Journal of Cleaner Production 225 (2019) 1e10

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Journal of Cleaner Production

journal homepage: www.elsevier.com/locate/jclepro

Fresh and hardened properties of one-part fly ash-based geopolymer

binders cured at room temperature: Effect of slag and alkali activators
Sajjad Yousefi Oderji a, b, Bing Chen a, b, *, Muhammad Riaz Ahmad a, b,
Syed Farasat Ali Shah a, b
a
State Key Laboratory of Ocean Engineering, Shanghai Jiao Tong University, Shanghai, 200240, PR China
b
Department of Civil Engineering, Shanghai Jiaotong University, Shanghai, 200240, PR China

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

Article history: Geopolymers are considered to be a sustainable and environmentally friendly replacement for ordinary
Received 19 January 2019 Portland cement as they lead to a reduction in carbon footprint. The dosage and type of precursors and
Received in revised form alkali activators have been known to be important parameters affecting the fresh and hardened prop-
13 February 2019
erties of geopolymers. This study investigates the effect of slag content as well as type and dosage of
Accepted 27 March 2019
Available online 1 April 2019
alkali activators on one-part fly ash-based geopolymers cured at room temperature. Different ratios of fly
ash were replaced with slag as a CaO-rich precursor. Setting time and flowability tests were carried out to
evaluate the fresh properties, compressive and flexural strength experiments were conducted to
Keywords:
One-part geopolymer
determine the mechanical properties of the geopolymers. The mineralogy and microstructure of the
Alkaline activator samples were evaluated by Optical microscope, X-ray Diffraction (XRD) and Scanning Electron Micro-
Room temperature curing scope (SEM-EDS) analysis. The experimental results revealed that the increase of slag content improved
Fly ash/slag ratio the strength and reduced workability. Moreover, some microcracks were observed when over 15% of fly
ash was replaced with slag. In terms of activators, the sodium metasilicate anhydrous provided optimum
strength and higher flowability compared to the others. Microstructural analysis results showed the
presence of more unreacted particles when less than 8% Na2SiO3 content as alkaline activator and also
less than 15% slag as replacement was used in the system.
© 2019 Elsevier Ltd. All rights reserved.

1. Introduction Geopolymers (GPs) have the potential to reduce energy con-

sumption and CO2 emissions by approximately 60% and 80%,
Ordinary Portland Cement (OPC) is one of the most commonly respectively, and are widely recognized as sustainable alternatives
used construction materials throughout the world. The high con- to OPC (Assi et al., 2018; Nematollahi et al., 2015; Van Deventer
sumption of OPC has led it to become a prominent source of CO2 et al., 2010). The terms “geopolymer” (GP) and “alkali-activated
emissions (Miller et al., 2016; Shen et al., 2017; Zhang et al., 2018). material” (AAM) have been used by different researchers. However,
OPC production is an energy-intensive process with the subsector the discussion regarding whether “GP” is the subset of “AAM” or it
consuming about 12e15% of the total worldwide industrial energy is a separated material class is still ongoing. These materials provide
consumption (Ali et al., 2011). The considerable energy demand, a beneficent utilization of industrial wastes (Humbert and Castro-
cost and supply of raw materials along with the CO2 emissions are Gomes, 2019; Zhang, 2013). The consequence of using partially or
significant concerns for cement industries (Ali et al., 2011; Zhang totally as precursors contribute to the reduction of industrial
et al., 2018). Therefore, offering environmentally friendly alterna- wastes in the landfill (Qin et al., 2018; Sandanayake et al., 2018; Tan
tives to OPC has become the subject of many studies (Shekhovtsova et al., 2018). In these materials, superior properties such as higher
et al., 2018; Shi et al., 2015; Vishwakarma and Ramachandran, strength, lower creep and shrinkage, better heat resistance, etc. can
2018). be achieved by proper material selection and mix proportion
design (Bernal and Provis, 2014; Hojati and Radlin
ska, 2017; Yazdi
et al., 2018).
* Corresponding author. State Key Laboratory of Ocean Engineering, Shanghai Conventional (two-part) geopolymes are prepared by poly-
Jiao Tong University, Shanghai, 200240, PR China. merization of the alumino-silicate materials in a reaction with an
E-mail address: [email protected] (B. Chen).

https://doi.org/10.1016/j.jclepro.2019.03.290
0959-6526/© 2019 Elsevier Ltd. All rights reserved.
2 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10

alkaline solution such as potassium hydroxide (KOH), sodium hy- The effects of CaO content, as well as type and content of alkali
droxide (NaOH), and sodium silicate or their combination (Provis, activator on the fresh and hardened properties of one-part fly ash-
2009; Somna et al., 2011; Yousefi Oderji et al., 2017). The most based geopolymer binders cured at room temperature are inves-
widely used alumino-silicates for alkali activation and also geo- tigated in this paper. Flowability and setting time along with
polymerisation are fly ash (FA), granulated blast furnace slag compressive and flexural strengths tests were performed to study
(GGBS), rice husk ash (RHA), metakaolin (MK), and wood ash (WA) the fresh and hardened properties of the geopolymer binders,
(Cheah et al., 2017; Mehta and Siddique, 2018; Zhuang et al., 2016). respectively. The microstructure and phase distribution of samples
In order to ease the production of GPs, recent studies have been were investigated by Optical microscope, Scanning Electron Mi-
more focused on one-part geopolymer materials (Duxson and croscopy (SEM-EDS) and X-ray Diffraction (XRD) analysis.
Provis, 2008; Nematollahi et al., 2015). One-part ‘‘just add water”
geopolymer concrete is a mix of solid alkaline activator and 2. Experimental procedure
alumino-silicate precursor, which can be used similarly as con-
ventional concrete (Adesanya et al., 2018; Luukkonen et al., 2018). 2.1. Materials
The properties of both one-part and two-part GPs are signifi-
cantly influenced by the dosage and type of the precursors and The precursors used in this study were class F fly ash (FA) and
activators. Calcium rich alumino-silicates such as slag are some- ground granulated blast furnace slag (GGBS), in accordance with
times used with low reactive precursors such as class F fly ash (FA) ASTM C 618 and ASTM C 989, respectively. The oxide composition of
to boost the reactivity of the system, and as a result, eliminates the precursors measured through X-ray fluorescence (XRF) test are
need of heat curing (Rashad, 2014; Saha and Rajasekaran, 2017; listed in Table 1. The particle size distribution was evaluated by
Shang et al., 2018). When the FA is replaced with GGBS, the primary Laser-diffraction analysis (LDA) shown in Fig. 1-a. Crystallinity and
component that mainly changes is the CaO content, which has been phase of raw materials (FA and GGBS) were analyzed by XRD as
reported as an effective component for the development of the shown in Fig. 1-b. Here, it can be seen that the nature of slag is
compressive strength in both GPs and AAMs (Lee and Lee, 2013; amorphous and fly's ash main crystalline peaks are quartz, mullite,
Temuujin et al., 2009). However, at high ratios of FA replacement calcite and hematite. The solid alkaline activators used in this study
with slag, where a considerable amount of CaO is presented in the were sodium hydroxide powder (NaOH, purity
96%), potassium
system, hardening occurs rapidly, compromising the applicability hydroxide pellets (KOH, purity
85%) and sodium silicate anhy-
of the system. (Pern and Hanzlí cek, 2016; Saha and Rajasekaran, drous (Na2SiO3 modulus of 0.92, Na2O ¼ 50.2%, and SiO3 ¼ 46%).
2017). Therefore, the amount of calcium in the system needs to
be optimized with consideration to its effects on both fresh and
2.2. Mix proportions and mixing procedure
hardened properties of geopolymer materials.
The experimental work in this study was conducted in three steps.
In step-I, the main focus was to study how CaO of the slag affects the
Table 1
mechanical strength and workability of one-part geopolymer binders
Chemical composition of fly ash and slag.
cured at room temperature. To this end, four mixtures were prepared
Main chemical oxides Fly ash (wt.%) Slag (wt.%) by replacement of FA with GGBS (as a CaO rich source, see Table 2) by
SiO2 49.4 35.4 0%, 10%, 15% and 20% (% by mass). Sodium metasilicate anhydrous
Al2O3 22.5 12.4 (Na2SiO3) was used at 8% of the mass of precursor(s). The GGBS mass
CaO 6.84 41.9
percentage was kept below 20% to produce a workable mix with
MgO 0.955 5.91
Fe2O3 4.89 0.424 satisfactory mechanical strength properties (Lee and Lee, 2013). Step-
Na2O 0.575 0.275 II concentrates on further optimizing the concentration of sodium
K2O 1.26 0.261 silicate on the selected mixture from step-I, with regards to work-
TiO2 1.36 0.650 ability and mechanical strength. Different concentrations of sodium
MnO 0.0746 0.175
silicate (8%, 7% and 6% by mass-AA3, AA3-SS7% and AA3-SS6%) were

Fig. 1. Fly ash and slag -a) Particle size distribution. -b) XRD pattern.
 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10 3

Table 2
Mix proportions and molar ratios in different mixes.

Mix Alkaline Activator Mix Proportions Molarity

Ad* (%) FA/GGBS SiO2 (wt.%) Na2O (wt.%) Al2O3 (wt.%) CaO (wt.%) Si/Al Na/Al CaO/Al2O3 CaO/SiO2 Na2O/CaO
(mol/mol) (mol/mol) (mol/mol) (mol/mol)

AA1 SS 8 100/0 49.16 4.25 20.84 6.33 2 0.34 0.55 0.14 0.61
AA2 SS 8 90/10 47.87 4.22 19.9 9.58 2.04 0.35 0.88 0.21 0.4
AA3 SS 8 85/15 47.22 4.21 19.43 11.2 2.06 0.36 1.05 0.25 0.34
AA4 SS 8 80/20 46.57 4.21 18.97 12.83 2.08 0.36 1.23 0.3 0.3
AA3-SS7% SS 7 85/15 47.23 3.78 19.62 11.31 2.04 0.32 1.05 0.26 0.3
AA3-SS6% SS 6 85/15 47.24 3.34 19.8 11.42 2.03 0.28 1.05 0.26 0.26
AA-SH SH 5.5 85/15 44.83 4.38 19.89 11.47 1.91 0.36 1.05 0.27 0.35
AA-K K 8 85/15 43.8 e 19.43 11.2 1.91 e 1.05 0.27 e
AA-SS/SH SSþSH (SS/SH ¼ 2.5 7.4 85/15 46.32 4.4 19.55 11.27 2.01 0.37 1.05 0.26 0..35

FA (Fly Ash-type f); GGBS (Slag); SS (Na2SiO3); SH (NaOH); K (KoH).Ad*(Activator dosage was considered as the mass% of precursors).

investigated. In the final step, three mixtures were made in order to used for flowability measurements. The initial setting time is
compare different types of alkaline activators, Na- based and K-based. calculated using Vicat apparatus according to the requirements of
In the first two mixtures (AA-SS/SH and AA-SH), NaOH was used with ASTM standard C191. The compressive strength test was conducted
and without Na2SiO3 (Na2O content was the same as that of the op- according to the requirements of ASTM C 109. Both compressive
timum condition in step- II). KOH, as a commonly used activator in and flexural strength tests were performed using a MTS servo hy-
geopolymers, was used with the same mass content as sodium silicate draulic testing machine.
(8%). For all steps, water to binder ratio (w/b) was kept constant at 0.3.
The mix proportions and oxide molar ratios of different mixes are 2.4. Microstructural analysis
presented in Table 2.
FA, GGBS and alkali activator(s) were dry mixed for 2 min in The Optical microscope (Stereo microscope, model Stemi 508)
Hobart mixer. After that, water was added to the mixture and was used to monitor cracking in the samples. X-ray diffraction
mixed for 3 more minutes. Binders were immediately casted in (XRD) was performed using Diffractometer system XRD D8. The
40  40  40 mm cube (for compressive strength test) and source was operated at a voltage of 40 KV using CuKa radiation with
40  40  160 mm plastic prism molds (for flexural strength test), a 2q scanning range of 5 e50 . Scanning Electron Microscopy
and then vibrated for 2 min using an electric vibrator. All specimens (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) were per-
were demolded after 24 h of casting and cured at a temperature of formed to evaluate the morphological characteristics of the sam-
23 ± 2  C and relative humidity of 70 ± 10%. ples using COXEMEM-30PLUS Scanning Electron Microscope.

2.3. Fresh and hardened tests 3. Results and discussion

The flowability of mixtures was measured using a flow table at 3.1. Influence of slag content
different elapsed times. Flowability of mixtures with slag was
determined until no changes in the flow diameter of samples was The influence of slag content on the fresh properties of geo-
observed. Fig. 2 shows a schematic of the conical mold and method polymer binders are given in Fig. 3(a and b). It can be observed that

Fig. 2. Test method schematic for flowability of the binder.

4 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10

Fig. 3. Results of FA replacement with GGBS -a) Flow diameter. -b) Initial setting time.

increasing the slag content from 0% to 20% (CaO from 6.33 wt % to properties of the optimum mixture (AA3: FA/GGBS of 85/15) are
12.83 wt %) led to a reduction in the workability. In addition, there reported in this section. The compressive and flexural strengths of
was a higher initial flow and lower loss in flow rate in the mixtures geopoylmer mixtures containing various percentages of Na2SiO3 at
without slag than mixtures with slag. This is in line with the pre- 7 and 28 days are shown in Fig. 5(a and b). As can be seen from the
vious study on the effect of slag on the workability of geopolymer figure, Na2SiO3 concentration has a significant effect on the me-
mixtures (Al-Majidi et al., 2016). The loss of flowability with the chanical strength of samples. The compressive strength of mixtures
increase in slag content can be due to the presence of CaO and the drastically decreased when the percentage of Na2SiO3 was reduced
coarse and angular structure of slag particles (Ismail and El-hassan, below 8%. The loss of strength with a reduction in activator con-
2018; Shang et al., 2018). Fig. 3-b shows the initial setting time of centration can be attributed to changes in Na2O content and are to
the GPs. As the results show, setting time decreased dramatically related molar ratios, which are important factors for strength gain
when a higher concentration of CaO was involved in the system i.e. through alkali activation reaction (Bignozzi et al., 2014; Khedmati
larger amounts of FA was replaced with GGBS. et al., 2018). According to the mechanical results, 8% proved to be
The results of mechanical testing of the properties of one- part the optimum dosage of sodium silicate.
geopolymer binders are shown in Fig. 4(a and b). Mechanical
strength of mixtures increased with the increase in slag content.
The compressive strength increases significantly between 10% and 3.3. Comparison of different alkaline activators
20% slag substitution of fly ash. However, an increase in the slag
content from 15% to 20% exhibited a decrease in flexural strength The flowability of one-part fly ash-based geopolymer binders is
and an increase the compressive strength. Based on the test results, presented in Fig. 6-a. As can be seen from the figure, the rate of
it can be concluded that 15% is the optimum amount of FA to be changes in flow diameter is significantly affected by the type of
replaced with GGBS (AA3 mixture with 11.20 wt% of CaO) to obtain alkaline activator. In general, mixtures activated with only NaOH
a workable mixture with satisfactory strength characteristics. had the lowest flowability, which could be attributed to the higher
heat released due to the exothermic reaction of NaOH with water.
Flow loss is fastest in NaOH activated followed by KOH activated
3.2. Na2O dosage effect mixtures, which lose all their flowability in the first 4 and 10 min,
respectively. Na2SiO3-activated mixture (AA3) showed the highest
The influence of Na2O concentration on the mechanical initial flow amongst the group, but it dropped significantly from

Fig. 4. Mechanical results of fly ash replacement with slag -a) Compressive strength. -b) Flexural strength.
 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10 5

Fig. 5. Influence of alkali concentration on -a) Compressive strength. -b) Flexural strength.

Fig. 6. Influence of different alkaline activators on -a) Flow diameter. -b) Compressive strength.

24 cm at 4 min to around 11 cm at 10min. 3.4. Mineralogy and microstructure

Fig. 6-b shows the compressive strength of one-part geo-
polymer binders activated with different type and concentration of 3.4.1. Optical microscope
activators at 7 and 28 days. It can be clearly seen from the graph Fig. 7 shows the microscopic images of one-part fly ash-based
that the compressive strength of mixtures is significantly influ- geopolmer binders with different ratios of slag. As can be
enced by the type of alkaline activator. As can also be observed observed from Fig. 7, some cracks appeared on the surface of
from Fig. 6-b, the compressive strength of mixtures activated with samples with 20% slag (AA4), which might be caused by shrinkage
sodium silicate i.e. mixture AA-SS/SH (activated with Na2SiO3 and of the reaction products (Lee and Lee, 2013). The reduction in
NaOH) and AA3 (activated only with sodium silicate) is signifi- flexural strength of samples with 20% slag (see Fig. 4-b) might be
cantly higher than other mixtures. This depicts that, the potential due to the presence of these microcracks.
of activation of Na2SiO3 is much higher compared to other acti- Optical microscopy was also performed on samples activated
vators used in this study. Similar results regarding the superior with different types of alkaline activators, and the images are
potential of activation of Na2SiO3 compared to other alkali acti- shown in Fig. 8. As can be seen from these images, white blooms
vators such as KOH, NaOH þ Na2CO3 and NaOH were also reported appeared on NaOH activated samples both with and without
in literature for alkali-activated fly ash geopolymers (Komljenovi
c Na2SiO3 (AA-SS/SH and AA-SH). The AA3 mix activated with 15% FA
et al., 2010). The compressive strength (at 28-day) of replacement with GGBS and with 8% of Na2SiO3 showed no signs of
NaOH þ Na2SiO3-activated binder was almost the same as that of surface cracking or white blooms (see Figs. 7 and 8).
Na2SiO3 activated binder in our study. However, based on the
experimental results in this study it can be concluded that AA3
3.4.2. XRD analysis
with 8% Na2SiO3 gives the best results in terms of both workability
The X-ray diffraction peaks of FA replacement with GGBS mix-
and compressive strength.
tures and different content of alkali activator mixtures are shown in
6 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10

Fig. 7. Samples with different fly ash replacement ratio.

Fig. 8. Samples with different solid alkaline activator.

Fig. 9(a and b). As can be observed from Fig, there were no signif- CeSeH gel coexist in the GP and AAM materials due to complex
icant differences between peaks of the mixtures except at around reaction mechanism (Bernal and Provis, 2014; Yip et al., 2005).
29 where a change in peak intensity can be seen in Fig. 9(a). One of These results might be a reason that high compressive strength was
the main reaction products of alkaline activation materials achieved when incorporating GGBS and using 8% of sodium silicate
including GGBS is CeSeH which mostly appears in the hump at the compared to 7% (see Figs. 4 and 5).
2q range of 25 e35 (Kim et al., 2013; Oh et al., 2010; Palomo et al.,
2007). In Fig. 9(a-b), a peaks centered around 29 were identified to 3.4.3. SEM&EDS analysis
be dominated by CeSeH phase. Moreover, aluminosilicate gel and The SEM images of the mixtures are shown in Fig. 10. According
 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10 7

Fig. 9. XRD patterns of samples. -a) Varying GGBS content. -b) Varying Na2SiO3 content.

Fig. 10. SEM Images at 2kx Magnification for various ratios of FA/GGBS.

to the figure, for each mixture there are different quantities of The SEM of AA3 (mixture with 8% Na2SiO3 (SS)) and AA3-SS7%
unreacted FA and GGBS particles along with the geopolymer mixtures were studied at higher magnifications of 5kx and 20kx
products. The microstructure of the mixtures containing various and are shown in Fig. 11. It is obvious that AA3-SS7%mixture con-
percentages of GGBS showed that the amount of C-A-S-H gel in- sists of larger amounts of unreacted particles of FA and GGBS with a
creases with the increase in slag content. The SEM analysis supports smaller amount of geopolymerisation products. The presence of
the compressive strength results (section 2.1) and is in line with more unreacted fly ash and slag particles at lower Na2SiO3 content
previous studies (Al-Majidi et al., 2016). In fact, AA4, with 20% of (AA3-SS7%) indicates that the dissolution of precursors was not
GGBS achieved the highest compressive strength and possessed the completed due to an insufficient amount of alkali activator content.
most homogeneous microstructure. Some microcracks were also In contrast, AA3 possesses a more homogeneous microstructure.
observed in sample with 20% slag, which might be caused by The SEM images of the AA3-(8%) and AA3-(7%) also supports the
shrinkage (Lee and Lee, 2013). This was also seen in microscopic compressive strength test results, where huge loss of strength was
image of AA4 (see Fig. 7). observed by reducing the amount of activator by only 1%.
8 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10

Fig. 11. SEM Images at 5kx and 20kx magnification for Na2SiO3-activated mixtures.

EDS analysis was performed on AA3-SS7% and AA3 to analyze 4. Conclusion

the constituents of the geopolymerisation products (see Fig. 12).
The presence of silicon, sodium, calcium and aluminum can be seen In this study, the influence of slag as well as type and content of
in the EDS images. The presence of these chemicals confirmed the alkali activator on one-part geopolymer binders cured at room
presence of aluminum-modified C-A-S-H gel in coexistence with N- temperature was investigated. Different alkali activators were
A-S-H gel (Puligilla and Mondal, 2013; Yazdi et al., 2018). compared and the optimum dosage and type of activator for one-

Fig. 12. EDS images of the AA3 and AA3-SS7%.

 S. Yousefi Oderji et al. / Journal of Cleaner Production 225 (2019) 1e10 9

part fly ash-based geopolmer was introduced. Following are the Na2O/SiO2molar ratio on properties of aggregate-paste interphase in fly ash-
based geopolymer mixtures through multiscale measurements. Constr. Build.
conclusions drawn from the study:
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Natural Science Foundation of China, Grant No.51778363. sium oxysulfate cement based lightweight building materials. J. Clean. Prod.
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