper

Characterisation of “One-part” Ambient Cured Engineered Geopolymer


Composites
Wee Teo1*, Kazutaka Shirai2 and Jee Hock Lim3

Received 14 September 2022, accepted 13 March 2023 doi:10.3151/jact.21.204

Abstract
Engineered geopolymer composites (EGC) recently emerged as a promising alternative to resolve traditional concrete’s
CO2 emission and brittleness. It features a cementless-based solution and possesses pseudo-strain-hardening (PSH) be-
haviour with high tensile ductility. There are two main obstacles associated with the use of geopolymer: firstly, the han-
dling of user-hostile alkaline solutions and secondly, the necessity of heat curing. This paper aims to summarize the
findings on the development and characterization of an ambient cured “one-part” EGC under the influence of various
parameters, namely binder proportion between fly ash (FA) and ground granulated blast furnace slag (GGBS), quartz
powder/binder ratio, alkali activator/binder ratio and water/binder ratio. Fresh and mechanical properties consisting of
compressive strength, uniaxial tensile performance, and microstructure analysis were conducted. The results obtained
indicate that increased FA content favours the attainment of PSH behaviour of the composite due to low matrix fracture
toughness and fibre-matrix interfacial bond strength. Low water content and increased alkali activator content would
greatly enhance the matrix toughness and fibre-matrix interfacial bond strength. The addition of quartz powder may favour
strength attainment, but excessive quantities may have unfavourable consequences on the PSH behaviour.

1. Introduction However, one of the major drawbacks of ECC is the


use of a high amount of ordinary Portland cement (OPC)
Concrete is inherently brittle in nature. The use of dis- due to the absence of coarse aggregates and low water-
crete randomly oriented fibres as reinforcement has long to-binder (W/B) ratio, typically between 0.2 and 0.3. It is
been recognized to be highly effective in controlling the a known fact that high cement contents are associated
brittleness of cementitious materials. Engineered ce- with high embodied energy and CO2 emissions. Cement
mentitious composites (or ECC) are a class of fibre-rein- production accounts for about 6-8% of global CO2 and
forced cementitious composites that possess pseudo- greenhouse gas emissions (Boden et al. 2016). This cre-
strain-hardening (PSH) behaviour with excellent tensile ates a negative impact on the environment and could po-
ductility of over 5% (Li 2003; Li et al. 2001). This mate- tentially compromise the sustainability credentials of
rial’s superior characteristics make it ideal to be used for ECC (Nematollahi et al. 2016, 2017a). The most effec-
structures subjected to extreme loading conditions such tive way to reduce the CO2 emissions of OPC in the ECC
as seismic, impact, and blast. There is also a potential ap- mix design is to partially replace it with supplementary
plication for strengthening and rehabilitation of buildings cementitious materials (SCMs), such as fly ash (FA) and
and infrastructure, such as from the work by Lepech and ground granulated blast furnace slag (GGBS). For in-
Li (2009) where they used ECC link slab to improve the stance, Yang et al. (2007) utilized high volumes of FA re-
bridge deck constructability, durability, and sustainabil- placement (up to 85% by weight of cement) to improve
ity; and van Zijl and de Beer (2019) of using sprayed ECC material greenness and sustainability. This approach
strain-hardening cementitious composites (SHCC) over- may partly resolve the issue, but on the way forward a
lay for shear strengthening of unreinforced load-bearing more technically viable solution or alternative to OPC is
masonry. In addition, an overview of existing research re- needed.
sults on the durability of SHCC has been presented by Geopolymer is a cement-less binder and is considered
van Zijl et al. (2012). one of the promising contenders as a viable substitute for
OPC. This binder is produced by synthesizing alumino-
silicate source materials of geological origin or industrial
1 by-products with highly alkaline activators. The most
Associate Professor, School of Energy, Geoscience,
commonly used aluminosilicate sources for alkali activa-
Infrastructure and Society (EGIS), Heriot-Watt
tion are FA, GGBS, rice husk ash, and palm oil fuel ash
University Malaysia, Putrajaya 62200, Malaysia.
(Hardjito et al. 2004; Hardjito and Rangan 2005; Nath
*Corresponding author, E-mail: t.wee@hw.ac.uk
2 and Sarker 2014; Kaur et al. 2018; Nadziri et al. 2018).
Associate Professor, Faculty of Engineering, Hokkaido
Geopolymer or alkali-activated binder (AAB) has been
University, Sapporo 060-8628, Japan.
3 regarded as an important element of “sustainable cement-
Associate Professor, Department of Civil Engineering,
ing binder systems” for the future (Provis 2018; Shi et al.
Universiti Tunku Abdul Rahman, Bandar Sungai Long,
2011). It offers a potential reduction in CO2 emissions by
Cheras, Kajang 43000, Malaysia.
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 205

as much as 80% or more when compared to OPC to be considered than conventional ECC design (Ohno
(Duxson et al. 2007b). Due to its potential, over the past and Li 2018; Zhang et al. 2020). This paper aims to sum-
decades, there has been growing interest in the develop- marize the recent characterisation of ambient cured one-
ment and application of geopolymer. This is reflected by part FA/GGBS-based EGC carried out by the authors.
the number of research articles published in various state- The main parameters in this study investigate the effect
of-the-art reports (Duxson et al. 2007a; Hassan et al. of blended proportion between FA and GGBS, the addi-
2019; Singh et al. 2015; Zakka et al. 2021). tion of quartz powder, solid alkaline activator content and
Recently, there is a growing interest in incorporating water content on the properties of the matrix and compo-
both concept of ECC and geopolymer to develop ductile site. A series of experiments including flowability, com-
fibre-reinforced geopolymer composites (FRGC), also pressive, uniaxial tensile tests and SEM/EDS tests were
known as engineered geopolymer composites (EGC). conducted to characterize the mechanical, tensile strain-
Lee et al. (2012) successfully demonstrated the feasibil- hardening behaviour and microstructure properties of the
ity of developing a ductile fibre-reinforced composite us- composites.
ing GGBS-based alkali-activated mortar. They proved
that tensile strain hardening behaviour and ductility of up 2. Experimental programme
to 4.7% could be attained. Another feasibility study was
conducted by Ohno and Li (2014) using a FA-based geo- 2.1 Materials and mix proportions
polymer. The developed EGC exhibit tensile strain hard- The main purpose of this experimental study is to char-
ening behaviour with high ductility of over 4%. They also acterize the mechanical, tensile strain hardening behav-
found out that curing temperature could greatly improve iour and microstructure properties of ambient cured one-
the tensile strength and ductility performance of the com- part EGC composite using blended FA and GGBS. Stud-
posites. Due to the complex variables involved in the de- ies into the impact of the addition of quartz powder (QP),
velopment of EGC material, Ohno and Li (2018) pro- solid alkali activator and water content on the composite
posed an integrated statistical design approach to deter- behaviour of EGC would be discussed. A total of 9 mix-
mine an optimum EGC design, which incorporates ma- tures were prepared. Table 1 summarizes the mix propor-
trix design, micromechanical modelling and material sus- tions of the matrices used in this investigation. Four main
tainability indices for the environmental design. Nema- parameters were chosen for this study, namely:
tollahi et al. (2015) studied the mechanical properties of 1. Blended proportion between fly ash (FA) and ground
FA-based EGC with different types of activator combina- granulated blast furnace slag (GGBS), i.e., fly ash to
tions, and further extended their work by investigating binder ratio (FA/B) or slag to binder ratio (GS/B).
the effects of water-to-geopolymer solids ratio, sand size 2. Quartz powder to binder ratio, QP/B ratio
and sand content on the matrix properties and uniaxial 3. Solid alkali activator to binder ratio, A/B ratio
tensile performance of the composites (Nematollahi et al. 4. Water to binder ratio, W/B ratio
2016). The matrix materials used comprised FA, GGBS, QP
Realizing the challenges of handling user-hostile alka- and solid alkali activator, sodium metasilicate anhydrous.
line solutions and the necessity of heat curing in conven- FA and GGBS used in this study were obtained locally
tional geopolymer, Nematollahi et al. (2017a) developed from YTL Cement Bhd Malaysia. The oxide analysis of
an ambient temperature cured “one-part” EGC using the FA and GGBS determined by X-ray Fluorescence
solid-based activators and blended FA/GGBS. The devel- (XRF) analysis is shown in Table 2. The morphology of
oped EGC gave comparable strain hardening behaviour FA and GGBS obtained from a scanning electron micro-
to typical ECC and offered up to 76% less CO2 emissions scope (SEM) is shown in Fig. 1. It is obvious that FA par-
and 36% less energy consumption. Through a detailed ticles exhibited the shape of more smooth spheres while
micromechanics-based investigation, Nematollahi et al. GGBS particles were mainly anomalous angular shapes.
(2017b) also investigated the effect of using polyethylene The pozzolanic compound level of the FA
(PE) fibres on the tensile performance of one-part EGC. (SiO2+Al2O3+Fe2O3) is 78.2% and can therefore be clas-
Alrefaei and Dai (2018) studied different precursor ma- sified as Class F fly ash according to ASTM C618-12a
terials and hybrid combinations of steel and PE fibres on (ASTM 2012) (i.e., >70%). GGBS was off-white in col-
the matrix and composite properties of one-part EGC. our and contained at least two-thirds by mass of glassy
They found out that GGBS-based EGC performed better slag and possesses hydraulic properties when suitably ac-
in tensile strain hardening and multiple cracking behav- tivated. The sum of CaO, MgO and SiO2 in the GGBS
iours than blended FA/GGBS EGC composites. In addi- constituted 78.7% of the total mass while the basicity ra-
tion, composite mixtures with greater PE fibre volume tio (CaO+MgO)/(SiO2) was 1.69, which both satisfy the
fraction would achieve higher tensile strain capacity. requirements specified in the British Standard BS EN
Gather on the currently available literature, it is con- 197-1 (BSI 2011) (i.e., two-thirds for the sum of CaO,
vincing that one-part EGC is a viable and promising ma- MgO and SiO2 (by mass) and >1.0 for the basicity ratio).
terial with excellent performance. Despite that, there still High-purity quartz powder was used in this study, which
exist many underlying challenges relate to the mixture consisted of 97.2% SiO2 content and 99% minimum
design of one-part EGC, which involves more variables passing at 200 mesh.
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 206

Table 1 Mix proportions.


PVA
FA GGBS QP Activator Water
fibre*
Mix ID
FA/B GS/B QP/B A/B W/B
kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 Vol.%
ratio ratio ratio ratio ratio
M1 0.50 602.15 0.50602.15 00 0.08
96.34 481.72 0.40
M2 0.60 716.26 0.40477.50 00 0.08
95.50 477.50 0.40
M3 0.70 828.39 0.30355.02 00 0.08
94.67 473.36 0.40
M4 0.70 820.14 0.30351.49 00 0.10
117.16 468.65 0.40
M5 0.70 812.05 0.30348.02 00 0.12
139.21 464.03 1.96
0.40
M6 0.70 881.59 0.30377.83 00 0.08
100.75 440.80 0.35
M7 0.70 872.26 0.30373.82 00 0.10
124.61 436.13 0.35
M8 0.70 833.16 0.30357.07 0.10
119.02 0.08
95.22 416.58 0.35
M9 0.70 789.78 0.30338.48 0.20
225.65 0.08
90.26 394.89 0.35
Notes:
1. FA: fly ash, GGBS: ground granulated blast furnace slag, QP: quartz powder, FA/B: fly ash/binder ratio, GS/B: slag/binder
ratio, QP/B: quartz powder/binder ratio, A/B: activator/binder ratio, W/B: water/binder ratio.
2. Binder content (B) comprised FA and GGBS.
3. *PVA fibre content is by volume fraction (percentage by volume).

Table 2 Oxide composition of FA and GGBS from XRF (mass%).


Material SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2O K2O TiO2 MnO
FA (%) 43.36 20.34 14.52 9.25 4.86 1.76 2.04 1.32 0.99 0.14
GGBS (%) 29.2 12.3 1.73 43.1 6.35 4.85 - - - -
QP (%) 97.2 1.07 - - - - - - - -

Table 3 Physical properties of PVA fibre.


Diameter Length Specific gravity Tensile strength Modulus of elasticity
Fibre ID
(μm) (mm) (g/cm3) (MPa) (GPa)
RECS 100L 100 12 1.3 1200 28

One-part or “just add water” geopolymer corresponds 2.2 Mixing and curing process
to using a solid-based alkaline activator to synthesize ge- All mixes were prepared using a 5-liter planetary mixer.
opolymer composites. The solid alkali activator used in Solid and dry materials, which comprised of FA, GGBS,
this study was sodium metasilicate anhydrous. The chem- QP and solid activator, were first added into the mixer
ical contents of the sodium metasilicate anhydrous used and then dry-mixed for 3 minutes. The water was then
in this study were 51.10% Na2O and 46.53% SiO2 with gradually added to the dry materials and the mixing was
modulus ratio (Ms) and relative densities of 0.91 and 2.4, continued. Every 3-minute intervals the mixing was
respectively. Polyvinyl alcohol, (PVA) fibres produced stopped for scraping the paste attached to the bottom and
by Kuraray Co. Ltd were used in this study at a moderate sides of the mixing bowl surface. This is to ensure a more
volume fraction of 1.96%. The physical properties of the uniform paste could be achieved. The whole mixing pro-
fibre are given in Table 3.

   
(a) Fly ash (b) Ground granulated blast furnace slag (GGBS)
Fig. 1 Morphology of fly ash and GGBS used in this study.
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 207

cess requires 12-15 minutes. The PVA fibres were gradu- in width by 80 mm in length in the middle section. The
ally added to the mixture afterwards. Once all fibres were tensile test was carried out by placing the specimen with
added, the composite mixture would be subjected to a jig at both ends and then performed using the universal
high-speed mixing to ensure well dispersion of the fibre. testing machine with a loading rate of 0.20 mm/minute.
After the fibre dispersion was confirmed, the fresh paste An extensometer was attached to one side of the middle
was then cast into the specimen moulds. section to measure the elongation over a gauge length of
Immediately after casting, the moulds were covered 80 mm. A total of five dogbone specimens were prepared
with plastic cling film to avoid water evaporation and in each mixture.
then left overnight for demoulding the following day. Af- Scanning Electron Microscopy (SEM) and Energy
ter demoulded the next day, the specimens were fully Dispersive X-Ray Spectroscopy (EDS) tests were per-
wrapped with a plastic sheet and left to cure under an am- formed to evaluate the microstructure and morphology
bient condition in the laboratory until the day of testing. properties of the one-part geopolymer matrix. The SEM
and EDS analyses were conducted using Hitachi 3400N
2.3 Test specimens and procedures VP-SEM. All samples were taken from 50 mm cubes af-
Immediately after mixing, the flow table test (or flow ter compressive strength tests.
test) as per the standard ASTM C230 (ASTM 2014) was
conducted to determine the consistency of the fresh geo- 3. Test results and discussion
polymer paste. The flow spread diameter was targeted at
a minimum of 200 mm to ensure that desirable rheologi- 3.1 Fresh properties
cal properties and self-compacting capability of the paste The flow characteristics of all mixtures taken immedi-
can be achieved. Compressive strength tests were con- ately after mixing are presented in Fig. 3. Flowability of
ducted at 3, 7, 14 and 28 days of age. A total of twelve 50 the fresh state was visually observed on all mixtures.
mm cubes were prepared in each mixture to determine Good flowability spread and uniform fibre dispersion
the compressive strength. Before testing, each specimen were achieved during the mixing process. Generally, all
was also weighed to obtain its respective densities. mixtures except M9 obtained an average flow spread di-
Uniaxial tensile tests were performed on dogbone- ameter exceeding our target of 200 mm.
shaped specimens following the recommendation by the The influence of the binder proportion between FA and
Japan Society of Civil Engineers (JSCE 2008). Figure 2 GGBS on the flowability could be interpreted from mix-
shows the dimensions of the dogbone tensile specimens tures M1, M2 and M3. As shown from the results, larger
and also the final uniaxial tensile test setup. The speci- FA content or FA/B ratio exhibited better flowability on
men has a thickness of 13 mm, with a test area of 30 mm the mixtures. It is mainly attributed to the spherical nature

   
(b) Dimensions of the dogbone tensile specimens
(a) Test setup for uniaxial tensile test
according to JSCE recommendation (JSCE 2008)
Fig. 2 Uniaxial tensile test setup and details of the dogbone specimen.
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 208

of the FA particle shape that contributes greatly to the en- Similar to conventional OPC-based binders, water
hancement of flowability. The effect of GGBS in the FA- content is also expected to play an important role in af-
based geopolymer mixture was well-documented. Nath fecting flowability. As observed between mixture M3 and
and Sarker (2014) concluded that higher GGBS content M6 with an A/B ratio of 0.08, decreased water/binder
in the FA geopolymer mixtures reduces the workability (W/B) ratio from 0.40 to 0.35 caused the flow spread di-
and setting time. As clearly demonstrated between mix- ameter to be reduced by 16% accordingly. A similar ob-
ture M1 and M3, where indicated mixture M1 with a servation was also reported between mixture M4 and M7
higher GS/B ratio of 0.50 exhibited a lower flow spread with an A/B ratio equal to 0.10. It should be noted that a
diameter than mixture M3 with a GS/B ratio of 0.30. greater reduction in flowability could be observed from
Keeping binder proportion and water content constant, mixtures with a higher A/B ratio. As depicted in mixture
the influence of the amount of solid alkali activator on M4 and M7, up to 31% reduction in flowability was at-
the flowability could be determined from mixture M3, tained compared with mixture M3 and M6 of only 16%
M4 and M5. It revealed that flowability reduces with a reduction.
gradual increase in the amount of activators. As demon- From mixtures M6, M8 and M9, it is clearly shown
strated in mixture M5 with an activator/binder (A/B) ratio that the addition of quartz powder (QP) reduced the flow-
equal to 0.12 attained a 13% reduction in the flow spread ability. Mixture M8 and M9 were added with 10% and
diameter compared with mixture M3 with an A/B ratio of 20%, by binder content, of QP, respectively. Their results
0.08. indicated a reduction of flow spread diameter up to
21.5% and 34.7% respectively compared with mixture
M6 without QP. Mixture M9 attained an average flow
spread diameter of 172.25 mm, which falls below the tar-
get average flow spread diameter of 200 mm.

3.2 Compressive strength


The compressive strengths of all mixtures taken at 3, 7,
14 and 28-days are presented in Fig. 4. Generally, all
mixtures show gradual strength development over the
age of curing. For ease of comparison, the average flow
spread diameters obtained in each mixture are also dis-
played along in the figure. Full results of the compressive
strength are given in Table 4.
Figure 4(a) summarizes the effect of various binder
proportions between FA and GGBS on compressive
strength. The trend indicates that the compressive
Fig. 3 Average flow spread diameters and percentage
strength reduces with the GGBS content. Mixture M1
flow.

Fig. 4 Compressive strength at 3, 7, 14 and 28 days of one-part geopolymer composites.


W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 209

Table 4 Mechanical properties of one-part geopolymer composites.


Average compressive strength (MPa) First cracking Ultimate tensile Tensile strain
Mix ID strength σfc* strength σult* capacity εcu* σult/σfc
3 days 7 days 14 days 28 days
(MPa) (MPa) (%)
M1 25.37 33.44 37.69 47.17 1.329 ± 0.140 1.367 ± 0.118 1.155 ± 0.093 1.029
M2 21.05 30.47 35.95 45.13 1.017 ± 0.144 1.270 ± 0.077 1.054 ± 0.528 1.249
M3 12.56 27.39 30.93 41.99 0.509 ± 0.385 1.245 ± 0.074 1.183 ± 0.252 2.446
M4 14.11 28.28 34.19 39.04 - - - -
M5 18.68 31.89 44.39 48.05 - - - -
M6 13.55 29.71 31.29 47.84 0.935 ± 0.128 2.506 ± 0.160 1.809 ± 0.053 2.680
M7 12.76 26.89 50.17 56.92 1.322 ± 0.171 2.596 ± 0.090 2.251 ± 0.107 1.964
M8 19.83 37.55 44.72 47.88 2.871 ± 0.302 3.220 ± 0.279 1.828 ± 0.261 1.122
M9 21.01 37.43 49.83 58.77 2.272 ± 0.159 4.374 ± 0.247 2.086 ± 0.245 1.925
Notes:
1. All dogbone specimens of mixture M4 and M5 were damaged during handling, therefore no values of σfc, σult and εcu were
obtained.
2. σfc is defined as the point where nonlinearity in the tensile stress-strain curves becomes evident, as proposed by Kim et al.
(2008), σult is defined as the point of peak ultimate stress in a tensile stress-strain curve, and εcu is defined as the point of ultimate
strain capacity before strain softening begins to occur in a tensile stress-strain curve.
3. *These values indicate average ± standard deviation.

with a GS/B ratio equal to 0.50 obtained an average com- pores and voids of the matrix resulting in a denser micro-
pressive strength at 28-days equal to 47.17 MPa. When structure. Furthermore, it could improve pore shape and
the GS/B ratio is reduced to 0.30 as in mixture M3, the size distribution, which substantially impacts compres-
average compressive strength attained at 28-days is 41.99 sive strength development. As shown in Fig. 4(d), mix-
MPa, i.e., 10.98% lower than M1. It should be noted that ture M9 with QP/B=0.20 achieved substantial compres-
the binder proportion between FA and GGBS at 70:30% sive strength at 28-days of 58.77 MPa i.e., 22.8% higher
(mixture M3) achieved the highest flowability with an than M6 without QP. It should be noted that compressive
average flow spread diameter up to 313.75 mm. strength at 28-days for mixture M8 was expected to be
Figure 4(b) shows that compressive strength in all higher than M6. This might be caused by poor handling
ages of curing increases with the amount of alkali activa- and errors during the period of testing. However, for
tor. It is expected that a high amount of alkali activator other ages of testing, it was clearly observed that mixture
encouraged more alkali activation process with the alu- M8 had higher compressive strength than M6 at 3, 7 and
minosilicate precursor materials, formation of more N-A- 14-days.
S-H/C-A-S-H gels with denser morphology, which even-
tually led to high compressive strength. Mixture M5 with 3.3 Uniaxial tensile performance
an A/B ratio of 0.12 attained a compressive strength at 3.3.1 Micromechanics of ECC
28-days of 48.05 MPa, corresponding to 14.4% higher According to the micromechanics design criteria of ECC
than mixture M3 with an A/B ratio of 0.08. (Li et al. 2001; Kanda and Li 1999), to ensure the attain-
Effects of water content (or W/B ratio) on the compres- ment of pseudo strain hardening (PSH) behaviour with
sive strengths are depicted in Fig. 4(c). Mixtures with multiple cracking, two criteria conditions must be satis-
lower W/B ratios attained higher compressive strength fied. There are strength criterion and energy criterion.
with a substantial reduction in flowability (up to 31% be- The strength criterion states:
tween mixtures M4 and M7). The strength gain is even
higher for a mixture with a high A/B ratio (mixture M7). σ fc  σ 0 (1)
It is known for facts (Hajimohammadi and van Deventer
where σ0 is the maximum fibre bridging capacity (or ul-
2017; Teo et al. 2022) that low water content would cre-
timate tensile strength of the composite σult); and σfc is
ate a high alkalinity system that encourages the greater
the tensile first cracking strength of the composite. Satis-
dissolution of SiO2 from the precursor materials and al-
faction of this strength criterion ensures that after initia-
kali activator. More participation of SiO2 in stages of gel
tion of the first crack, immediate failure with loss of ca-
formation implied the generation of a denser matrix and
pacity does not occur.
higher compressive strength. As shown in Fig. 4(c), mix-
The second criteria condition is the energy criterion
ture M7 had A/B=0.10 and W/B=0.35 attained an aver-
which states:
age compressive strength at 28-days of 56.92 MPa, which
is 19% and 45.8% higher than M6 with A/B=0.08 and M4 J tip  J b (2)
with W/B=0.40 respectively.
The addition of QP improves the compressive strength where J'b is the complementary energy calculated from
of the mixtures, as shown in Fig. 4(d). According to the bridging stress (σ) versus crack opening () curve of
Rashad (2018), QP is an excellent filler that could fill the strain hardening composite as shown in Fig. 5; and Jtip is
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 210

the crack tip toughness can be estimated from the follow- strength and ultimate tensile strength were found in mix-
ing equation: tures incorporated with quartz powders. Mixture M8
achieved the highest first-cracking strength with an aver-
K 2m age value of 2.871 MPa. On the other hand, mixture M9
J tip  (3)
Em achieved the highest ultimate tensile strength with an av-
erage value of 4.374 MPa. It should be noted that none of
where Km and Em are the fracture toughness and elastic the mixtures exceeded the tensile strain capacity of 3%.
modulus of the matrix, respectively. The energy criterion This may probably cause by the low viscosity of the mix-
assures steady-state flat crack propagation mode can be tures as confirmed by the high average flow spread diam-
attained where the crack opening is uniform at ss. This eters shown in Fig. 3. It is reported by Si et al. (2020) and
requires a balance of energy so that the work done due to Zhang et al. (2022) that the viscosity of the mortar matrix
applied tensile load σss must equate to the energy required could tailor the fibre dispersion and affect significantly
to break down the crack tip material Jtip and open the the hardened properties.
crack against fibre bridging from 0 to ss (Li 2012). The influence of FA content on the tensile performance
According to the two criteria conditions for PSH be- is illustrated in mixtures M1, M2 and M3. As shown in
haviour [Eqs. (1) and (2)], Kanda and Li (2006) proposed Table 4, increasing FA content in the proportion resulted
two performance indices, namely stress-performance in- in a reduction in the first cracking strength (σfc) and ulti-
dex (σult/σfc) and energy-performance index (J'b/Jtip). Both mate tensile strength (σult). According to Li et al. (2001),
performance indices must exceed unity to ensure achiev- low σfc of the composite is an indication of low Jtip. The
ing PSH behaviour in a fibre-reinforced composite. σfc of the mixture M2 and M3 were 23.5% and 61.7%
Therefore, the higher the performance indices the greater respectively lower than mixture M1. This implies that
the possibility of achieving saturated multiple cracking higher FA content (FA/B ratio) leads to lower Jtip which
and PSH behaviour, which results in a higher tensile is beneficial for the PSH behaviour of the composite. The
strain capacity εcu (Kanda and Li 2006; Nematollahi et al. reduction of σult in mixture M2 (7.1%) and M3 (8.9%)
2015). compared with M1 was mainly attributed to the interfa-
cial properties (Nematollahi et al. 2015, 2016). High FA
3.3.2 Tensile stress-strain responses content would probably lower the fibre-matrix interfacial
The uniaxial tensile stress-strain responses of the mix- bond strength resulting in lower fibre bridging strength
tures are presented in Fig. 6. The first-cracking strength, (lower σult). Based on the results, it has been found that
ultimate tensile strength, and tensile strain capacity from high FA content has a more pronounced influence on the
each mixture are summarized in Table 4. It should be σfc than σult. As shown, a larger reduction was observed
noted that the values depicted in Table 4 are based on the in σfc than σult. Therefore, as expected for mixtures with
average values taken from multiple tensile stress-strain high FA content, such as M3, a relatively high stress-per-
curves in a mixture. Also, included in Table 4 is the ratio formance index (σult/σfc ratio) was obtained.
of the ultimate tensile strength (σult) to the first cracking The effect of water content (W/B ratio) on the tensile
strength (σfc). As shown from the σult/σfc ratio, the ulti- performance can be explained between mixtures M3 and
mate tensile strength for all mixtures was higher than the M6. It indicates that the reduction of the W/B ratio from
first cracking strength which satisfies the strength crite- 0.40 to 0.35 greatly enhanced the tensile performance of
rion of PSH. the composite. As shown in Table 4, the σfc, σult and εcu
Based on the observation, the highest first-cracking of the mixture M6 with W/B=0.35 were 83.7%, 101.3%
and 52.9% respectively higher than mixture M3 with

Fig. 5 Typical σ-δ curve for tensile strain hardening composites.


W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 211

W/B=0.40. In terms of σult/σfc ratio, interestingly it also the σfc and σult. As shown in Table 4, the σfc of the mixture
indicates improvement with M6 obtained σult/σfc ratio of M8 and M9 with QP was 207.1% and 143% respectively
2.68, which is 9.6% higher than M3. Increasing the higher than mixture M6 without QP. While for σult, mix-
amount of alkali activator further increases the σfc, σult ture M8 and M9 achieved 28.5% and 74.5% higher than
and εcu of the composite. As shown in mixture M7 with M6. The results from this observation indicate that the
A/B=0.10, the σfc, σult and εcu were 41.4%, 3.6% and addition of QP enhances greater on the σfc than σult. This
24.4% respectively higher than mixture M6 with ultimately would reduce the stress-performance index
A/B=0.08. The interpretation gathered from the results (σult/σfc ratio), as clearly demonstrated in mixture M8 and
indicates that a lower W/B ratio and increased A/B ratio M9. As mentioned earlier, high σfc reflects high Jtip or ma-
could enhance the matrix toughness and fibre-matrix in- trix fracture toughness Km [see Eq. (3)]. Therefore, this
terfacial bond strength, which is in favour of attaining may also result in a lower energy-performance index
high σult and εcu values. (J'b/Jtip), which may unfavour the attainment of saturated
The addition of QP enhances the packing effect of the multiple cracking and PSH behaviour. Interestingly, the
composite with denser microstructure, which enhances

Fig. 6 Tensile stress-strain responses of one-part geopolymer composites.


W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 212

εcu of the mixture M8 and M9 still shows a marginal in- and partially reacted FA particles in the matrix could be
crease of up to 1.1% and 15.3% respectively compared observed, as clearly shown in mixture M3. From the EDS
with M6. analysis, it indicates that mixture M3 with reduced
GGBS content had a lower amount of Si, Al and Ca than
3.4 Microstructure properties (SEM and EDS mixture M1. It also confirms that the main reaction prod-
analysis) uct in FA/GGBS-based mixtures is C-A-S-H geopolymer
Figure 7 presents the SEM images and EDS analysis of gel in the binding phase (Askarian et al. 2019; Oderji et
the one-part EGC mixtures measured after 28-days of age. al. 2019).
The SEM micrograph of mixture M1, M2 and M3 shows Increasing alkali activator content as demonstrated in
that with a larger FA proportion to GGBS more unreacted mixture M3, M4 and M5 clearly show a more compact

Fig. 7 SEM images and EDS analysis of one-part geopolymer mixtures (continue to p.213 and p.214).
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 213

and denser microstructure with lesser unreacted particles. The reduction of water content (W/B ratio) further en-
As widely known, a high amount of alkali activator con- hances the microstructure. As demonstrated between
tent encourages the geopolymerisation process and mixtures M3 and M6 (or M4 and M7), reduced water
greater dissolution of precursors, which leads to the for- content possesses a more homogenous microstructure.
mation of more geopolymer gels. This is supported by the This is also supported by the compressive strength results
compressive strength results shown in Fig. 4(b). The shown in Fig. 4(c), where compressive strength increased
EDS results also confirmed the reaction products of the with the reduction of the W/B ratio.
mixtures, which show an increase of Si, Al, Ca, and Na The effect of the inclusion of QP in mixture M8 and
content with an increase of alkali activator. M9 showed enhancement in the microstructure. The EDS
results confirm a substantial reduction in voids with the

Fig. 7 SEM images and EDS analysis of one-part geopolymer mixtures (continue from p.212 to p.214).
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 214

addition of QP content. It is without a doubt that the mix- 3.5 Discussion of results
ture M8 and M9 possess higher compressive strength due The results from this investigation show that effect of in-
to the denser and less porous matrix compared with M6. creased alkali activator content and reduced water con-
This also explained the rationale behind of high matrix tent enhances the mechanical properties of the compo-
toughness and fibre-matrix interfacial bond strength ob- sites, namely compressive strength, σfc, σult and εcu. The
served from the tensile performance on mixture M8 and stress performance index (σult/σfc ratio) with reduced wa-
M9. ter content shows improvement. On the other hand, with
increased alkali activator content, it shows a decline in

Fig. 7 SEM images and EDS analysis of one-part geopolymer mixtures (continued from p.212 and p.213).
W. Teo, K. Shirai and J. H. Lim / Journal of Advanced Concrete Technology Vol. 21, 204-217, 2023 215

the stress performance index. The quantities of alkali ac- attainment of PSH behaviour of the composite due to
tivator content have a pronounced influence on the σfc, low matrix fracture toughness and fibre-matrix inter-
where a higher increment was found in σfc than σult. The facial bond strength.
σfc of the composite corresponds to the matrix fracture 2. An increasing amount of alkali activator content en-
toughness Km, which is directly proportional to the crack couraged more alkali activation processes with the
tip toughness, Jtip. Therefore, high σfc produces high Km aluminosilicate precursor materials, the formation of
value (or Jtip), which may also result in a lower energy- more C-A-S-H gels in the binding phase with denser
performance index (J'b/Jtip). The improved adhesion be- morphology, which eventually led to high compres-
tween the geopolymerisation products and the fibres due sive strength. Although a marginal reduction in flow-
to increase activator content was mainly responsible for ability took place, generally, all flow spread diameters
the high matrix fracture toughness of the mixtures. still exceeded more than 250 mm. The SEM and EDS
Based on current literature, it is a known fact that high results confirmed the microstructure transformation
compressive strength induces high matrix fracture tough- and increased the quantities of reaction products when
ness, which may cause unfavoured circumstances on the the alkali activator content increased.
tensile ductility. For instance, Ling et al. (2019) devel- 3. Similar to conventional concrete, a reduction in water
oped a FA/GGBS-based EGC with high compressive content would reduce the flowability of the mixtures
strength of up to 102 MPa but achieved a relatively low and increase compressive strength. This is supported
tensile ductility of only 1.0%. On the other hand, Nguyen by the SEM and EDS results, which showed mixtures
et al. (2021) developed an ultra-ductile FA-based EGC with low water content possess a more homogeneous
with a tensile strain capacity of up to 13.7% but with low microstructure.
compressive strength, around 20 MPa. This observation 4. Low water content (W/B ratio) and increased alkali
was also shown in our mixtures added with QP. As QP activator content (A/B ratio) would enhance the matrix
facilitate denser microstructure, enhancement in the me- toughness and fibre-matrix interfacial bond strength,
chanical properties of the matrix could be observed. which in favour of increasing first-cracking strength
However, this does not reflect any substantial benefit to σfc, ultimate tensile strength σult and tensile strain ca-
tensile ductility. pacity εcu.
It should be noted that all mixtures do not undergo a 5. QP offer an excellent filler that could fill the pores and
substantial tensile strain capacity of more than 3%. There voids of the matrix resulting in a denser microstructure.
is still more work that needs to be done. A revisit into It is supported by SEM and EDS results which show
proper material selection and mixture design should be that a huge substantial reduction in voids; and more
explored. The present study does not investigate the use compact and homogenous microstructure were formed
of fine silica sand. For practical reasons, it is essential to when added with QP. Therefore, it is without surprise
use silica sand to reduce cement content and improve the that significant enhancement of the compressive
elastic modulus of the material. Although this can induce strength took place.
high matrix fracture toughness and cracking strength. In 6. Addition of QP had a higher influence on the σfc than
addition, the viscosity of the matrix is crucial for tailoring σult, which may lead to a reduction in the stress-perfor-
fibre dispersion and should be further investigated. mance index (σult/σfc ratio) and possibly result in a
lower energy-performance index (J'b/Jtip). This may
4. Conclusions unfavour the attainment of saturated multiple cracking
and PSH behaviour.
This paper summarizes the findings on the characteriza-
tion of one-part EGC under the influence of various pa- Acknowledgements
rameters, namely binder proportion between FA and The authors would like to thank former research assistant
GGBS, alkali activator/binder ratio, water/binder ratio Mr Woo Chee Zheng (Ron) for his contribution to the la-
and QP/binder ratio. Fresh and mechanical properties boratory work. This research was funded by the Ministry
consisting of compressive strength and tensile perfor- of Higher Education (MOHE) Malaysia through the Fun-
mance, along with microstructure analysis were con- damental Research Grant Scheme (FRGS), grant number:
ducted. The following conclusions can be derived from FRGS/1/2018/TK01/HWUM/02/3, and in part by the
this study: 2021 ASAHI GLASS Foundation Research Grant
1. Increasing FA content in the binder proportion favour through with Hokkaido University, Sapporo, Japan.
the flowability of the mixture. This is mainly due to
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