ACI MATERIALS JOURNAL

TECHNICAL PAPER

Title no. 110-M46

Effect of Plasticizer and Superplasticizer on Rheology of

Fly-Ash-Based Geopolymer Concrete
by Aminul Islam Laskar and Rajan Bhattacharjee
An attempt has been made in this investigation to study the variation of yield stress, plastic viscosity, and slump of fly-ash-based
geopolymer concrete with the variation of lignin-based plasticizer
dosage and polycarboxylic-ether-based superplasticizer dosage. It
has been observed that a critical value of molar strength of sodium
hydroxide exists that is equal to 4 M. Beyond this critical molar
strength, superplasticizer and plasticizer have an adverse effect on
yield stress, plastic viscosity, and slump of fly-ash-based geopolymer
concrete. Below the critical molar strength of sodium hydroxide,
there is a decrease in both the rheological parameters and an
increase in slump. Lignin-based first-generation plasticizer shows
better performance in terms of workability over third-generation
superplasticizer below the critical value of molar strength. It was
also observed that there is a good correlation between the rheological parameters and slump for fly-ash-based geopolymer concrete
incorporating plasticizer andsuperplasticizer.
Keywords: geopolymer concrete; plastic viscosity; rheology; superplasticizer; thixotropy; yield stress.

INTRODUCTION
Single-point workability tests such as the slump test, Vebe
test, and compaction factor test are widely used test methods
to assess the workability of fresh concrete. The majority of
these test methods are empirical in nature and they measure
distance or time that serves as an index of workability.
These tests do not provide any information about fundamental properties of fresh concrete rheology. Tests such as
the slump, compacting factor, and Vebe test are empirical
in nature and these tests cannot characterize workability of
todays advanced concrete mixtures.1,2 Researchers3-5 treat
fresh concrete as a concentrated suspension of aggregates in
cement mortar; therefore, fluid rheology methods are used to
describe fresh concrete behavior. Rheology is defined as the
science of flow and deformation of matter. Fluid rheology
is a useful tool that is used by researchers to characterize
and describe various fresh concrete properties such as
workability loss, stability, compactibility, and pumpability.
Rheological parameters are used to understand the interactions among the ingredients in concrete.
It has been established that cement concrete as a fluid
can be assumed to behave like a Bingham fluid with a good
accuracy.1,2 In the Bingham Model, flow is described by
two parameters: yield stress and plastic viscosity. Yield
stress and plastic viscosity are considered to be fundamental
parameters of fresh concrete rheology. Yield stress gives
initial resistance to flow and plastic viscosity governs the
flow after it is initiated. The Bingham Model is represented
by the following equation

= 0 + 

ACI Materials Journal/September-October 2013

(1)

where t is the shear stress; t0 is the yield stress constant; m is

the plastic viscosity; and g is shear strain rate.
Geopolymer concrete is a promising field of research
because it uses industrial waste and by-products. Fly-ashbased geopolymer concrete contains alkali-activated fly
ash as binder. Fly ash is readily dissolved in the alkaline solution and lends itself to geopolymerization. In
geopolymer concrete, polymerization takes place yielding
Si-O-Al bonds as follows
Mn[(SiO2)zAlO]n wH2O
where Mn is the alkaline element; the symbol indicates
the presence of a bond; z is 1, 2, or 3; and n is the degree
of polymerization.6-11 The end product is an amorphous
polymer. The alkali activation of fly ash and other mineral
admixtures is a complex chemical process involving dissolution of raw materials, transportation or orientation,
and polycondensation of the reaction products. Fly-ashbased geopolymer concrete has shown its superior durability over ordinary portland-cement concrete. The alkali
activators normally used in geopolymer concrete are either a
mixture of sodium hydroxide and sodium silicate or a mixture of
potassium hydroxide and potassium silicate.6-8,12 Zhang,9 Khale
and Chaudhary,10 and Duxson et al.11 presented a review on
geopolymer and summarized previous research on geopolymer.
There has been extensive research on geopolymer concrete
for strength and durability in recent years and several
researchers highlighted the potential use of fly-ash-based
geopolymer concrete in the concrete industry. Published
literature on fly-ash-based geopolymer concrete for conventional single-point workability tests is also available. A
review of the literature shows that no attempt has been made
so far to investigate the effect of mixture parameters and
superplasticizer dosage on rheological parameters of fly-ashbased geopolymer concrete. However, there are few reports
available on rheological behavior of geopolymer paste and
geopolymer mortar. Palacios et al.13 conducted rheological
tests for slag-based geopolymer mortar and concluded that
slag paste and mortar followed the Bingham Model when
NaOH was used as an activator. Criado et al.14 studied rheological behavior of fly-ash-based geopolymer paste with
NaOH as an activator and observed that the Bingham Model
could be fitted to those pastes. It is only recently that Laskar
ACI Materials Journal, V. 110, No. 5, September-October 2013.
MS No. M-2011-389.R2 received July 17, 2012, and reviewed under Institute
publication policies. Copyright 2013, American Concrete Institute. All rights
reserved, including the making of copies unless permission is obtained from the
copyright proprietors. Pertinent discussion including authors closure, if any, will be
published in the July-August 2014 ACI Materials Journal if the discussion is received
by April 1, 2014.

513

Aminul Islam Laskar is a Professor in the Department of Civil Engineering, National

Institute of Technology, Silchar, India. He received his BE (Civil) from the National
Institute of Technology, Silchar; his MTech from the Indian Institute of Technology, New
Delhi, India; and his PhD from the Indian Institute of Technology, Guwahati, India. His
research interests include high-performance concrete and geopolymer concrete.
Rajan Bhattacharjee is a Research Scholar in the Department of Civil Engineering,
National Institute of Technology, Silchar. He received his BE (Civil) from Jorhat
Government Engineering College, Assam, India; and his MTech from the National
Institute of Technology, Silchar.

and Bhattacharjee15 reported that fly-ash-based geopolymer

concrete behaves like a Bingham fluid with good accuracy.
An attempt has therefore been made in this paper to study
the effect of several mixture parameters as well as plasticizer
and superplasticizer dosage on the rheological parameters of
fly-ash-based geopolymer concrete.
RESEARCH SIGNIFICANCE
Rheological behavior of fly-ash-based geopolymer
concrete incorporating plasticizers and superplasticizers
has never been reported and needs to be explored. This
study reveals the effect of plasticizer/superplasticizer
after interacting with alkaline solutions on yield stress and
plastic viscosity of fly-ash-based geopolymer concrete. The
outcome of this investigation is new and will be very useful
for a better understanding of the behavior of the material
during the production stage.
EXPERIMENTAL INVESTIGATION
Mixture proportions
Two geopolymer mixtures were prepared with different
mixture proportions with Class F fly ash, sand, and coarse
aggregates. The mixture proportions and designations are
listed in Table 1. In Table 1, M represents molar strength
of NaOH, and R is the ratio of the weight of sodium silicate
solution to the weight of the sodium hydroxide solution.
Fine aggregate
Locally available river sand (water absorption = 1.5%;
moisture content = 0.5%; specific gravity = 2.6) was used in
this work. Sieve analysis, specific gravity, moisture content,
and water absorption were determined as per Indian Standard Code IS 2386.16 The particle size distribution is shown
in Table 2.
Coarse aggregate
Graded crushed stone aggregate (water absorption = 0.9%;
moisture content = 0.25%; specific gravity = 2.6) of 16 mm
(0.624 in.) maximum size was collected and stored in the
laboratory. The physical properties were determined as per
the code stated previously. The particle size distribution is
presented in Table 2. Aggregates were not sieved and were
used as received directly from the stockpile.
Fly ash
Class F fly ash (specific gravity = 2.10) collected by electrostatic precipitator, obtained from Farakka, India, was used

in this study. The specifications of the fly ash conform to the

Indian Standard Code of Practice IS 3812.17 The chemical
composition of fly ash is presented in Table 3.
Alkaline activators
In geopolymer concrete, either a mixed solution of sodium
hydroxide and sodium silicate or a mixed solution of potassium hydroxide and potassium silicate is commonly used.
A mixed solution of sodium hydroxide and sodium silicate
was chosen in this study as alkali activators. Sodium-based
solutions were chosen because they were less expensive
and because it was reported that NaOH possesses a greater
capacity to liberate silicate and aluminate monomers.11 It is
also reported that sodium cations have better zeolitization
capabilities in geopolymer forming systems.11 The commercialgrade sodium hydroxide in pellets (purity = 97%; specific
gravity = 2.13) and sodium silicate solution (Na2O = 18.2%;
SiO2 = 36.7%; water = 45.1%; specific gravity = 1.53) were
used to prepare the solution. The mass of NaOH pellets in a
solution varied according to molar strength M and the mass
of silicate solution was taken according to the ratio R.
Water-reducing admixtures
To study the effect of water-reducing admixtures (WRAs)
on rheological parameters, two types of chemical admixturesnamely, first-generation lignin-based water reducer
(lignin) and third-generation polycarboxylic-ether-based
high-range water reducer (PC) were used. The water reducers
dosage used in this study is the weight of water reducer
expressed as a percentage of fly ash content.
Mixing
Concrete was mixed in a tilting mixer (laboratory type).
The weight of the materials was taken with a digital weighing
balance. The mixing sequence was as follows:
1. Requisite quantity of sodium hydroxide and sodium
silicate solution was prepared 24 hours in advance.
2. Solutions of sodium hydroxide and sodium silicate
solution was mixed on the day of casting.
3. Coarse aggregate, fine aggregate, and fly ash was mixed
for 2 minutes in a tilting mixer.
4. Alkaline solutions and WRA were added during mixing
and mixed for two more minutes.
5. Mixing was stopped and the concrete mixture
waspoured.
Mixing and testing of geopolymer concrete mixtures were
performed at approximately 20 to 22C (68 to 72F).
Rheological measurements
The rheological measurements were performed with a
rate-controlled concrete rheometer developed at the National
Institute of Technology, Silchar, India. The details of the rheometer, such as conceptual design, actual design, calibration,
and validation, are published elsewhere.18 Figure 1 shows
the schematic diagram of the rheometer.
The prepared concrete was transferred to the cylindrical
container with a trowel from the same height every time.

Table 1Mixture designation and mixture proportions, kg/m3 (lb/yd3)

Mixture No.

Fly ash

Sand

Coarse aggregate

NaOH solution

Na2OSiO2 solution

Molar strength

546 (906)

598 (993)

864 (1434)

300.2 (498)

68.4 (113.5)

2.5 M

0.23

200 (8)

546 (906)

598 (993)

864 (1434)

328.5 (498)

39.4 (113.5)

6.3 M

0.12

140 (5.6)

514

Slump, mm (in.)

ACI Materials Journal/September-October 2013

Table 2Sieve analysis of aggregates

Percent by mass passing
Sieve size, mm (in.)

Fine aggregate

Coarse aggregate

16 (0.624)

100

12.5 (0.50)

42.20

10 (0.393)

31.80

6.3 (0.246)

25.0

4.75 (0.185)

98.2

0.9

2.36 (0.0937)

96.5

1.70 (0.0663)

94.6

1.18 (0.0469)

91.2

0.60 (0.0234)

66.3

0.30 (0.0117)

20.3

0.15 (0.0059)

1.6

Fig. 1Schematic diagram of rheometer used in this study.

Table 3Chemical composition of fly ash
Particulars

Composition, %

SiO2

57

Al2O3

27.1

Fe2O3

5.4

CaO

6.1

MgO

2.0

K 2O

0.6

SO3

1.4

Loss on ignition

0.8

The rheological test was carried out after exactly 15 minutes

from the instant of the addition of the alkaline solution. Every
time, a new batch of concrete with the desired composition
for a particular mixture was prepared. The mixing sequence
and the time at which the rheological test was performed
were identical for each batch and for all mixtures.
Over the years, it was established by many workers that the
down-curve of the torque-speed plot follows the Bingham
model in the case of cement-based materials such as cement
paste, cement mortar, and cement concrete. Recently, Laskar
and Bhattacharjee15 observed that thixotropy is also present
in fly-ash-based geopolymer concrete. Thixotropy will lead
to erroneous test results in terms of yield stress and plastic
viscosity if it is not properly taken care of. Mewis19 used the
term thixotropy to describe an isothermal gel-sol transition due to mechanical agitation. Barnes et al.20 has given a
comprehensive review of the topic and described thixotropy
as a decrease of the apparent viscosity under constant shear
stress or shear rate, followed by a gradual recovery when
stress or shear rate is removed. Thixotropy is governed by a
combination of reversible coagulation, dispersion, and then
recoagulation of cement particles.21 Researchers suggested
several approaches to investigate and measure thixotropy.
The simplest approach mentioned by Mewis19 is to measure
torque under a linear increase and then a decrease in rotational frequency. The hysteresis loop, if obtained, indicates the presence of thixotropy, although the loops do not
provide a good basis for quantitative treatment. For cementbased materials, a stepwise increasing shear rate sequence
ACI Materials Journal/September-October 2013

followed by a stepwise decreasing shear rate sequence is

used to investigate the presence of thixotropy, if any, for
concrete mixtures.22 In this study, a stepwise increasing
shear rate sequence and then decreasing shear rate sequence
was used for every mixture for rheological measurements.
The down-curve was used to estimate Bingham parameters. To minimize the danger for particle migration, the
maximum rotational frequency was taken as 40 rpm in this
study for all the observations.
In addition to the rheological test, a slump test was also
carried out as per Indian Standard Code of Practice IS 7320.23 A
slump cone was filled with concrete in three layers. Each
layer was tamped 25 times with a standard 16 mm (0.624 in.)
diameter steel rod and the top was struck off by means of a
screeding and rolling motion of a tamping rod. Immediately
after filling, the cone was lifted vertically and the decrease
in the height of the center of the concrete was measured
as slump.
EXPERIMENTAL RESULTS AND DISCUSSION
The dosage of plasticizer/superplasticizer affecting yield
strength and plastic viscosity of fly-ash-based geopolymer
concrete, the effectiveness of plasticizer/superplasticizer at
different molar strengths, and the correlation between slump
and rheological parameters have been studied and presented
in the subsequent paragraphs.
Figure 2 presents the variation of slump with the variation
of WRA dosage for Mixture 1. It can be observed that there
is an appreciable increase in slump incorporating both the
admixturesnamely, lignin and PC. The admixtures seem
to serve their plasticizing effect by dispersing the particles
apart, which in turn improves workability by releasing water
trapped in the flocs. It may also be observed that the improvement of workability in this study is greater with ligninbased water reducer (first-generation plasticizer) than with
PC-based admixture (third-generation superplasticizer). At
a lignin dosage of 1.5% and above, there was segregation
of the mixture; the particles constituting the paste separated,
forming a dense lower phase and a creamy upper phase. The
variation of workability in this study contradicts the works
reported by Criado et al.,14 Bakharev et al.,24 and Douglas
and Brandstetr.25 It should be mentioned that Criado et
al.14 observed improvement in flow value for fly-ash-based
515

Fig. 2Variation of slump with water-reducer dosage

(Mixture 1).

Fig. 3Variation of yield stress with water-reducer dosage

(Mixture 1).

Fig. 4Variation of plastic viscosity with water-reducer

dosage (Mixture 1).
geopolymer mortar incorporating PC but observed a decrease
in flow value using lignin-based chemical admixture.
Bakharev et al.24 and Douglas and Brandstetr25 concluded
that presence of a naphthalene-based admixture (secondgeneration superplasticizer) did not improve alkaline system
workability. Criado at el.14 also observed that the addition of
lignin resulted in segregation of fly-ash-based geopolymer
516

Fig. 5Effect of superplasticizer/plasticizer type and

dosage on thixotropy (Mixture 1).
mortar. Palacios and Puertas26 studied the chemical stability
of different types of superplasticizers (melamines, naphthalenes, vinyl copolymers, and polycarboxylates) in highly
alkaline media and concluded that all (except the naphthalenebased admixture) in an NaOH environment were chemically
unstable at pH > 13. At such high values, polycarboxylate-based
admixtures underwent alkaline hydrolysis that altered their structure and consequently their dispersing and fluidizing properties.
The variations of yield stress and plastic viscosity of
Mixture 1 with the WRA dosages are presented in Fig. 3 and
4, respectively. It can be observed that both the rheological
parameters decrease with the increase in WRA dosage, and
the decrease is greater in mixtures with lignin. The admixtures were able to make the mixtures more fluid; therefore,
less yield stress and plastic viscosity were obtained compared
to the control mixture. The admixtures served their purpose
by dispersing the particles apart; subsequently, smaller
forces (compared to the control mixture) were required to
initiate flow and, hence, the mixture had lower yield stress.
Criado et al.14 observed similar variation of yield stress and
plastic viscosity of fly-ash-based geopolymer mortar incorporating PC- and lignin-based admixtures.
To study the effect of WRAs on the thixotropy of
geopolymer concrete, the up- and down-curves of mixtures
are plotted as shown in Fig. 5. It can be observed that upand down-curves of all the mixtures, including the control
mixture (Mixture 1), form thixotropic loops. It is also can be
observed from Fig. 5 that the area under the loop (although
this is not a very good method to estimate thixotropy), and
hence the degree of thixotropy, continuously decreases with
the increase in PC dosage. The degree of thixotropy is the
least for the mixture with lignin. The admixtures in this
study are able to prevent the formation of flocs to an extent,
depending on the dosage of the admixtures. The reason for
the least degree of thixotropy with lignin is unknown at the
moment and needs further study.
The variation of slump with the variation of plasticizer/
superplasticizer dosage for Mixture 2 is presented in Fig. 6.
It may be observed that there is a tremendous decrease in
slump after the addition of plasticizer/superplasticizer,
which is just opposite to that shown in Fig. 2. As before,
lignin-based plasticizer shows better performance compared
to third-generation PC superplasticizer. The probable
reason for the decrease in slump may be a higher molar
concentration of NaOH solution compared to Mixture 1,
although the exact reason is to be investigated further. The
ACI Materials Journal/September-October 2013

slump values at different water-reducer dosage were very

low after the addition of chemical admixtures, and the rheological tests were not conducted for Mixture 2.
To investigate the probable effect of molar strength of
NaOH solution on the effectiveness of plasticizer/superplasticizer, Mixture 2 was chosen as the reference mixture.
A slump test was carried out for mixtures by changing the
molar strength of NaOH for Mixture 2. The results are
shown in Fig. 7. It may be observed that at 4 M concentration, the effect of the addition of superplasticizer/plasticizer is negligible. Mixtures containing NaOH solutions
with molar strength above 4 M show a decrease in slump,
whereas there is an increase in workability for all mixtures
with chemical admixtures at molar strengths less than 4 M.
It may also be observed from Fig. 7 that the performance
of lignin-based plasticizer is still better compared to thirdgeneration superplasticizer at all molar strengths of NaOH
solution, except 1.5 M.
The behavior of fly-ash-based geopolymer concretes
using lignin-based plasticizer and PC-based superplasticizer are contradictory to the OPC system incorporating
these admixtures. In the OPC system, PC is much more
effective compared to lignin-based admixture. It is to be
remembered that these admixtures are proven suitable for
the OPC system and established theories are available for
their mode of action. The hydration reaction mechanism
of OPC and the alkali activation reaction mechanism are
completely different; the hydration product of OPC and
reaction product of fly-ash-based geopolymer concrete are
also different. Water reducers, including PC, are designed to
form complexes with the dissolved Ca2+ formed during early
phases of OPC hydration.27 In the case of a fly ash system,
there are no dissolved Ca2+ ions. Therefore, the mode of
action by which slump increases or decreases is difficult to
explain within the context of this study and needs further
investigation. For the same reason, it is not clear why lignin
imparts better workability than PC admixtures.
The segregation of fly-ash-based geopolymer concrete
after the addition of lignin also needs further study. In a study
of activated slag systems, Palacios and Puertas26,28 reported
changes in infrared spectra of a naphthalene-based admixture when stored in a mixed solution of sodium hydroxide
and sodium silicate. The changes in spectra were attributed
to certain changes in sulfonates responsible for a plasticizing
effect. Lignin-based admixture might have experienced
similar alterations in this study, and concrete containing
lignin suffered from segregation.
Correlation between slump and rheological parameters
such as yield stress and plastic viscosity determined by the
present rheometer has been studied. Immediately after the
rheological test for each sample, concrete was transferred to
the mixer. Leftover concrete in the cylindrical container was
cleaned manually so that all the mortar is taken out. Concrete
was mixed again for 2 minutes and transferred for subsequent
testing. A slump test was performed after 30 minutes from
the addition of water. It should be noted that that similar
procedure was adopted by Wallevik.21 Moreover, it has
already been demonstrated that there is no significant change
in the workability of fly-ash-based geopolymer concrete for
a longer period because there is hardly any geopolymerization at a room temperature of approximately 20C (68F).
The variation of yield stress and plastic viscosity of
Mixture 1 with various plasticizer/superplasticizer dosages
with the variation of slump are shown in Fig. 8. It can be
ACI Materials Journal/September-October 2013

Fig. 6Variation of slump with water-reducer dosage

(Mixture 2) at 6.3 M.

Fig. 7Effectiveness of plasticizer/superplasticizer with

variation of molar strength of NaOH solution (Mixture 2).

Fig. 8Correlation between slump and rheological parameters (Mixture 1). (Note: 1 Pa = 0.0201 lb/ft2; 1 Pa.s =
0.0201 lb.s/ft2.)
observed that there is a good correlation between slump
and yield stress, and slump and plastic viscosity. As slump
increases, yield stress and plastic viscosity of concrete with
plasticizer/superplasticizer decreases. It should be mentioned
in this connection that Wallevik,21 Laskar,29 and other
517

researchers observed that for cement-based concrete, there

is a good correlation between yield stress and slump, and
plastic viscosity and slump. For fly-ash-based geopolymer
mortar, however, Criado et al.14 reported that no correlation
exists between slump and rheological parameters of fly-ashbased geopolymer mortar incorporating lignin-based plasticizer and PC-based superplasticizer.
CONCLUSIONS
The following conclusions may be derived from this study:
1. Plasticizer and superplasticizer dosage improves workability (measured by slump test) of fly-ash-based geopolymer
concrete for a molar strength of a NaOH solution less
than 4 M. As the dose of water reducer increases, there is a
decrease in the value of rheological parameters. First-generation lignin-based water reducer has been found to be more
effective than third-generation PC-based superplasticizer for
mixtures having a molar strength greater than 4 M. However,
segregation of concrete takes place with the addition of
lignin-based water reducer at 1.5% and above.
2. The degree of thixotropy, assessed by area under a
torque-speed curve, decreases as WRA dosage increases
and the thixotropy is the least with lignin-based WRA. This
is observed for molar strength of an NaOH solution less
than 4 M.
3. At a higher molar concentration of NaOH (more
than 4 M), plasticizer/superplasticizer dosage has an
adverse effect on slump and the rheological parameters of
fly-ash-based geopolymer concrete. Lignin-based plasticizer still shows better performance, as measured by the
slump test, than PC-based superplasticizer at higher molar
concentrations.
4. The correlation between rheological parameters and
slump test results has been found to be good for fly-ashbased geopolymer concrete containing plasticizer and
superplasticizer.
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ACI Materials Journal/September-October 2013