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A Mix Design Procedure for Alkali Activated Fly

Ash-based Geopolymer Concretes

Conference Paper January 2012

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 2012 International Conference
on
Engineering and Applied Science

July 24-27, 2012, Beijing

Proceedings of the 2012 International Conference on Engineering and Applied Science,

ISSN 2227-0299, ISBN 978-986-87417-1-3
 835
Mix Design Procedure for Alkali Activated Fly Ash-based
Geopolymer Concretes
M Talha Junaid*
School of Engineering and Information Technology
University of New South Wales at the Australian Defence Force Academy, Australia
Obada Kayali
School of Engineering and Information Technology
University of New South Wales at the Australian Defence Force Academy, Australia
Amar Khennane
School of Engineering and Information Technology
University of New South Wales at the Australian Defence Force Academy, Australia
*m.junaid@adfa.edu.au

Abstract
The procedures of selecting mix proportions for Ordinary Portland Cement Concrete (OPC) are well
established and widely accepted by various codes and standards and are performed by the concrete
technologist/practitioner with a high level of confidence. However with the advent of Geopolymer
Concrete (GPC) and its ever increasing usage over the last decade or so, there is a definite requirement
for similar procedures of proportioning a GPC mix design. Such a procedure should be versatile, easy
to follow and repeat, cover a range of strength and workability requirements as well as give the user
control over the proportion of constituents to satisfy cost requirements. This paper presents a formal
step by step procedure for the design of Geopolymer Concrete mixes. The mix design process is
developed for Class F Fly Ash activated using sodium silicates and sodium hydroxide as alkaline
liquids (AL). The paper looks critically at the water to geopolymer solid (W/GPS) and alkaline liquid
to fly ash (AL/FA) ratios as a direct measure of strength and workability. The ratio of alkaline liquid to
water (AL/W) is found to be most closely linked to the strength of GPC mixes. The paper also
illustrates several examples on how to follow the proposed system to achieve a GPC mix design. The
mean strength values as compared to the target strength values of such mixes are also presented.
Keywords: Alkali-activated GPC, mix design procedure, water to geopolymer solid ratio (W/GPS),
alkaline liquid to fly ash ratio (AL/FA), alkaline liquid to water ratio (AL/W)

1. Introduction
Alkali liquids (usually a soluble metal hydro-oxide and/or alkali silicate) can be used to react with
silica (SiO2) and alumina (Al2O3) rich natural materials, like metakaolin or with industrial by-products,
like Fly Ash (FA), Silica Fume, rice husk ash or slag to produce binders[1, 2]. Such binders mixed with
typical coarse and fine aggregates can form concrete, usually known as Geopolymer Concrete, with
mechanical and thermal properties comparable or even superior to ordinary concrete. The term
Geopolymers was coined as the chemical reaction between the aluminosilicates and the alkaline
liquid was a polymerization resulting from a source material of natural or geological origin. Although
other researchers prefer using the term alkali activated FA (AAFA) when FA is used as a source of
139
aluminosilicates, alkali activated slag when slag is the source of aluminusilicates, and so on [3].

1.1 Nature and Characteristics of Geopolymer Concrete

Though details are still debated, many researchers agree that the basic reaction mechanism is in three
stages namely: dissolution of Si and Al from the source material, hydrolysis or gelation, and
condensation forming a 3D network of silico-aluminates also termed as the geopolymer backbone [1,
3-8]. Davdidovits describes geopolymerization as an exothermic reaction and has schematised it using
equation (1.1) given below [4].
GPC does not require any Portland cement as a binder. The role of FA in GPC is entirely different from
that when it is used as a cement replacement material in OPC concrete to enhance certain properties
such as workability or to reduce the heat of hydration [9, 10]. In such cases FA has no pronounced
effect on the strength of concrete [11] especially early strength, however, in GPC Fly Ash is the sole
source of aluminosilicates for reaction with the alkaline solution to form the binder and is thus a critical
factor in strength development. Coarse and fine aggregates make up 75 to 80% of the mass of GPC, as
is the case with OPC concrete.
Though extensive research is being conducted to determine and understand the chemical composition
of GPC and the factors affecting it, the focus is now shifting to probable applications to civil and
infrastructural engineering.
The following two stage chemical equation, represent the development of the geopolymer as suggested
by Davidovits [4] and currently widely accepted:

In addition to numerous engineering benefits, GPC offers economic and environmental advantages
over OPC concrete some of which are discussed in the next section.

1.2 Economic and Environmental Case of GPC

Production of Portland cement, which is the main ingredient of OPC concrete, is not only an
energy-intensive high carbon emitting process resulting in a large carbon footprint [12-14] but it also

140
consumes a significant amount of virgin natural material, thus delivering additional harm to the
environment. In todays era of carbon conscious industry and society, and with a focus on sustainable
development, the concrete industry needs an alternative binder to Portland cement.
The biggest economies in the world depend on coal fuelled power generation for the majority of their
power requirements. This is driven by the low cost and availability of high quality coal. As a
by-product, Fly Ash is produced from the combustion of coal and though efforts are being made to
increase the use of this by-product, supply far exceeds the constructive use of Fly Ash. In Australia it is
estimated that only 11% of the 13 million tonnes of FA produced annually is used in the construction
industry while the rest is either disposed off or used for landfill purposes [15].
GPC also offer motivation on the economical spectrum of the construction industry. The price of Fly
Ash is only a fraction of cement and the resulting GPC, despite the high priced alkaline solutions, is
estimated to be 10- 30% less than that of OPC concretes [2]. Moreover, through schemes like Carbon
Reduction Scheme and Carbon-Credit Trade, additional economic benefits can be gained. Furthermore,
the superior durability of GPC offers an opportunity to substantially lower repair, maintenance and
replacement costs.
Despite the apparent economical and environmental benefits, GPC needs to fulfil its role as an effective
and versatile construction material. As a first step to include GPC in the mainstream of construction
materials, efforts need to be made to standardize design practices. However, there is no widely
accepted procedure for the mix design of such concretes. This is largely due to the fact that the
properties of hardened GPC are heavily dependent of the type and composition of the binder as well as
that of the activator. More recently however, the use of fly ash has been widely accepted as the main
binder in practical GPC applications. GPC made with Class F fly ash has far superior durability
properties, owing to the low amounts of CaO, when compared with Class C fly ash. In addition to
durability issues, GPC made from Class C fly ash tend to set far too quick to be used in any practical
application [5]. Owing to these reasons the focus of this paper is on class F fly ash based alkaline
activated geopolymer concrete systems.

2. Basic Terminology in GPC

Though identified elsewhere in literature, a few basic terms frequently used in GPC technology are
defined here for the sake of completeness:
Water to Geopolymer Solid Ratio (W/GPS)
This is the ratio of the total mass of water in the system, including water in the hydroxide and
silicate solution and any additional free water, to the sum of the mass of fly ash, alkaline hydroxide
and alkaline silicates solids. As these solids contribute to the geopolymerization process they are
termed as geopolymer solids (GPS). The solid and aqueous content of the solutions may be
determined using the concentrations and chemical compositions of the solutions in conjunction with
basic chemistry. It has been proposed that this ratio is analogous to the water to binder ratio in OPC
with similar effects on the GPC mix [16].

141
 Alkaline Liquid to Fly Ash Ratio (AL/FA)
The alkaline hydroxide and alkaline silicates are referred to as the Alkaline Liquids (AL) and the
ratio of their sum by mass to the total mass of fly ash is defined as the AL/FA ratio. Since this is the
direct sum of the alkaline liquids, it is independent of the concentrations and chemical compositions
of the solutions in question. Therefore, this ratio has not been identified in the literature as a
measure of strength but more so of the workability of the mix.
Curing Time and Rest Period
Although GPC can set at ambient temperatures, application of heat to the specimen greatly increases
the compressive strength. It has been found [3, 5, 6, 8] that the temperature of curing as well as the
time plays a significant role in the final strength of GPC mix. However, the start of the heat curing
may be delayed for several days without affecting the properties of GPC. The time lapsed between
the end of casting of GPC and the start of the heat curing is referred to as the rest period. An
increase in the rest period significantly increases the strength of the final product [16].

3. Controlling Ratios in GPC

Unlike OPC where the controlling ratio, as far as strength, workability and to an extent, durability is
concerned, is water/binder ratio: GPC systems are far more complex and depend on a range of ratios
which are at times interlinked. The parameters that have been reported affecting the strength and/or
workability of GPC are W/GPS ratio, AL/FA ratio, curing time and temperature and the ratio of
Silicates to Hydroxides. Though the extent of dependence of the strength of GPC on these ratios
remains a focus of research, it is generally agreed [5, 8, 16,
17] that:
W/GPS has an inverse impact on the strength of GPC
AL/FA has a direct effect on the workability
Strength increases as the time and temperature of curing is increased
Dry curing results in higher strengths when compared to wet curing at similar temperatures
Higher Silicates to Hydroxide ratios result in higher strength, but also increase the unit cost
of the GPC system.
Though these parameters have been identified and their effects on GPC strength and/or workability
have been established, there are no formal procedures which may guide a user to utilize these
parameters towards an optimal mix design. In the following sections, this paper discusses these
parameters and their effect on the mix design of GPC systems.

4. Differences and Similarities of OPC and GPC

The basic difference between OPC and GPC mixes is the binder and its chemistry. OPC attributes its
strength to the hydration of cement which results in, among other compounds, C-S-H and Ca(OH)2.
The strength of the binder largely depends on these two compounds. The skeleton of aggregates, both
fines and coarse, is held together with this binder to give OPC its characteristic strength. Though the

142
function of aggregates in GPC is the same as to that in OPC, the binder in GPC is formed by the
reaction of silica and alumina rich material with alkaline liquids. It is therefore reasonable to
consider/employ the same methods for selection of aggregate proportions in GPC as adopted by several
codes of practice for OPC.
This similarity in the function of aggregates in OPC and GPC systems has led to several researchers
correlating other parameters of the two concretes. In fact, GPC mix design has largely been considered
as an off shoot of OPC mix design procedures [5, 16]. Researchers have related W/GPS ratio of GPC to
strength and workability, much in the same way as W/Binder ratio in OPC. However there has been no
justification to this end. The current research shows that W/GPS ratio cannot be independently
identified as a parameter to denote either the strength or workability of GPC. Similarly, AL/FA ratio
autonomously cannot serve as a measure of strength or workability. This paper explicitly identifies that
these two ratios are interlinked and must both be identified for a mix to determine its strength and
workability characteristics.

5. Material Properties
As is the case with OPC, the material properties of the constituents play a key role in determining the
mix proportions of GPC. Standard material testing methods were used [18-21] in determining the
absorption and moisture content, and specific gravity of fine and coarse aggregates. These are given in
Table 1 along with the sieve analysis of the aggregates in Figure 1.

It must be noted here that changing the aggregate type will affect the strength and workability of GPC
but this change, as discussed in the earlier section, is similar to that of OPC mixes and can be dealt with

143
as in the well established procedures of OPC mix design. Laboratory grade D sodium silicate solution
(Na2SiO3) with SiO2/Na2O between 1.95 and 2.05 was procured from IMCD Australia Limited.
Sodium Hydroxide solutions were made from 98% purity flakes supplied by Redox Pyt Ltd., Australia.

Class-F fly ash obtained from the Eraring Thermal Power Plant supplied by Blue Circle Pvt Ltd. in
Australia was used in all mixes. The chemical composition of the fly ash used as found using the
X-Ray Diffraction (XRD) method is given in Table 2.
Though the results expressed in this research are
obtained from the fly ash composition shown in
Table 2, other fly ash obtained from sources within
Australia have been reported to have a similar
composition [7], especially from the Tarong region.
This would indicate that the use of such fly ash
would give comparable results if used with the
proposed procedure; however, tests need to be
conducted to confirm this.

6. Proposed Sample Preparation

Several mixing procedures were used during the
testing and these procedures as suggested by
different researchers are summarized below:
Method 1: The alkaline liquids were mixed 24
hours prior to casting. Aggregates were dry mixed with fly ash for 2 minutes. The alkaline liquids
along with any additional water and plasticizer were then added and mixed for 3 to 5 minutes.
Method 2: Fly ash was mixed with the hydroxide solution for 2 minutes and then the Silicates
were added and mixed for another 2 minutes. Aggregates were then added to the paste and mixed
for another 3 minutes. Additional water along with any plasticizer were then added and mixed for
2 more minutes.
Method 3: Aggregates were dry mixed with fly ash for 2 minutes. The silicates solution was then
added to the dry mix and mixed for 3 minutes. Hydroxide was then added and mixed for 2 more
minutes. Additional water along with any plasticizer was then added and mixed for additional 2
minutes.
It is worth noting that the mixing process had an insignificant effect on the strength of the GPC.

144
However, the authors suggest the use of Method 3 above as it does not need any pre-preparation and is
very similar to the process generally used for OPC concrete. The following procedure is suggested for
the preparation of the samples of GPC.
After mixing, cast the GPC and compact on a vibrating table for 3-5 minutes depending on the
workability of the mix. Sealed samples should then be placed in a temperature and humidity controlled
room (23oC and 50% RH) for a 24 hours rest period. Heat cure the samples after the rest period at
required temperatures and time to attain target strength. Subsequent to curing, the samples are to be
returned to the temperature and humidity controlled room till the time of testing.

7. Mix Design Procedure

Similar to OPCs mix design procedures, the proposed procedure is based on widely accepted
performance criteria of strength, workability and cost. The overall design process is schematically
illustrated in Figure 2. Initially the designer has to set a target 7 day strength along with the time and
temperature of curing. This paper only presents the design chart for 3 day curing at 80C (Graph G-80-3)
using a NaOH concentration of 16M while other charts are under development and will be presented in
future publications. Using the G-80-3 graph (Figure 3) various combinations of AL/FA with
corresponding W/GPS ratios may be obtained. Keeping in mind the workability requirements and the
achievable workability of the mix as per the workability bands on the chart, a set of AL/FA and W/GPS
ratio is selected. A value of Fly Ash may be assumed here as a starting value. Test results have shown
that for strength requirements between 32 MPa and 40 MPa a fly ash value of 380-400 kg/m3 is
optimum. A fly ash range of 400-420 kg/m3 works best for a strength range of 40-50 MPa, while
strength of 50-60 MPa is constantly achieved for fly ash range of 420-440 kg/m3. It must be noted here
that though these values of fly ash quantities are most favourable in achieving the stated strength
ranges, lower values of fly ash may still result in a reasonably close strength value as demonstrated by
mix T-4-50 in the subsequent section.

145
The silicate to hydroxide ratio has a profound effect on the compressive strength of GPC, and it has
been reported that a value range of 2.3 to 2.8 is appropriate for practical purposes. However using
values close to the upper scale of this range results in uneconomical mixes due to an increased silicate
solution content (the most expensive constituent of GPC mix by far). Values closer to the lower band
of this range result in mixes that do not reach their optimal strength. It is therefore recommended that a
value of 2.5 be used for economically optimised mixes.
Once the values of fly ash, silicates to hydroxides, and molar concentrations of hydroxide have been set,
they can be used in conjunction with the determined value of AL/FA ratio to calculate the quantities of
the hydroxide and silicate solutions. These values in conjunction with W/GPS ratio are then used to
work out the quantity of any additional water that may be required. This can be done using the
chemical composition of the hydroxide and silicate solution to determine the GPS content in the GPC
mix. As the W/GPS and AL/FA ratios are interlinked, changing one will affect the other; e.g., altering
the AL content affects the total water as well as the total GPS. It may therefore be impossible to
achieve the required W/GPS and AL/FA with the calculated values of constituents. The user may use
engineering judgement to slightly alter the constituents to achieve the two ratios.

146
It has been found through experimentation that GPC has a density value of 2300 kg/m3 which is
slightly lower than OPC concrete density. As is the case with OPC concrete, aggregates make up
between 75 to 80% of the mass of GPC while the percentage of fines may be taken as 30% of the total
aggregates. Altering the values and ratios of coarse and fine aggregates has the same impact on GPC as
is well established for OPC mixes. Once the values of all constituents are determined, a final volume
check is performed and fine adjustments can be made. It is recommended that the adjustment only be
done in the quantities of aggregates, as altering the values of FA, alkaline liquid or water may have
significant effect on the strength. A trial mix can now be made to determine the adequacy of the mix.

8. Alkaline Liquid to Total Water Ratio (AL/W)

As has been discussed in the earlier sections, W/GPS and AL/FA ratios are interlinked and cannot be
used independently as a measure of the strength of GPC as for the same value of W/GPS ratio a GPC
mix may have over 40% higher strength when the AL/FA value is changed from 0.35 to 0.50 (Figure 3).
It has been found, however, that the ratio of alkaline liquid to total water in the GPC system (AL/W)
gives a good estimate of the strength of GPC mixes for a wide range of fly ash, AL/FA and W/GPS
ratios as is represented in Figure 4. The relationship could be idealized by a linear correlation with an
R2 value of 0.9433. The AL/W ratio indirectly corresponds to the total alkalinity of the GPC system
and a higher alkalinity results in a higher strength value. These results support the hypothesis presented
by several researchers [5] towards the basic geopolymerization process. It has been reported by these
researchers that C-S-H and C-A-S-H are formed when calcium in the system reacts with the silicates
and aluminates from the source material (fly ash). As the calcium silicate hydrates and calcium

147
aluminates react with water, a water deficiency is generated which results in an increase in the
alkalinity of the system. This increase in alkalinity results in a higher dissolution of aluminates and
silicates from the fly ash resulting in higher strength.

Although at this point the AL/W ratio cannot be used directly in the mix design process of GPC
systems, it can be used as a guide to alter the trial mix proportions (mainly the values of alkaline
liquids and free water) if it falls short of the target strength. It is also a good tool to predict the strength
of a GPC mix with a high level of confidence. Currently research is undergoing to develop similar
relationships for varying curing conditions and hydroxide molar concentrations.

9. Example Mixes Using the Proposed Procedure

An example mix design of GPC is undertaken here so as to illustrate the suggested procedure.
Assuming that the design strength required at 7 day with dry heat curing at 80C for 3 days is 44 MPa.
Using Graph G-80-3 and a strength value of 44 MPa, one can obtain an Alkaline Liquid to Fly Ash
(AL/FA) ratios of 0.375 and 0.425 for Water to Geopolymer Solid (W/GPS) ratio of 0.25 and 0.27
respectively. Proceeding with the lower AL/FA and W/GPS ratio set (whose values are 0.375 and 0.25
for AL/FA and W/GPS respectively) and assuming FA quantity as 400kg/m3 and Na 2SiO3/NaOH ratio
of 2.5 as discussed in the earlier sections, NaOH and Na2SiO3quantities are determined as 42.7 kg/m3
and 107kg/m3 respectively. Keeping the W/GPS ratio constant at 0.25 and using the composition by
weight of NaOH and Na2SiO3 the free water requirements for the mix can be determined as 33.5 kg/m3
for 16M NaOH solution. With the quantities (kg per cubic meter) of Fly Ash,
Alkaline Liquids, and free water established the total aggregate requirements can be found using an
estimate GPC density of 2300kg/m3. The authors have used a combined aggregate weight percent of

148
77% to total weight of GPC. The fine to coarse aggregate percentage is 30 to 70 as commonly used in
OPC concretes. Commercially available super-plasticisers and viscosity modifiers are added as per the
recommended suppliers dosage. If needed the quantities of aggregates are slightly altered to satisfy the
unit volume requirements. The final quantities along with the strength achieved are listed in Table 3
below as mix T-1-44.
An alternative approach would be to initiate the process using the higher values of AL/FA and W/GPS
ratios of 0.425 and 0.27 respectively. A similar procedure to the one described above is followed and
the strength results of mix T-2-44 are given in Table 3 below.
Attempts were made to achieve a target strength of 50 MPa at 7 days using the proposed procedure.
Although, as discussed earlier, a fly ash value of 420 to 440 kg/m3 is recommended for this strength
range, two mixes were made using much lower values of 400 and 380 kg/m3 respectively. Mix
quantities along with achieved strength results of T-2-50 and T-4-50 are summarized below. The
maximum variation of achieved strength to target strength for all trial mixes carried out (those
presented and others) is well within 10%.
It is worth noting here that the workability of the mixes with higher AL/FA ratios is greater than those
with lower values of this ratio even when the W/GPS ratio is unchanged. However, higher AL/FA
ratios result in higher cost of the mix owing to the high price of silicates and is discussed in the next
section.

149
10. Cost of GPC Mixes
It is evident that the cost of GPC mixes is highly dependent on the cost of silicates in the system. In
fact silicates make up to 50% of the cost of the mixes. A comparison between T-1-44 and T-2-44
reveals that increasing the AL/FA ratio from 0.37 to 0.43 (an increase of 0.06) results in an increased
cost of about 10% with no advantage as far as strength is concerned (Table 4). However, other
considerations, such as ease of placement and compaction may dictate the use of one mix over the
other. A similar increase of 0.06 in the AL/FA ratio for T-2-50 and T-4-50 results in a cost increase of
under 6%. This indicates that the effect of silicates on cost is significant at lower ranges of AL/FA
ratios and as the ratios are increased the significance is reduced. It must be noted here that the costs
given are just for comparison purposes and will vary with certain factors. These may include, but are
not limited to, the distance from point of manufacture to point of use, demand of these materials,
and the total quantities required. The initial material cost of GPC may be 25-35% higher than that of
OPC of similar strengths.

11. Conclusion
Though GPC has been used in various applications in the construction industry, and its usage is
growing by the day, there are no formal procedures for carrying out a mix design of such concretes.
Moreover, GPC mix design cannot be handled in the same manner as that of OPC as the binder
chemistry of GPC is entirely different from that of OPC. It is therefore imperative, that the GPC mix
design be looked at with a fresh approach, identifying and including significant parameters as an
integral part of the mix design. A basic formal framework to perform a mix design for geopolymer
concretes is presented along with useful design aids. These design aids (G-Graphs) cater for a wide
range of strength and workability requirements and further work is currently underway to extend this
for a range of OH molar concentrations, curing times and temperatures as well as to include higher
ranges of AL/FA ratios.

150
12. References
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