Construction and Building Materials: N.K. Lee, H.K. Lee
Construction and Building Materials: N.K. Lee, H.K. Lee
Construction and Building Materials: N.K. Lee, H.K. Lee
h i g h l i g h t s
The setting time was decreased with increasing amounts of slag, water glass and NaOH.
The proper slag content in the mixture was determined to be 15–20% considering setting, slump and strength.
The mean pore size of alkali activated fly ash/slag mortar was smaller than that of OPC.
The increased mesopore volume resulted in decreases in the elastic modulus and long-term compressive strength.
a r t i c l e i n f o a b s t r a c t
Article history: This study aims to investigate the setting and mechanical properties of alkali-activated fly ash/slag con-
Received 14 September 2012 crete manufactured at room temperature. It also examines to what extent the slag in the alkali-activated
Received in revised form 3 May 2013 fly ash/slag mixture improves the mechanical properties of the mixture under room-temperature curing
Accepted 27 May 2013
conditions. A series of tests of the compressive strength, elastic modulus, splitting tensile strength, flow,
Available online 5 July 2013
setting time, and porosity of the alkali-activated fly ash/slag concrete were carried out. The test results
showed that the setting time decreased as the amount of slag and the concentration of the NaOH solution
Keywords:
increased. The proper slag content in an alkali-activated fly ash/slag mixture was determined to be 15–
Alkali activation
Fly ash/slag blended concrete
20% of total binder by weight considering the setting time and compressive strength of the alkali-acti-
Setting time vated fly ash/slag concrete cured at room temperature. In addition, the modulus of elasticity and splitting
Mechanical property tensile strength of the alkali-activated fly ash/slag concrete were slightly lower than those of ordinary
Room temperature manufacturing concrete as predicted by the ACI code and Eurocode 2. The total porosity of the alkali-activated fly
ash/slag mortar was similar to that of ordinary cement mortar, whereas the mean pore size tended to
be smaller than that of ordinary cement mortar.
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1202 N.K. Lee, H.K. Lee / Construction and Building Materials 47 (2013) 1201–1209
particular, a critical factor. Palomo et al. [26] concluded that an in- have been very little studied. The purpose of this paper is to inves-
crease in the curing temperature accelerated the activation of fly tigate the properties of alkali-activated fly ash/slag blended con-
ash with an alkali activator. In other work, van Jaarsveld et al. crete manufactured at room temperature through various
[31] studied the compressive strength change versus the curing experiments which assess the flow, setting time, compressive
age at various temperatures and showed that the compressive strength, strength development with time, elastic modulus, split-
strength increased by 100% when the curing temperature ranged ting tensile strength and porosity. The degree to which the slag
from 50 to 80 °C relative to that at 30 °C. In addition, Hardjito added to alkali-activated fly ash/slag concrete improves the
et al. [16] studied the compressive strength of a geopolymer mor- mechanical properties is also investigated here.
tar cured at 65, 70, and 80 °C for 24 h and showed that the early
compressive strength increased with the curing temperature. 2. Experimental program
These results show that curing temperature plays an important
role in the geopolymerization process of fly ash-based geopolymer. 2.1. Materials
However, high-temperature curing runs counter to the motiva-
In the present study, F-class fly ash and slag were used instead of Portland ce-
tion for not using Portland cement, i.e., reducing CO2 emissions, as ment. The chemical compositions and physical properties of the fly ash and slag are
it consumes more energy compared to room-temperature curing. listed in Table 1.
In addition, this type of curing process may diminish the degree NaOH with a purity level of 98% and water glass (Korean Industrial Standards,
of industrial field applicability. Therefore, the realization of the KS 3-grade; SiO2 (29%), Na2O (10%), H2O (61%), specific gravity 1.38 g/mL) were
used as alkali activators. Distilled water was used to dissolve the NaOH solid, and
room-temperature curing of geopolymer is critical for various the alkali activator was prepared by mixing NaOH solution with water glass. A solu-
commercial uses. tion of 85% phosphoric acid (H3PO4) was used as a set-retarding admixture to retard
Several studies have focused on adding slag containing CaO to the setting time of the alkali-activated fly ash/slag concrete. River sand and crushed
fly ash-based geopolymer in an effort to improve the compressive gravel were used as fine aggregate and coarse aggregate materials, respectively. The
physical properties of the sand and gravel are listed in Table 2.
strength of geopolymers cured under ambient room temperatures.
Several studies involving the use of calcium have reported that cal-
2.2. Mix proportion
cium has a positive effect on the compressive strength of the geo-
polymer [32,35]. Yip et al. [34] found that the form of added Ca2+ The mix proportion of the alkali-activated fly ash/slag paste is provided in Ta-
plays a significant role in improving the mechanical properties of ble 3 and denoted with specific codes. The labels ‘S’ , ‘M’, and ‘H’ represent the slag,
the geopolymer. It was reported that the simultaneous formation molarity of the NaOH solution and the phosphoric acid, respectively. The first num-
ber, ‘10’, ‘15’, ‘20’, ‘25’, or ‘30’, refers to the percentage of the slag replacement for
of a geopolymeric gel and calcium silicate hydrate (CSH) gel within
the fly ash by weight. The second number, ‘4’, ‘6’, or ‘8’, refers to the molarity
a single binder is possible [35]. Yip et al. [36] examined seven dif- (mol/l) of the NaOH solution. The third number, ‘0.5’, ‘1.0’, and ‘1.5’, refers to the ra-
ferent calcium-based materials to investigate the role of calcium in tio of water glass to NaOH solution by weight. The fourth number, 0.5–2.5, refers to
the geopolymerization process, finding that the effects of different the ratio of phosphoric acid to total binder (fly ash + slag) weight expressed as a
calcium silicates on geopolymerization depend significantly on the percentage.
Table 3 shows the mix proportions of alkali-activated fly ash/slag paste for the
crystallinity of the calcium-based materials and on the alkalinity of
setting time tests. The ratio of alkali activator to total binder (fly ash + slag) by
the alkali liquid used. weight was 0.38 for all specimens, and NaOH solutions with three different molar-
In a previous study of geopolymer mixed with fly ash and gran- ities (4 M, 6 M and 8 M) were chosen for the setting time tests. The mass ratios of
ulated blast furnace slag (GBFS), Kumar et al. [22] conducted the water glass to NaOH solution were 0.5, 1.0, and 1.5. The percentages of the slag
replacement for the fly ash by weight were 10%, 15%, 20%, 25% and 30%.
experiments to investigate the isothermal conduction calorimetry,
Because the 8 M NaOH solution caused the rapid setting of the alkali-activated
heat of hydration, microstructure, and compressive strength of fly ash/slag paste, the molarities of the NaOH solution were set to 4 M and 6 M and
geopolymer. In their study, they added GBFS at 5–50% of the total the mass ratios of the water glass to NaOH solution were 0.5 and 1.0 for compres-
binder by weight in an effort to improve the low reactivity of alka- sive strength tests. The mix proportions of alkali-activated fly ash/slag concretes
li-activated fly ash. Temuujin et al. [30] studied the influence of
CaO and Ca(OH)2 on the mechanical properties of fly ash-based Table 1
geopolymers and found that an addition of calcium to fly ash im- Properties of the binder materials.
proved the mechanical properties of the specimens cured at ambi- Fly ash (FA) Blast furnace slag
ent temperatures, whereas the mechanical properties of the
Chemical composition (%)
specimens cured at 70 °C instead showed a decrease. Lloyd et al. CaO 2.60 56.10
[23] revealed that fly ash/slag blended inorganic polymer cement SiO2 46.00 21.00
activated by silicate had a denser microstructure than that acti- Al2O3 33.00 17.00
vated by hydroxide. Recently, in alkali-activated granulated blast Fe2O3 10.50 0.62
SO3 – 0.77
furnace slag/metakaolin blends, the addition of metakaolin to the
slag mixture resulted in an increase in the total setting time, a Physical properties
Specific gravity (S.S.D) 2.38 2.90
reduction of the heat release and a slight reduction in the final Surface area (m2/kg) 290 (Blaine) 485 (Blaine)
mechanical strength of the mortars [4]. In geopolymers based on
Particle size (lm)
fly ash/slag blends, a moist curing condition led to a higher 10% 2.74 2.45
strength of the binders and a less porous system compared to a 50% 19.96 12.12
dry curing condition, as open air curing allowed water to evapo- 90% 95.33 32.89
rate, which reduced the water availability for the geopolymer ma-
trix to grow [17]. Thus, studies of the characteristics of fly ash-
based geopolymer concrete with slag, which contains a consider- Table 2
Properties of the aggregates.
able amount of CaO, may have significant implications with respect
to strength enhancement and the utilization of industrial by- Specific gravity Absorption
products. (%)
O.D. (oven dry S.S.D (saturated surface dry
To date, most studies on geopolymer mixed with fly ash and condition) condition)
slag have focused on micro-structural analysis, characterization, Sand 2.54 2.55 0.08
and the compressive strength of pastes and mortars. Mechanical Gravel 2.68 2.70 0.56
properties of geopolymer concrete mixed with fly ash and slag
N.K. Lee, H.K. Lee / Construction and Building Materials 47 (2013) 1201–1209 1203
Table 3
Mix proportion of alkali-activated fly ash/slag paste for the setting time tests.
Specimens Ratio of solution to binder Ratio of H2O to binder NaOH solution molarity (M) NaOH:water glassa Binder fly ash:slaga H3PO4 (%)
b
S20-8M0.5 0.38 0.28 8 1:0.5 80:20 0
S20-6M0.5b 0.38 0.28 6 1:0.5 80:20 0
S20-6M1.0b 0.38 0.27 6 1:1.0 80:20 0
S20-6M1.5b 0.38 0.26 6 1:1.5 80:20 0
S20-4M0.5b 0.38 0.30 4 1:0.5 80:20 0
S20-4M1.0b 0.38 0.28 4 1:1.0 80:20 0
S20-4M1.5b 0.38 0.27 4 1:1.5 80:20 0
S10-4M0.5b 0.38 0.30 4 1:0.5 90:10 0
S30-4M0.5b 0.38 0.30 4 1:0.5 70:30 0
S20-6M0.5c 0.38 0.28 6 1:0.5 80:20 0
S20-6M1.0c 0.38 0.27 6 1:1.0 80:20 0
S20-4M0.5c 0.38 0.30 4 1:0.5 80:20 0
S20-4M1.0c 0.38 0.28 4 1:1.0 80:20 0
S20-4M0.5c-H0.5 0.38 0.30 4 1:0.5 80:20 0.5
S20-4M0.5c-H1.0 0.38 0.30 4 1:0.5 80:20 1.0
S20-4M0.5c-H1.5 0.38 0.30 4 1:0.5 80:20 1.5
S20-4M0.5c-H2.0 0.38 0.30 4 1:0.5 80:20 2.0
S20-4M0.5c-H2.25 0.38 0.30 4 1:0.5 80:20 2.25
a
Mass ratio.
b
Specimens manufactured at 17 °C.
c
Specimens manufactured at 28 °C.
manufactured with four different types of alkali activators are listed in Table 4. The according to ASTM C 469-10. In addition, the pore size distribution of the alkali-
mix proportions were also determined according to the percentage (10–30%) of the activated fly ash/slag mortar was measured by the MIP method in accordance with
slag replacement for the fly ash by weight. The mass ratio of fine aggregate to bin- ASTM D 4284-07 using an Autopore VI machine by Micromeritics Corp. Mortar frag-
der (fly ash + slag) and the mass ratio of coarse aggregate to binder were 2 and 2.65, ments except for coarse aggregate materials were used for the MIP test. Splitting
respectively. tensile strength tests were conducted after 28 days of curing according to ASTM C
496-04.
Table 4
Mix proportion of alkali-activated fly ash/slag concrete.
Specimens Ratio of solution Ratio of H2O to NaOH solution Ratio of water glass Alkali solution Binder (kg/ Sand Gravel H3PO4
to binder binder molarity (M) to NaOH (kg/m3) m3) (kg/m3) (kg/m3) (kg/m3)
Fly Slag
ash
S20-6M0.5 0.56 0.42 6 0.5 215 293 88 760 1005
S20-6M1.0 0.56 0.40 6 1.0 215 293 88 760 1005
S20-4M0.5 0.56 0.44 4 0.5 215 293 88 760 1005
S20-4M1.0 0.56 0.42 4 1.0 215 293 88 760 1005
S10-4M0.5 0.56 0.44 4 0.5 215 344 34 760 1005
S15-4M0.5 0.56 0.44 4 0.5 215 316 63 760 1005
S20-4M0.5- 0.56 0.44 4 0.5 215 293 88 760 1005 8.5
H2.25
S25-4M0.5- 0.56 0.44 4 0.5 215 272 108 760 1005 8.5
H2.25
S30-4M0.5- 0.56 0.44 4 0.5 215 253 126 760 1005 8.5
H2.25
1204 N.K. Lee, H.K. Lee / Construction and Building Materials 47 (2013) 1201–1209
slag paste was very sensitive to the room temperature during the
manufacturing process.
Fig. 3 shows the setting times with the replacement ratio of the
slag for the fly ash. A higher replacement ratio of the slag for the fly
ash led to a faster setting time, as an increase in the CaO content,
which is the main chemical component of slag, accelerated the
hydration reaction of the mixture, as noted in a previous study
[34].
In Fig. 4, when phosphoric acid (H3PO4) was added to the mix-
ture up to 2.0% of the total binder (fly ash + slag) amount by
weight, the initial time increased slightly and the final time de-
creased. In contrast, when the ratio of phosphoric acid to binder
was 2.25% by weight, the initial and the final setting times in-
creased to 53 min and 90 min, respectively. Phosphoric acid had
a positive effect on retarding the setting of the alkali-activated
Fig. 1. Effect of the NaOH solution molarity on the setting time (solution/binder:
0.38, slag/fly ash: 0.2 by weight). fly ash/slag paste. Gong and Yang [14] found from SEM observa-
tions that phosphate in alkali-activated slag paste promoted a
new needle-like phase formation, which formed a membrane cover
Fig. 2. Effect of the ratio of water glass to NaOH solution by weight on the setting
time (solution/binder: 0.38, slag/fly ash: 0.2 by weight). Fig. 3. Effect of the slag on the setting time (solution/binder: 0.38, water glass/
NaOH solution: 0.5 by weight).
Table 5
Setting time test results.
on the surface of the slag particles. They concluded that the forma- solid in the mixture may degrade the compressive strength of alka-
tion of this new phase may cause the phosphate to retard the alka- li-activated fly ash/slag concrete.
li-activated slag paste. Chang et al. [6] stated that the phosphoric
acid reacted with calcium ions to produce Ca3(PO4)2 which corre- 3.3. Effect of slag on the compressive strength of alkali-activated fly
spondingly reduced the concentration of calcium ions. Therefore, ash/slag concrete
the formation of C–S–H slowed down. Similarly, the calcium from
slag in the present study was consumed to react with phosphoric Fig. 5 shows the compressive strength of the specimens with
acid, which retarded the hydration of alkali-activated fly ash/slag different replacement ratios of the slag for the fly ash. As shown
paste. in Fig. 5a, as the replacement ratio of the slag for the fly ash in-
creased from 10% to 15%, the compressive strength increased from
3.2. Effect of alkali activator on the compressive strength of alkali- 15.5 MPa to 23.0 MPa at 28 days. It was found in previous work
activated fly ash/slag concrete that 100% fly ash-based geopolymers without slag had very low
reactivity at room temperature [26,31]. Accordingly, a high-tem-
Table 6 shows the compressive strength of alkali-activated fly perature curing method was selected to increase the compressive
ash/slag concrete with time. Although larger amounts of NaOH so- strength of geopolymer. In the present study, the compressive
lid and water glass were added to the 6M1.0 specimen compared strength was improved by adding slag, which contains a large
to the other specimens, the compressive strength was lower than amount of CaO, into the mixture. This arose because the presence
that of the 4M0.5 and the 4M1.0 specimens. In addition, the com- of CaO improved the strength of the geopolymer by forming an
pressive strength of the 6M1.0 specimen at 28 days (26.6 MPa) was amorphously structured Ca–Al–Si gel, as also reported in a previ-
lower than that at 14 days (27.4 MPa), while the compressive ous study [34]. Kumar et al. [22] also suggested that the increase
strengths of the 4M0.5 and the 4M1.0 specimens at 28 days in the compressive strength with the addition of slag could result
(29.9 MPa and 30.7 MPa) were equal to or higher than those at from the formation of gel phases (C–S–H and A–S–H) and the com-
14 days (29.9 MPa and 27.4 MPa). According to a previous study, pactness of the microstructure. They concluded that the alkali acti-
geopolymer activated with NaOH solution alone showed a de- vation of slag is predominant in a fly ash/slag mixture at an
crease in its compressive strength compared to geopolymer acti- ambient temperature (27 °C), whereas the interaction between
vated with sodium silicate (Criada et al. [11]). Lloyd et al. [23] fly ash and slag is predominant at 60 °C [22]. Lloyd et al. [23]
also found from microstructural observations that geopolymer showed from a microanalysis that the calcium within the alkali-
activated with a silicate-based solution showed a more homoge- activated fly ash/slag binder is essential to the high early strength
neous microstructure than that activated with a NaOH-based solu- development, although the exact mechanism was not well under-
tion, which may improve the compressive strength. However, this stood in their study. Buchwald et al. [5] showed that the addition
does not correlate well with the results of the present study. The of slag into a slag/metakaolin mixture activated by a sodium
increase in the water glass content resulted not in an increase in hydroxide solution accelerated the condensation reaction of the al-
the compressive strength here. The reason for this is not clear, kali-activated blends compared to both single phases. Thus, the re-
but the compressive strength may decrease due to the high shrink- sults of the present study correlate well with these previous
age amount resulting from an increase in the alkali-activator con- results.
tent. Particularly, an increase in the water glass content from The S30 specimen showed compressive strengths of 14.9 MPa
6M0.5 to 6M1.0 resulted in a significant reduction in the compres- and 26.6 MPa at 3 and 7 days, respectively, as shown in Fig. 5b.
sive strength from 37.4 MPa to 26.6 MPa, while an increase in the These values were higher than that of the S20 and the S25 speci-
water glass content from 4M0.5 to 4M1.0 led to a slight increase in mens. However, the compressive strength of the S30 specimen
the compressive strength from 29.9 MPa to 30.7 MPa. It can be said was lower at 14 days (24.1 MPa) than that of the S30 specimen
from these results that high amounts of water glass and NaOH at 7 days, and that of the S30 specimen at 28 days (28.0 MPa)
Table 6
Summary of test results.
Specimens NaOH solution Ratio of water glass to Ratio of slag to (fly Slump Compressive strength (MPa)
molarity (M) NaOH ash + slag) (mm)
3 Days 7 Days 14 Days 28 Days 56 Days
S20-6M0.5 6 0.5 0.2 200 34.6 37.4
(2.51) (4.04)
S20-6M1.0 6 1.0 0.2 250 27.4 26.6
(0.33) (1.48)
S20-4M0.5 4 0.5 0.2 205 29.9 29.9
(0.15) (4.11)
S20-4M1.0 4 1.0 0.2 200 27.5 30.7
(2.06) (1.03)
S10-4M0.5 4 0.5 0.1 220 2.2 (0.87) 10.4 13.1 15.5 18.4
(0.38) (0.52) (1.26) (1.13)
S15-4M0.5 4 0.5 0.15 240 5.7 (0.62) 12.9 19.9 23.0 25.5
(0.06) (0.11) (0.28) (0.25)
S20-4M0.5- 4 0.5 0.2 200 3.4 (0.14) 10.8 27.6 30.6 29.5
H2.25 (0.57) (2.35) (1.49) (0.20)
S25-4M0.5 4 0.5 0.25 160 17.98 27.15 29.15 39.01 40.96
(0.50) (2.60) (2.06) (1.64) (0.20)
S25-4M0.5- 4 0.5 0.25 160 3.8 (0.14) 18.3 24.9 27.8 27.3
H2.25 (1.95) (3.32) (2.67) (2.72)
S30-4M0.5- 4 0.5 0.3 160 14.9 26.6 24.1 28.0 19.8
H2.25 (2.10) (2.82) (0.57) (0.57) (5.20)
Values in parentheses are standard deviations.
1206 N.K. Lee, H.K. Lee / Construction and Building Materials 47 (2013) 1201–1209
Table 7
Measured density and porosity of alkali-activated fly ash/slag mortar and concrete.
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