CE Yu - Aaron Lok - Wai - Yu - Aaron - Final - 3437285 - 265807687

UCL DEPARTMENT OF CIVIL, ENVIRONMENTAL &
GEOMATIC ENGINEERING
MSc DISSERTATION SUBMISSION
Student Name: ____________LOK WAI YU AARON_________ (BLOCK CAPITALS)
Programme: ___________MSc Civil Engineering______________ (e.g. MSc GIS)
Supervisor: ___________Dr. Mingzhong Zhang__________________
Dissertation Title:
Internal Curing of Cement Free Geopolymer Mortar Using Superabsorbent Polymer
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Signature: Lok Wai Yu Aaron Date: 12th September 2018

Lok Wai Yu Aaron CEGEG 099 MSc Project Student No. 13055984
Internal Curing of Cement Free Geopolymer Mortar Using

Superabsorbent Polymer
By
Lok Wai Yu Aaron
Student No. 13055984
Supervisor:
Dr. Mingzhong Zhang
Submitted in partial fulfilment of requirement for the Degree of Master of

Science in Civil Engineering
Department of Civil, Environmental and Geomatic Engineering
University College London (UCL)
12th September 2018
1
ABSTRACT
Alkali-activated fly ash/slag (AAFS) system is an exciting alternative of ordinary Portland cement
(OPC) that has gained increasing attention in recent years because of its environmentally friendliness
and decent engineering properties. However, the major problem associated with AAFS is its
shrinkage problems. This paper aims to investigate the potential of including internal curing into
AAFS mortar to mitigate its limitation on shrinkages. A series of experiments were carried out to
determine workability, setting time, density, compressive strength, internal relative humidity (IRH),
drying shrinkage and autogenous shrinkage of AAFS mortar. Alkaline activator to binder ratio (AL/B)
of 0.4, molarity of sodium hydroxide solution (SH) of 10M, sodium silicate to sodium hydroxide ratio
(SS/SH) of 2.0 were selected to design and prepare the mixes. Superabsorbent polymer (SAP) content
of 0%, 0.2%, 0.3%, 0.4% and 0.5%, together with four fly ash (FA) to ground granulated blast-
furnace slag (GGBS) (i.e. FA/BBGS) ratio of 85/15, 80/20 ,75/25 and 70/30, were selected as variable
to investigate the effect of SAP and slag on the engineering properties of AAFS.
The results showed that both SAP content and FA/GGBS ratio brought significant influence on the
properties of AAFS mortar. Workability and setting time increased with the rise of SAP content and
the reduction in slag replacement level. The ultrasonic pulse velocity (UPV) of specimens correlates
well with the strength development of AAFS mortars. It illustrates that the structure of the specimens
was kept developing and the density gradually improved during curing ages, which is similar to
observations made on conventional concrete.
The compressive strength of AAFS mortars decreased with the addition of SAP as well as the
decrease of slag replacement level. It was observed that the addition of SAP and slag also have a
strong influence in the strength development of AAFS mortar. Besides, the IRH increased with the
rise of SAP content, but declined with the increase of slag replacement level. The autogenous and
drying shrinkage declined with the addition of SAP, but increased with the rise of slag replacement
level. It was revealed that shrinkage of the mixture is closely related to its IRH, chemical reactions
2
and pore structure, and the improvement of IRH could well explain how SAP mitigates shrinkages.
The results proved that although the addition of GGBS could lead to the drawbacks on fresh
properties and shrinkages, it has a crucial role in improving the mechanical properties of AAFS.
Meanwhile, a series of results also show that internal curing could solve the corresponding issues
from the addition of GGBS in AAFS. However, a good balance has to be made between the
proportions of SAP, FA and GGBS, in order to have a mixture that has decent engineering properties
with less shrinkages.
3
ACKNOWLEDGEMENTS
I would like to express sincere appreciation to my project supervisor, Dr Mingzhong Zheng,
Department of Civil, Environmental and Geomatic Engineering, University College London (UCL).
Dr Mingzhong Zheng has been very supportive throughout my project. He has given a lot of guidance
and valuable opinions in facilitating my critical thinking which helps to overcome different challenges
and obstacles throughout my research.
I am truly grateful to Dr Mingzhong Zheng for all his effort and comprehensive advice on my project.
Thank you Dr Mingzhong Zheng for giving me the opportunity to work on a topic which I am
fascinated in. It is a great honour to work under his supervision.
Furthermore, most profound gratitude is expressed to Wenlin Tu who assist me throughout the
research. She is one of the key persons who made this research possible and proceeds smoothly.
Wenlin Tu has taken her precious time in providing with a lot of valuable information and assistance
despite her tight schedule. Miss Tu is always willing to solve my queries with patience, her feedback
and advice are influential throughout the project.
Moreover, I would like to appreciate every member of staff in the laboratories who provided me
guidance for the experimental works. Their cooperation and patience are one of the most crucial
factors which allow me to obtain decent experimental data and to produce this research paper.
Appreciation is also given to all the researchers and experts who spent a considerable amount of effort
on topics related to geo-polymer concrete and internal curing. Their effort has created a
comprehensive database to allow people to explore even further on the related field. Their
contribution has significantly facilitated the development of geo-polymer concrete for the benefit of
future generations.
4
TABLE OF CONTENT
ABSTRACT …………………………………………………………………………………...………2
ACKNOWLEGEMENTS ……………………………………………..…………………..…………4
TABLE OF CONTENT …………………………………………………….…………...……………5
ABBREVIATIONS ……………………………………………………………………...……………7
LIST OF FIGURES ……………………………………………………...…………...………………8
LIST OF TABLES ………………………………………………………..................………………10
1. INTRODUCTION ………………………………………………………...…..……………11
1.1. Background ………………….………………….……………………......………….11

1.2. Research Novelty ………………….………………….……………...…..………….14
1.3. Research Strategies ………………….………………….……………...…...……….14
1.4. Objectives of the Study ………………….………………….…………….…………16
1.5. Outline of the Study ………………….………………….…………...…..………….17
2. LITERATURE REVIEW…………………………………………………..………………17
2.1. Alkali-Activated (AA) Materials ………………….………………..………...….….17

2.2. Concern Over Alkali-Activated Fly Ash/Slag (AAFS) System ……………..……...18
2.3. Shrinkages ………………….………………….…………………………...….…….20
2.3.1. Plastic Shrinkage ………………….……………………………….....…….21
2.3.2. Chemical Shrinkage ………………….……………..…………………...….21
2.3.3. Autogenous Shrinkage ………………….………..………………...……….21
2.3.4. Drying Shrinkage ……….………………………..….……………...………22
2.4. Internal Curing ………………….………………….…..……………………...…….23
2.4.1. General Benefits of Internal Curing ………...……………………...………24
2.5. Different Internal Curing Agents …………………...….……………………...…….25
2.5.1. Superabsorbent Polymers (SAPs) ………………….……….................……25
2.5.1.1. Mechanism and Effectiveness of Superabsorbent Polymers ……...28
2.6. Selection of Internal Curing Agent ………………….…………………….……….29
2.7. Saturation of Fine Aggregate ………………….……………….…………....………30
2.8. Summary of Literature Review ………………….………………………..…..…….31
3. EXPERIMENTS ……………………………………………………………………………32
3.1. Materials ………………….………………….………………………..…………….32
5
3.2. Mix Proportions ………………….………………….……………………...……….35

3.3. Specimens Preparation ………………….………………………………...……...….37
3.4. Testing Methods ………………….…………………….………………..………….39
3.4.1. Fresh Properties ………………….……………………………...………….39
3.4.1.1. Workability ………………….…………..…………...…………….39
3.4.1.2. Setting Time ………………….………….…………..…….………40
3.4.2. Physical Properties ………………….……………………..……………….41
3.4.2.1. Ultrasonic Pulse Velocity (UPV) ……..……………..….…………41
3.4.3. Mechanical Properties ………………….………………...……..………….42
3.4.3.1. Compressive Strength …………………………......……………….42
3.4.4. Shrinkages ………………….………………………..….….………………43
3.4.4.1. Autogenous Shrinkage …………………………....….…………….43
3.4.4.2. Drying Shrinkage ………………….………………...…….……….44
3.4.5. Internal Relative Humidity (IRH) ………………………………..…………45
4. DISCUSSION AND RESULTS …………………………………………...….……………46
4.1. Workability ………………….………………….…………………...………...…….46

4.2. Setting Time ………………….………………….…………...……………..……….48
4.3. Ultrasonic Pulse Velocity (UPV) ………………………………………...………….54
4.4. Compressive Strength ………………….……………….......……….………………56
4.5. Autogenous shrinkage ………………….………………………..………………….60
4.6. Drying Shrinkage ………………….…………………...…………...……………….63
4.7. Internal Relative Humidity (IRH) ………………….…………….....……………….67
4.8. Relationship Between Autogenous Shrinkage, Pore Structure and IRH .…………...69
5. CONCLUSIONS …………………………………………………………………...….……70
5.1. Concluding Remarks ………………….…………………...…………..……………70

5.2. Future Work ………………….………………….……………………...……..…….72
5.3. Prospectus ………………….………………….……………………...…….……….72
6. REFERENCES …………………………………………………………...…………………73
7. APPENDICES …………………………………………………………...….………………87
7.1. Appendix A – Example of Mix Proportion Calculation – M1………………..…..…87
6
ABBREVIATIONS
Name
A-S-H Amorphous aluminosilicate gel
AA Alkali Activated
AL Alkaline activator
AL/B Alkaline activator to binder ratio
AAC Alkali-activated concrete
AAF Alkali-activated fly ash
AAFS Alkali-activated fly ash/ slag
AAS Alkali-activated slag
ASTM American Society for Testing and Materials
CaCO3 Calcium carbonate
CaO Calcium oxide
CO2 Carbon dioxide
C-S-H Calcium silicate hydrate gel
FA Fly ash
FRC Fibre reinforced composite
GGBS Ground granulated blast-furnace slag
IRH Internal relative humidity
LA Lightweight aggregate
LCA Life cycle analysis
LVDT Linear variable differential transformer
MIP Mercury Intrusion Porosimetry
Na2SiO3 Sodium silicate (water glass)
NaOH Sodium hydroxide powder
NWA Normal weight aggregate
OPC Ordinary Portland cement
PWLA Pre-wetted lightweight aggregate
SAP Superabsorbent polymer
SEM Scanning Electron Microscopy
SH Sodium hydroxide solution
SS Sodium silicate solution
SSD Saturated surface-dry
S/B Sand to binder ratio
UPV Ultrasonic pulse velocity
7
LIST OF FIGURES
Title
Figure 1 Fly Ash (FA) (Source: Lizmar, 2016) [70]
Ground Granulated Blast-furnace Slag (GGBS) (Source:

Figure 2
Ecocem, 2018) [37]
Five aspects of investigation of AAFS mortars involved in

Figure 3
the present study
Figure 4 Tests involved in the present study
Visual illustration of external curing (conventional Curing)

Figure 5 compared with internal curing (Source: Bentz and Weiss,
2011) [15]
Figure 6 Microstructure of SAPs
SAP particles in dry condition (left) and after absorption of

Figure 7
water (right) (Source: Schwarz, 2005) [95]
Four aggregate moisture conditions (Source: NRRMCA,

Figure 8
2018) [83]
Figure 9 Selected FA
Figure 10 Selected GGBS
Figure 11 Particle size distribution of FA, GGBS and SAP
Figure 12 Selected SP
Figure 13 Selected fine aggregate
Figure 14 Microstructure of SAPs (Source: Tu and Zhu, 2018) [108]
Figure 15 Selected SAPs
Figure 16 Mixing procedures of AAFS mortars with SAP
Figure 17 Mixing procedures of AAFS mortars without SAP
Figure 18 Medium size mixer used in the present study (Capacity 10L)
Figure 19 Small size mixer used in the present study (Capacity 1.5L)
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Figure 20 Flow table used in the present study
Figure 21 Vicat setting test apparatus
Figure 22 UPV test apparatus
Figure 23 Machine for compression test
Visual presentation of laser displacement method (Source:

Figure 24
Fang et al, 2018) [39]
Figure 25 Mould for laser displacement method
Figure 26 Laser displacement method setup
Figure 27 Length comparator
Visual presentation of IRH measurement setup (Source:

Figure 28
Fang et al. 2018) [39]
Figure 29 IRH setup sample
Figure 30 Flow value of AAFS mortars with different SAP content
Figure 31 Flow value of AAFS mortars with different slag content
Figure 32 Setting time of AAFS with different SAP content
Figure 33 Setting time of AAFS mortars with different slag content
Heat evolution of AAFS pastes with different SAP content

Figure 34
(Source: Tu and Zhu, 2018) [108]
Chemical shrinkage of AAFS pastes with different SAP

Figure 35
content (Source: Tu and Zhu, 2018) [108]
Heat evolution of AAFS pastes with different slag content

Figure 36
Chemical shrinkage of AAFS pastes with differrent slag

Figure 37
content (Source: Tu and Zhu, 2018) [108]
Relationship between compressive strength and UPV for all

Figure 38
AAFS mortars
Compressive strength of AAFS mortars with differernt SAP

Figure 39
content
Compressive strength development of AAFS mortars with

Figure 40
differernt SAP content
Compressive strength of AAFS mortars with differernt slag

Figure 41
content
9
Compressive strength development of AAFS mortars with

Figure 42
differernt slag content
Autogenous shinakge of AAFS mortars with differernt SAP

Figure 43
content
Autogenous shrinkage of AAFS mortars with differernt slag

Figure 44
content
Drying shrinkage of AAFS mortars with differernt SAP

Figure 45
content
Change in mass of AAFS mortars with differernt SAP

Figure 46
content
Drying shrinkage of AAFS mortars with differernt slag

Figure 47
content
Change in mass of AAFS mortars with differernt slag

Figure 48
content
Figure 49 Samples with curvature
Figure 50 IRH of AAFS mortars with different SAP content
Figure 51 IRH of AAFS mortars with different slag content
LIST OF TABLES
Title
Table 1 Literature review of mix proportions
Table 2 FA and GGBS chemical composition (wt%)
Table 3 Specific gravity of each material
Table 4 Properties of selected SP
Characteristics of selected SAP (Source: Tu and Zhu, 2018)

Table 5
[108]
Table 6 Mix Proportion of AAFS mortars
Table 7 Summary of the tests performed in this study
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1. INTRODUCTION
1.1. Background
Concrete is one of the most widely used construction materials in the world, which is
conventionally produced using OPC. The production of OPC reaches approximately 12 million
tonnes each year in the UK (British Geological Survey, 2007) [18]. As the primary binder of
conventional concrete, the ratio of OPC occupies approximately 10% to 15% by the mass of
concrete. Nevertheless, the production of OPC brings severe environmental problems over the
production of carbon dioxide (CO2). According to Malhotra (2002) [73], the amount of CO2
emission from the production of OPC corresponds to about 7% of the global CO2 emissions,
which is mainly associated with the de-carbonation where CO2 is driven from the decomposition
of calcium carbonate (CaCO3).
CaCO3 (limestone) + Heat -> CaO + CO2
Apart from carbon emission, the cement industry also consumes approximately 10% of the
global energy used (Ali et al., 2011) [3]. The production of cement clinker from various raw
materials, such as limestone, shale and chalk, is carried out in a large kiln at 1500oC, which
consumes a considerable amount of energy. As the demand for OPC is gradually increasing,
emissions and energy consumption are expected to rise which attract attention from both local
and international level. In recent years, the concrete industry has adopted a transformation, from
a traditional approach to a new approach that aims to reduce adverse environmental impact from
OPC. The three traditional approaches to reducing CO2 emissions are energy efficiency,
alternative fuels and clinker substitution (Conesa et al., 2008; Barker et al., 2009) [25] [12].
However, it is anticipated that these existing approaches are not able to face the increasing
demand for cement in long-term.
The use of alkali-activated (AA) binders has gradually got higher attention as an alternative to
OPC because of its environmental benefits. While conventional concretes requires OPC that is
manufactured using considerable energy and involves de-carbonation, the production of alkali-
11
activated concrete (AAC) only requires AA binders. According to Turner and Collins (2013)
[109], AA binders can result in approximately 45% reduction in total CO 2 emissions. Studies
over the past decades also discovered that AAC has superior engineering properties, such as
excellent mechanical properties that comparable with OPC concrete (Provis et al., 2015;
Siriwardena et al., 2015) [89] [98], and excellent durability (Roy, 1999) [91]. AAC is somehow
classified as a green building material, because its binder (i.e. source material) is usually
industrial by-products, such as FA and GGBS. FA is fine powder produced from the burning of
pulverised coal in power plants, as shown in Figure 1, while GGBS is a powder by-product from
the blast-furnaces used to make iron, as shown in Figure 2. They have been extensively
investigated over the past decades and widely used as cement substitute (Bakharev et al., 1999;
Roy, 1999; Gruskovnjak et al., 2006; Kumur et al., 2009) [11] [91] [43] [63].
Figure 1. Fly Ash (FA) (Source: Lizmar, 2016) [70] Figure 2. Ground Granulated Blast-furnace
Slag (GGBS) (Source: Ecocem, 2018) [37]
Curing is a crucial process to develop the microstructure of concrete, which affects its strength
development, durability and serviceability. Conventional concrete often relies on external curing
to prevent rapid water loss during its hydration process, and making sure the concrete stays
moist. However, external curing often faces many limitations, which include:
1. Inconsistent moisture distribution within the mixture, limited by the permeability of the
mixture;
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2. Increase labour cost and time to carry out the work and supervision;
3. A significant amount of water is required while the curing effect is less effective;
4. Run-off may contaminate groundwater and soil;
5. As water is not able to penetrate the whole depth, moisture gradient could develop within
the material, resulting in warping/ curling (Jeong and Zollinger, 2004) [56]
In order to solve the limitations of external curing, some researchers introduced internal curing. It
has been studied extensively in the past 60 years and incorporated into concrete mixtures, via
several types of internal curing agents, such as pre-wetted lightweight aggregates (PWLA) and
superabsorbent polymer (SAP). The first publication is Paul Klieger in 1957 [60] who discovered
that LWA could pre-wetted, and used as an internal curing agent. Soon after, some researchers,
including Weber and Reinhardt (1995) [111], Bentur et al. (1999) [13], Kovler and Jensen
(2005) [62] and Henkensiefken et al. (2009) [46], investigated the internal curing effect via the
use of PWLA, and claimed that water could be transferred to the mixture during hydration
process.
It has been observed that internal curing can bring several benefits, which includes the
improvements in the degree of hydration in the early and later age as well as shrinkages (Dang et
al., 2017). The potential of using other internal curing agents was also investigated in-depth later
on, such as SAP (Jensen and Hansen, 2001, 2002, 2013) [54] [52] [51] and pre-wetted wood
fibres (Mohr et al., 2005) [79]. Until now, an increasing number of researchers have identified
the benefits and limitations of slag inclusion on the properties of AAF. Overall, shrinkage
problems are recognised as the major limitation of AAFS, which severely lower its crack
resistance and durability (Deb et al., 2015; Lee et al., 2014) [32], [66]. Yet, there is a limited
number of researchers has identified the corresponding solution.
13
1.2. Research Novelty
In recent years AAFS binder has been investigated as an exciting alternative of OPC. Among all
AAC, AAFS concrete has the most all-rounded engineering properties. However, it has the
problem with shrinkages, which in turn affects its crack resistance and durability. This reason has
severely limited the development and application of AAFS.
A number of researchers studied the effectiveness of internal curing, several internal curing
agents, and it was proven that they could improve the relative humidity, degree of hydration and
induced stresses of the specimen; hence, mitigate its shrinkages. However, there is a limited
number of researches have been carried out to investigate the inclusion of internal curing on
AAFS. Therefore, the present study would like to investigate the potential of using SAP on
AAFS mortar to mitigate its limitation on shrinkages.
1.3. Research Strategies
The primary attention of this study is the internal curing effect on AAFS mortar, especially how
it affects shrinkages. Fresh, physical and mechanical properties were also investigated to evaluate
how the inclusion of SAPs could affect the fundamental engineering properties of AAFS mortar.
Alongside with SAP, the effect of slag on AAFS was also evaluated. This study includes the
examination of five aspects of AAFS mortar with and without SAPs. Figure 3 and Figure 4
present the boundary of this study and all the tests involved respectively.
14
Workability
1. Fresh properties
Setting time
2. Physical properties Density
3. Mechanical properties Compressive strength
4. Shrinkages Autogenous shrinkage
Drying shrinkage
5. Internal relative humidity
Figure 3. Five aspects of investigation of AAFS mortars involved in the present study
Workability Flow table test
Setting Time Vicat setting time test
Density Ultrasonic pulse velocity (UPV) test
Compressive Strength Compression test
Autogenous shrinkage Non-contact laser measurements
Drying shrinkage Length comparator measurements
Internal relative humidity Humidity data logger measurements
Figure 4. Tests involved in the present study
15
1.4. Objectives of the Study
The primary objectives of the present study is as follows:
- Facilitate the development of AAFS by solving its shrinkage problems;
- Investigate the potential of applying internal curing on AAFS to mitigate shrinkages;
- Conduct a literature review of AA binders, AAFS system, internal curing and different
internal curing agents;
- Evaluate the effect of internal curing and slag on the engineering properties of AAFS
regarding workability, setting time, density, compressive strength, IRH, drying shrinkage
and autogenous shrinkage;
- Elaborate chemical shrinkage slightly using previous studies observations to understand
the reaction of AAFS, and discover how it correlates with other types of shrinkages and
setting;
- Consider the relationship between IRH, pore structure and shrinkages;
- Make recommendations for future development of AAFS concrete.
16
1.5. Outline of the Study
This study begins with a literature review of different AA materials, AAFS system, shrinkages,
internal curing and different internal curing agents. This is followed by the methodology of this
paper which includes details of the materials used, mix proportions and the tests involved.
Afterwards, experimental results on workability, setting time, density, compressive strength,
IRH, drying shrinkage, and autogenous shrinkage of AAFS mortar were evaluated and discussed
with observations made in previous studies. Further discussion was then made on the relationship
between IRH, pore structure and autogenous shrinkage. Then, conclusion and prospectus were
drawn to summarise the present study. Finally, based on the adopted scope of mix proportion, an
optimal mix proportions of AAFS with SAP is suggested.
2. LITERATURE REVIEW
2.1. Alkali-Activated (AA) Materials
In general, alkali-activated materials can be classified into three systems,
- Alkali-activated fly ash (AAF)
- Alkali-activated ground granulated blast-furnace slag (AAS)
- Alkali-activated fly ash/slag (AAFS)
Some studies have investigated the reaction mechanism of AAF and AAS. It was noted that the
primary reaction product of AAF is amorphous aluminosilicate gel (A-S-H) (Komljenovic et al.,
2010; Criado et al., 2008; Jun and Oh, 2014) [61] [28] [59]. And, the primary reaction product of
AAS is calcium silicate hydrate gel (C-S-H) (Melo Neto et al., 2008; Bernal et al., 2011; Chi,
2012) [77] [16] [23]. Comparing with AAF and AAS, the alkaline reaction of AAFS is more
complicated which consists of two reaction processes of both AAF and AAS systems. The two
primary reaction products of AAFS are sodium aluminosilicate hydrate (N-A-S-H) gel and
aluminium-modified calcium silicate hydrate (C-A-S-H) gel.
17
Both AAF and AAS system have their strengths. The significant features of AAF are low
shrinkage, high acid resistance and high heat resistance (Lee and Deventer, 2002) [67].
Meanwhile, the features of AAS are rapid setting, high strength and high fire resistance (Melo
Neto et al., 2008; Shi et al., 2011; Yang et al., 2011; Chi, 2012) [77] [96] [113] [23]. However, it
was discovered that both AAF and AAS also have their drawbacks. For example, AAF has to be
cured under elevated temperature and requires a high dosage of alkaline solution due to its low
activity pozzolanic reaction (Fan et al. 1999) [38] while AAS has several problems with its fresh
properties (Palacios et al. 2008) [86]. Soon after, several researchers, including Ismail et al.
(2014) [49], Bernal et al. (2013) [17], Nath and Sarker (2014) [81] and Deb et al. (2014) [31],
started to evaluate the potential of combining both systems and identify its properties. They
concluded that AAFS system is having decent engineering properties, which has the advantages
of each system and no heat curing is required. Taking mechanical property as an example, a
previous research has found that the 28-days compressive strength of AAFS mortar can reach up
to 57.88 MPa (Hojati and Radlińska, 2017) [47]. Therefore, AAFS is now a major investigation
focus of researchers.
2.2. Concern Over Alkali-Activated Fly Ash/Slag (AAFS) System
Slag replacement level is often a primary concern of most studies on AAFS because a slight
difference in the proportions of FA and GGBS could lead to significant properties difference.
Nath and Sarker (2014) [31] found that the slag content together with the type and concentration
of alkaline activator are the influencing factors on the properties of AAFS. The results of
Merjanovic et al. (2015) [74] revealed that the compressive strength of AAFS mixtures is
depended on the FA/GGBS ratio. Meanwhile, an increase of slag content would lead to the
decrease of workability and setting time (Lee and Lee, 2013) [64].
Slag content also having a relationship with the degree of shrinkages. As stated in a previous
study by Jiang et al. (2014) [57], the higher the slag content, the more significant the autogenous
shrinkage. This may be attributed to the physical presence of GGBS. Firstly, the surface of
18
GGBS may act as nucleation sites for hydrates. Moreover, the inclusion of slag may lead to the
formation of fine pores, resulting in the increase of autogenous shrinkage. Lee et al. (2014) [66]
and Fang et al. (2018) [40] both revealed that although higher slag content caused shrinkage
problems, it leads to higher compressive strength. Thus, mix proportion is particularly crucial to
AAFS system that a balance has to made between mechanical properties and shrinkages.
When designing the mixture proportion of AAFS, the slag content is not the only focus. Other
influencing factors include AL/B ratio, molarity of SH solution and SS/SH, which are also
affecting the properties of AAFS to a certain extent. For instance, it was evaluated by Fang et al.
(2018) [40] that the workability of AAFS could be significantly reduced when the molarity of SH
increases, and the compressive strength could be increased significantly when AL/B ratio
decreases. Up till now, several researches have been carried out to study the effect of different
parameters on the engineering properties of AAFS, including different AL/B, molarity of SH,
SS/SH ratio and slag content, as shown in Table 1. Lee and Lee (2013) [64] who studied the
setting time and compressive strength of AAFS concrete, suggested a slag replacement level
from 15% to 20% of the total binder is suitable to obtain a balance between the two properties.
Moreover, not long ago, apart from examining the effect of the parameter mentioned above on
AAFS concrete, Fang et. al. (2018) [40] also suggested an optimal mixture proportions of AAFS
with 20% to 30% slag content, AL/B ratio of 0.4, SP to binder ratio of 0.01, 10M of SH and
SS/SH ratio between 1.5 and 2.5 in terms of the criteria on fresh and mechanical properties.
Considering AAFS mortar, the proportion of binder and fine aggregate were in the ratio of 1.0
and 2.0 in a relevant study (Lee et al., 2014) [66]. Until now, the optimal mix proportions of
AAFS is still a subject of much discussion.
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Table. 1
Literature review of mix proportions
Type AL/B W/B S/B SS/SH SAP SP FA/GGBS Source
90/10;
AAFS
0.34 2.0 80/20; Lee et al. (2014) [66]
mortar
70/30
90/10;
AAFS 1% of Fang et al. (2018) [39]
0.4 2.0 80/20;
paste binder
70/30
90/10;
85/15;
AAFS
0.4 1.5-2.5 80/20; Fang et al. (2018) [40]
Concrete
75/25;
70/30
AAS 0.3% of Oh, S. and Choi, Y.

0.4 2.37 (2018) [84]
mortar binder
0% to
AAS
0.4 2.4 0.6% of Song et al. (2016) [104]
mortar
binder
2.3. Shrinkages
Shrinkage generally used to describe various aspects of volume reduction in concrete. Volume
changes are particularly significant to concrete because they directly affect the long-term
strength, crack resistance and durability of the concrete. Cracks can easily be formed due to
shrinkage, and these cracks would lead to ingress of water which could severely harm the
performance and service life of concrete. Concretes are subjected to volume changes in different
ways after casting, which have overlapping effects but with different mechanisms. According to
Brooks (2015) [19], shrinkage of concrete can be classified into:
1. Plastic shrinkage
2. Chemical shrinkage
3. Autogenous shrinkage
4. Drying shrinkage
5. Carbonation shrinkage
20
2.3.1. Plastic Shrinkage
Plastic shrinkage happens in young concrete, within the first few hours the concrete is cast.
The concrete is still in plastic state at this stage that water can still move freely. Due to the
density difference between the binder and water, water tends to move upwards to the
surface, which is known as bleeding. As evaporation occurs at the surface layer of concrete,
tensile stresses develop and form cracks. Such type of shrinkage can often be reduced by
adequate curing, utilisation of admixtures and via the use of fibres.
2.3.2. Chemical Shrinkage
Jensen and Hansen (2001) [53] described chemical shrinkage as “the change in total internal
volume as cement hydrates”. Chemical shrinkage is caused by two major mechanism, one is
the volume reduction associated with hydration process as the overall volume of reaction
products are smaller than the volume of the original unreacted binder, the other is due to
self-desiccation.
Continual desiccation causes the water in pores to vaporise (Bentz and Snyder, 1999) [14],
resulting in the decrease in relative humidity and high curvature of menisci, followed by
shrinkage stresses (Collins and Sanjayan, 2000) [24]. External curing water often replaces
the water in the capillaries consumed by desiccation. However, external curing is not
efficient in delivering uniform moisture throughout the cementitious mixture. Such type of
shrinkage has a significant contribution to the early volume change of concrete.
2.3.3. Autogenous Shrinkage
Autogenous shrinkage takes place in young concrete when water is consumed during
hydration process. Jensen and Hansen (2001) [53] described it as “the change in external
volume of a concrete mixture due to chemical shrinkage”. At liquid state, autogenous
shrinkage is an outcome of chemical shrinkage. When the mixture hardened, external
21
volume is restricted by its rigid skeleton, resulting external volume cannot be changed
equivalently with chemical shrinkage, and autogenous shrinkage (i.e. external volume
reduction) becomes smaller than chemical shrinkage (i.e. internal volume reduction)
(Henkensiefken et al., 2009) [46]. The difference between chemical shrinkage and
autogenous shrinkage will lead to the formation of voids. According to Fang et al., (2018)
[39], chemical shrinkage is responsible for approximately 70% of total autogenous
shrinkage.
Such shrinkage is due to the loss of water from capillaries and gel pores for the hydration
process. In other words, the internal moisture of the concrete is reduced during the hydration
process. This creates fine capillaries where surface tension will occur and causes autogenous
shrinkage, and therefore, forming cracks.
2.3.4. Drying Shrinkage
Drying shrinkage happens when water is evaporated from concrete during drying, which is a
long lasting process. Drying shrinkage is unpreventable unless the concrete is completely
submerged in water. When the concrete is exposed to drying condition, there is a difference
in the relative humidity between the environment and that of concrete, as a result, water
within the concrete will be lost. Such shrinkage is due to the loss of water held in gel pores,
and the water within concrete is lost gradually over an extended period. Continual drying
also leads to an increase of attraction forces between C-S-H hydration products, causing
shrinkage (Mindess et al., 2003) [78].
The magnitude of carbonation shrinkage is relatively small compared to other shrinkages;
thus, it is usually less considered. As the magnitude of autogenous and drying shrinkage are
relatively more significant than the others. They are often the primary concern in researches.
22
2.4. Internal Curing
Internal curing is a technique that provides an internal water reservoir in specimens. It is
anticipated as an effective means to produce mixtures that are more durable and have much
better resistance to shrinkage cracking. For long-term durability, the control of early-age
cracking due to shrinkage is essential.
According to the American Concrete Institute, internal curing is defined as,
“supplying water throughout a freshly placed cementitious mixture using reservoirs, such as pre-
wetted lightweight aggregates (PWLA) and other internal curing agents, that readily release
water as needed for hydration or to replace moisture lost through evaporation or self-
desiccation”.
In other words, the principal idea of internal curing is to use absorptive materials that possess
decent absorption and desorption ability to supply additional moisture within the specimens to
enhance the uniformity of moisture distribution and temperature variation, especially to maintain
the IRH of mixtures during self-desiccation. When water in capillaries pores are drawn rapidly,
the IRH in the mixture is reduced rapidly, which increases internal stresses and causing cracks.
This is notably more significant when the mixture is having a low water content (Neville, 2012)
[82]. Moreover, internal curing is particularly useful for concretes with low permeability because
water transport is limited throughout the whole specimen when the microstructure is dense.
Autogenous shrinkage is often hard to reduce significantly through external curing.
Moreover, researches on the hydration mechanism of cement shown that one of the critical
parameters in producing high strength concrete is the use of low liquid binder ratio (Dudziak and
Mechtcherine, 2010) [35]. For instance, high performance concretes and newly introduced
concretes, such as AAC and fibre reinforced concrete (FRC) are both having a low water-to-
binder ratio. However, this will result in the decrease of IRH, which makes them susceptible to
23
autogenous shrinkage. And one possible solution is to use internal curing agents that serve as
water reservoirs to distribute water evenly throughout the concrete. Internal curing has appeared
as a promising technology that significantly improves the cracking resistance and durability of
concretes.
2.4.1. General Benefits of Internal Curing
Campbell and Tobin in 1967 [22] first identified the benefit of internal curing. Unlike to
conventional curing that external water can only penetrate into the limited depth of the
concrete, internal curing can be very beneficial to have a uniform moisture distribution
within the concrete, as illustrated in Figure 5.
Figure 5. Visual illustration of external curing (conventional curing) compared with internal
curing (Source: Bentz and Weiss, 2011) [15]
The main benefits of internal curing are 1) Reduced autogenous shrinkage, and its
corresponding stresses - Water disport from internal curing agents will fill the capillaries
pores that can cause autogenous shrinkage. Internal curing water released prevents self-
desiccation and hence, autogenous shrinkage. Usually, internal curing can reduce the rate
of shrinkage significantly.
2) Improved durability – When internal curing is incorporated, it can provide additional
water to concrete mixture within the concrete itself which decreases the chance of cracking
24
(Delatte and Cleary, 2008) [33]. In other words, internal curing provides better crack
resistance to concrete. Moreover, the application of internal curing can reduce the
permeability of the concrete, which minimise the ingress of aggressive substances, such as
chloride ions. Also, concretes with internal curing experiences tighter cracks, resulting in
better durability.
3) Reduced curling - According to Wei and Hansen (2008) [112], the curling effect on
concrete can be reduced significantly with the use of internal curing without changing the
w/c ratio. Curling generally arises when there is a moisture gradient within concrete. By the
introduction of internal curing, concrete structures can have more uniform moisture
distribution.
2.5. Different Internal Curing Agent
Byard and Schindler (2010) [21] claimed that highly absorptive materials could function internal
curing. Pre-wetted lightweight aggregate (PWLA) is used to provide internal curing effect since
long ago; therefore, it has a more comprehensive and developed database compared to SAP and
wood pulp, which are newly discovered. According to Byard and Schindler (2010) [21], PLWA
may contribute to the strength of the cementitious mixture while SAP and wood pump do not.
2.5.1. Superabsorbent Polymers (SAPs)
SAPs are white powder in irregular shapes as shown in Figure 6. Although only very few
SAPs are added into mixtures, they could significantly enhance the properties and
performance of the mixture in its fresh and hardened state. SAP offers different possibilities
over rheological properties.
25
Figure 6. Microstructure of SAPs
Jensen and Hansen first investigated the application of SAPs as an internal curing agent in
2001 and 2002. A number of studies, including Jensen and Hansen (2001) [54], Jensen
(2013) [52], Dudziak et al. (2008) [36] and Craeye and De Schutter (2008) [26], proved that
SAP works exceptionally well with cementitious materials and could be used to mitigate
autogenous shrinkage by changing the rheology of fresh material (Jensen, 2008) [55],
increase the freeze/thaw resistance (Mönnig and Lura, 2007) [80], self-sealing (Snoeck et
al., 2012) [101] and even promote autogenous healing (Snoeck et al., 2012) [102]. SAP’s
chemical stability in a highly alkaline environment, together with absorption and desorption
behaviour in concrete and its particle size are all very satisfying (Pourjavadi et al., 2008)
[88]. Nowadays, SAP is one of the most commonly used internal curing agents because of
its decent water absorption and desorption ability and the various benefits that it could bring
to the mixture.
It has been shown that the application of SAP as an internal curing agent has both positive
and negative effects on concrete. According to Mechtcherine et al. (2008) [75], the
additional of SAP can increase porosity but may reduce the strength of concrete. Moreover,
some previous researches, such as Dudziak et al. (2008) [36], Geiker et al. (2004) [41],
Igarashi and Watanabe (2006) [48] and Pierard et al. (2006) [87], also indicated that SAP
can effectively reduce the degree of autogenous, promote hydration process and resulting
26
in a better microstructure of matrices. Also, when SAP collapses, it will leave pores that
bring significant changes to the microstructure of hardened concrete or mortar, which
eventually provides extra spaces for deposition of later products (Snoeck et al., 2015)
[103].
The establishment of “Application of Superabsorbent Polymer in Concrete Construction” –
RILEM Technical Committee 225-SAP coordinated and concluded the results of studies
with respect to the influence of SAPs on concrete, such as rheological properties, shrinkage
behaviour and durability, it has well established a database for future usage of SAPs on
concretes, especially as an internal curing agent.
27
2.5.1.1. Mechanism and Effectiveness of Superabsorbent Polymers
In general, SAPs are crossed linked networks of flexible polymer chains. As the
polymers are crossed linked, they swell to accommodate the additional molecules
instead of dissolving when they are in contact with water. They could absorb a
considerable amount of liquid relative to its mass. The effectiveness of SAP as an
internal curing agent is mainly related to its swelling ratio, which is the rate at which
the SAP absorbs and releases water and the spacing within SAP particles (Siramanont
et al., 2010) [97]. These factors are dependent on the structure of SAP and its particle
size.
Figure 7. SAP particles in dry condition (left) and after absorption of water (right) (Source:
Schwarz, 2005) [95]
The absorption ability of SAP were first explored by Jensen and Hensen (2002) [52]
using the time measurement method. They revealed that the internal curing efficiency
of SAPs increased with the decrease of particle size and the optimum size is
approximately 100 μm. Some recent studies indicated that as long as the average size of
the SAPs is in the range of 300μm to 1000 μm, it is still effective in improving the
degree of hydration and mitigate autogenous shrinkage (Wang et al., 2009; Schröfl et
al., 2012) [110] [94].
When incorporating SAP into mixtures, it is important to determine its absorption
ability because it directly affects the amount of additional water required for mixing. In
a previous study conducted by Oh and Choi (2018) [84], about 4.2 wt% of binder
28
additional water was added with 0.3% of SAP content. ‘Tea bag’ method has been
explored in a number of studies by researchers including Schröfl et al. (2012) [94] and
Mechtcherine et al. (2015) [76], and it is known as the most commonly used method to
determine the absorption capacity of SAP. In general, SAP with higher water
absorption capacity (i.e. low particle size) is said to be more efficient in reduction of
autogenous shrinkage because it could release more water within the material when
necessary.
2.6. Selection of Internal Curing Agent
The two most commonly used agents for internal curing are either PWLA or SAP. For
PWLA, both coarse aggregate and fine aggregate are also applicable for internal curing.
However, there are several requirements in using aggregate for water entrainment. To be used
as an internal curing agent, the aggregate needs to have a pore structure that is relatively good
at absorption and desorption (Lura et al., 2004) [72]. Also, the aggregate should have a
similar grading as the original sand that is replaced and should have no adverse effects on
workability (Alexander and Mindess, 2005) [2]. Moreover, when coarse LWA is used, a
relatively higher replacement level of normal coarse aggregate is required to eliminate
autogenous shrinkage (de Sensale and Goncalves, 2014) [30].
Conversely, SAP can absorb a significant amount of water, and release it when the conditions
within mixture changes. Compared to LWA, the use of SAPs has some particularities. SAPs
are applied as a dry ingredient, while the degree of saturation of LWA directly affects the
effectiveness of its internal curing effect, such that partially saturated LWA is not able to
deliver the proper effect. Thus, extra effort is required when using PWLA as an internal
curing agent.
Water entrainment using SAP is considered as the one of the most straightforward internal
curing methods. Pierard et al. (2006) [87] demonstrated that SAPs could prevent autogenous
29
shrinkage more effectively than traditional shrinkage reducing agent, such as PWLA and
shrinkage-reducing admixture. However, according to Schrofl et al. (2012) [94] and Assmann
(2013) [5], the performance of SAP in mixtures is influences by the type and size of the SAP
along with the interaction with the binder. Therefore, the selection of SAP must be carefully
made when using it as an internal curing agent.
2.7. Saturation of Fine Aggregate
When carrying out mixing, it is essential to use moist aggregate with saturated surface dry (SSD)
condition. SSD refers to the condition of the aggregate when all permeable pores are completely
saturated with water, and its surface has no free moisture and no excess water. When the
aggregate is dry, the high water absorption from the mixture can lead to rapid loss of workability.
On the other hand, when moist aggregate is used, the aggregate will not draw water from the
mixture and the water it contains may even be available for the hydration process. This helps to
sustain the desired workability and reduce shrinkage stresses. In general, there are four aggregate
moisture conditions:
1. Oven-dry (Pores are completely empty)
2. Air-dry (Pores are partially filled)
3. Saturated surface dry (SSD) (Pores are completely filled but no excess water)
4. Wet (Excess water)
Figure 8. Four aggregate moisture conditions (Source: NRRMCA, 2018) [83]
30
2.8. Summary of Literature Review
- AA binders are getting more attention as an alternative of OPC because of environmental
friendliness;
- AAF, AAS and AAFS are the three most commonly used systems of AA binders.
Among them, AAFS is said to have the combined benefits of AAF and AAS system, that
AAFS has a high potential to be further developed;
- AAFS is having decent mechanical properties according to several studies. However, its
main problem is shrinkages that has limited its development. It is considered that mixture
with 20% to 30% slag replacement level for FA, AL/B ratio of 0.4, SP to binder ratio of
0.01, 10M of SH and SS/SH ratio of 2.0, S/B ratio of 2.0 and SAP content in the range of
0.2% to 0.5% would be a suitable scope of mix proportions for AAFS mortars with SAP.
- Internal curing is well established and proven works well with cementitious materials
and bring a number of benefits to mixtures. Different internal curing agents are being
used nowadays. However, it is believed that SAP is one of the most straightforward
internal curing agents;
- SAP mechanism is mainly related to its crossed linked polymers, and they will swell to
accommodate the additional molecules when in contact with water. The absorption and
desorption ability of SAP is associated to its structure and particle size;
- The fine aggregate has to be at SSD condition to ensure that it will not absorb water from
the mixture and affect the desired mixture properties.
Based on the literature review, the potential of incorporating internal curing to AAFS mortar was
investigated.
31
3. EXPERIMENTS
3.1. Materials
In this study, the binder of the AAFS mortars is class F FA and GGBS. The mean particle size of
FA and GGBS are 26.81 𝜇𝑚 and 14.77 𝜇𝑚 respectively. The chemical composition of FA and
GGBS are shown in Table 2. Specific gravity and particle size distribution of each material are
listed in Table 3 and Figure 11 respectively. The alkaline activator was prepared using sodium
hydroxide (NaOH) pellets which have a density of 1.2145 kg/m3, with distilled water and sodium
silicate solution (SS), which has the chemical composition of 31.1% SiO2 and 12.5% Na2O by
mass. The alkaline solution is prepared 24 hours before each mixing. The molecular ratio of SiO2
to Na2O is 2.58.
Figure 9. Selected FA Figure 10. Selected GGBS
Table. 2
FA and GGBS chemical composition (wt%)
SiO2 Al2O3 CaO MgO K2O Fe2O3 TiO2 Na2O SO3 MnO
FA 53.24 26.42 3.65 9.55 2.57 1.65 0.86 0.76 0.56 -
GGBS 34.30 15.00 39.40 8.00 0.38 0.40 0.70 0.45 - 0.50
32
Table. 3
Specific Gravity of each material
FA GGBS SS SH SPs
Specific
2.25 2.9 1.309 1.45 1.08
Gravity
100
FA
GGBS
SAP
80
Cumulative volume (%)
60
40
20
0
1 10 100 1000
Particle diameter (m)
Figure 11. Particle size distribution of FA, GGBS and SAP
Superplasticizer (SP) was used in all mixtures to improve the workability of AAFS mortars. The
SP, which is supplied by Sika group, has a density of 1.08 kg/l. Detail properties of the
superplasticizer are listed in Table 4.
Figure 12. Selected SP
33
Table. 4
Properties of selected SP
Content of Chloride ion Content of Alkaline
Specific Gravity (25 oC) pH value (25 oC)
(%) (%)
2.25 4-5 <0.1 Max 0.40
For fine aggregate, natural sand with maximum nominal size of 4 mm was used, and it was used
in SSD condition according to ASTM C128-15 [10]. The SAP (AQUASORBTM 3005 S) is
supplied by SNF, UK. It is cross-linked copolymer or acrylamide and potassium acrylate with
irregular particle shape which has the particle size of < 300 𝜇𝑚. The characteristics of the
selected SAP is shown in Table 5.
Figure 13. Selected fine aggregate
Figure 14. Microstructure of SAPs Figure 15. Selected SAPs

34
Table. 5
Characteristics of selected SAP (Source: Tu and Zhu, 2018) [108]
Product characteristics Maximal absorption
Very fine white
Appearance m/m de-ionised water (pH 6.5) 400 g/g SAP
powder
Moisture content 10% m/m tap water (pH 6.8) 200 g/g SAP
m/m modelled reaction

Approximate bulk density 900 kg/m3 18 g/g SAP
environment (pH)
m/m during AAM paste mixing
Solubility Insoluble in water 12.5 g/g SAP
(pH)
3.2. Mix Proportion
In this study, AAFS specimens with same AL/B ratio, S/B ratio, SP content, molarity of SH and
SS/SH were prepared and tested. The scope of mixture proportions of AAFS mortars was
adopted after reviewing previous studies, as shown in Table 1. Labels ‘S’ and ‘G’ represent two
different sets of specimen series and the number, ‘0.2’, ‘0.3’, ‘0.4’ and ‘0.5’ is the percentage of
superabsorbent polymer (SAP) by weight. The number ‘15’, ‘20’ and ‘30’ represents the
percentage of GGBS replacement level for FA by weight.. For ‘S’ series, M0 to M4 are mixtures
with 0%, 0.2%, 0.3%, 0.4% and 0.5% SAP content respectively. The proportion between FA and
GGBS was constant at 75/25 for all these mixtures. Therefore, the effect of internal curing on the
engineering properties and shrinkages of AAFS mortars can be investigated.
For ‘G’ series, the proportion between FA and GGBS of M5 to M7 was changed to 85/15, 80/20
and 70/30 respectively, while the SAP content was kept constant at 0.3%. This way, the effect of
FA/GGBS ratio on the engineering properties of AAFS mortars can be studied using this series.
The AAFS mortars were prepared and the mix designs were listed below.
‘Tea-bag method’ was carried out by Tu and Zhu (2018) [108] to determine the absorption
ability of the selected SAP. It was noted that a single gram of the SAP could absorb
35
approximately 12.5 g of water. Therefore, additional water was added accordingly when
preparing mixtures. The total binder was kept constant as 400 kg/m3 for all the mixtures.
Table. 6
Mix proportions of AAFS mortars
Fine
Mix Binder FA GGBS SS SH SPs SAP Water
Labels aggregate
No. (kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3)
(kg/m3)
M0 S0 400 800 300 100 106.5 53.5 4 0 0
M1 S0.2 400 800 300 100 106.5 53.5 4 0.8 10
M2 S0.3 400 800 300 100 106.5 53.5 4 1.2 15
M3 S0.4 400 800 300 100 106.5 53.5 4 1.6 20
M4 S0.5 400 800 300 100 106.5 53.5 4 2.0 25
M5 G15 400 800 340 60 106.5 53.5 4 1.2 15
M6 G20 400 800 320 80 106.5 53.5 4 1.2 15
M7 G30 400 800 280 120 106.5 53.5 4 1.2 15
Note: FA: Fly Ash; GGBS: Ground granulated blast-furnace slag; SS: Sodium hydroxide; SH: Sodium hydroxide; SPs:
Superplasticizer; SAP: Superabsorbent polymers; Mix No. 0 – 4, constant 25% slag level; Mix No. 5 – 7, SAP content
is 0.3 wt% of binder
# Detail example of calculation of M1 is in appendix A
36
3.3. Specimens Preparation

AAFS mortars with and without SAP in the present study were prepared using the procedures as
shown in Figure 16 and Figure 17 respectively:
Mixing Time: 30s

Mix dry binder: FA and
GGBS
Mixing Time: 90s

Add half of the alkaline
activator and additional
water
Mixing Time: 60s
Add SAP powder into the

mixture
Mixing Time: 180s

Add the rest of the
solution
Complete mixing
Figure 16. Mixing procedures of AAFS mortars with SAP
Mixing Time: 30s

Mix dry binder: FA and
GGBS
Mixing Time: 90s

Add half of the alkaline
activator and additional
water
Mixing Time: 180s

Add the rest of the
solution
Complete mixing
Figure 17. Mixing procedures of AAFS mortars without SAP
37
Mixtures were then casted into different moulds,
▪ Cube moulds for compressive strength test (50 x50 x 50 mm3) - ASTM C109/C109M
▪ Cube moulds for autogenous shrinkage test (70 x 70 x 70 mm3) – non-contact laser
method
▪ Rectangular moulds for drying shrinkage (285 x 25 x 25 mm3) – ASTM C596-09
Followed by compaction using vibration table. All specimens were de-moulded after 24 hours
and stored in the curing room (20±1 oC, 50±10% RH) until they were tested.
Figure 18. Medium size mixer Figure 19. Small size mixer
used in the present study used in the present study
(Capacity 10L) (Capacity 1.5L)
38
3.4. Testing Methods
Table. 7
Summary of the tests performed in this study
No. of
samples
Aspects Tests ASTM
for each
mix
Workability Flow Table C1437-15 1

Fresh
properties
Setting Time Vicat setting test C191-13 1
Physical
Density Ultrasonic pulse velocity (UPV) C597 3
Properties
Mechanical
Compressive strength Compression test C109 3
properties
Autogenous shrinkage Non-contact laser method / 1

Shrinkage
Drying shrinkage Length comparator C596-09 4
Internal relative humidity

Moisture Data logger / 1
(IRH)
3.4.1. Fresh Properties
3.4.1.1. Workability
Workability of AAFS mortars was investigated using flow table test according to
ASTM C1437-15, in which the base diameter in two direction of the mortar is
measured to calculate the flow value. The flow value was then calculated using the
equation below,
𝐷1 + 𝐷2
2 − 𝐷𝑖
𝐹𝑙𝑜𝑤 𝑣𝑎𝑙𝑢𝑒 (%) = × 100
𝐷𝑖
Where D1 and D2 are the diameter (mm) of the spread in first and second direction
respectively, and Di is the original inside base diameter (mm) (i.e. 100 mm)
Flow mould with diameter of 100 mm was placed at the centre of the flow table. The
mould is filled completely with mortars, followed by a cut off of mortars across the top
39
of the mould. After the mould is lifted away, flow table was dropped 25 times within
15s. Afterwards, the diameters in vertical and horizontal direction were measured. To
ensure the uniformity and better results, the mortar was tapered 20 times when the
mould is half filled.
Figure 20. Flow table used in the present study
3.4.1.2. Setting Time
Vicat setting test was used to determine the setting time of the mixtures according to
ASTM C191-13 [7], in which the initial and final setting time were specified. The
change of penetration depth when the mixture hardened was measured by the Vicat
needle, and it is the difference between the depth at first drop and the depth of the drop
after it.
The initial setting time is the time when the penetration is measured to be 25 mm, while
the final setting time is the time when the maximum change of penetration depth is
reached, which is 36 mm in this case. The tests were carried out in a room with
temperature of 23 oC.
40
Figure 21. Vicat setting test apparatus
3.4.2. Physical Properties
3.4.2.1. Ultrasonic Pulse Velocity (UPV)
UPV tests of the specimens were carried out according to ASTM C597 [9].
Measurements were obtained before the mortar cubes were brought to compression
test. UPV test is measuring the travel time of waves in a specimen, and it correlates to
its mechanical properties and density. UPV test allows to monitor the density and
homogeneity of the material. It can provide information about strength evolution and
the existence of voids. Sufficient coupling gel and pressure were applied to ensure
stable and accurate readings.
Figure 22. UPV test apparatus
41
3.4.3. Mechanical Properties
3.4.3.1. Compressive Strength
Compressive strength tests of the specimens were conducted according to ASTM C109
[6]. 50 x 50 x 50 mm3 cube moulds were prepared and three samples of each mix were
tested at the age of 1, 7, 14 and 28 days to determine their average compressive
strength. According to Fang et al. (2018) [40], the compressive strength of AAFS
concrete develops rapidly in the first 28 days but after that the rate of strength
development became slow. Therefore, compressive strength of AAFS mortars after 28
days is not assessed in this study.
Load rate of 1200 N/s and sensitivity of 10 kN were used for the compression test.
Failure load is obtained from the testing machine and the compressive strength is
calculated as follows:
Failure Load (F)

Strength (σ) = Area of the loaded surface (A)
Figure 23. Machine for compression test
42
3.4.4. Shrinkage
3.4.4.1. Autogenous Shrinkage
Autogenous shrinkage can often be identified by linear or volumetric measurements.
Linear measurements can be classified into non-contact and contact methods. Linear
variable Differential Transformer sensors (LVDTs) is one of the example of contact
methods. In this study, a non-contact method with laser displacement sensors was used
for autogenous shrinkage measurements because it can provide more accurate results
compared to contact methods. For mortars, autogenous shrinkage measurements have
been observed to work well using non-contact laser measurements (Sant et al., 2006)
[93].
Mixtures were casted into 70 x 70 x 70 mm3 cubic PVC mould with sealed cover.
Plastic sheets were placed into the mould followed by spreading oil between the plastic
sheet and the mould to control the friction between them. After mixtures were casted
into the mould, it was covered by a plastic sheet and a thin PVC plate to limit
evaporation of the mixture.
The mould was then placed in the shrinkage testing chamber with a constant humidity
of 40% and temperature of 20 oC. When the sample shrinks, the plates were moved
together with the sample in the horizontal direction. And the laser sensor could detect
the displacement. The data were logged at 0.2 second interval for a period of 48 hours.
Setup of the laser displacement method is shown in Figure 26.
43
Figure 24. Visual presentation of laser displacement method (Source: Fang et al, 2018) [39]
Figure 25. Mould for laser displacement method Figure 26. Laser displacement method setup
3.4.4.2. Drying Shrinkage
Drying shrinkage tests of the specimens were conducted according to ASTM C596-09
[8]. Mixtures were casted into 285 x 25 x 25 mm3 (ASTM C490) moulds and then
demoulded after 24 hours. Specimens were then placed in the curing room with
humidity 50 ± 10% at the temperature of 20±1 oC. Length measurements were taken
using length comparator according to ASTM C490. The mass of the samples was also
measured under the same condition after length measurements were obtained. The
initial length of the specimens was measured as datum followed by the length of the
specimens up to 28 days. The change in length is calculated using equation (1).
44
(𝐿𝑖 −𝐿𝑥)
Change in length (%) = × 100% (1)
𝐺
Where Li = initial length; Lx = Length of the specimens measured at different curing
ages; G is nominal effective length (250 mm)
Figure 27. Length comparator
3.4.5. Internal Relative Humidity (IRH)
IRH of AAFS mortars was measured using humidity data logger. A cylindrical filter with
plenty of small holes was used to contain the data logger. AAFS mortars were casted into
cylindrical moulds and the cylindrical filters were placed into the moulds, as shown in
Figure 28.
After casting the mortar, the moulds were sealed by many layers of cling film to minimise
water evaporation and protect the data logger. The samples were then placed in a room with
humidity of 65 ± 10 % at the temperature of 23 ± 2 oC for 48 hours. The relative humidity
data was logged at 1 minute interval during that period.
45
Figure 28. Visual presentation of IRH Figure 29. IRH setup sample
measurement setup (Source: Fang et al.
2018) [39]
4. DISCUSSION AND RESULTS
4.1. Workability
Figure 30 shows the variation in flow value of AAFS mortars with different SAP content. It
revealed that the flow value increases with the increase of SAP content. When the SAP content
increases from 0% to 0.5%, the flow value increases from 95% to 167.5%, which indicates that
the addition of SAP could lead to significant difference in workability. The higher SAP content,
the lower viscous degree the AAFS mortar is having. It can be seen that the flow value of AAFS
mortars without SAP is much lower than those with SAP. However, the effect varied with
different amount of SAP, the flow value of M1, M2, M3 and M4 was found to be improved by
33.68%, 65.26%, 72.11% and 76.32% respectively as compared to M0 (0% SAP content). For
the increment of SAP content from 0% to 0.5%, the effect of M1 (0.2% SAP) is the most
pronounced.
Generally, the variation among workability of different mortars can be attributed to the spherical
shape and volume of SAP. The results indicated that the spherical shape of SAP could contribute
46
a lubrication effect in mixtures to reduce friction between fine aggregate and the paste, resulting
better fluidity of the mixture.
Figure 30. Flow value of AAFS mortars with different SAP content
Figure 31 shows the flow values of four different AAFS mortars in series ‘G’. It can be realised
that the variation of flow value follows a trend that mortars with higher slag content, exhibited
declines in workability. When the slag content varies from 15% to 30%, the flow value decreases
from 172.5% to 155%. These results indicate that for higher slag content, the workability of the
mixture drops, which is aligned with previous studies (Deb et al., 2014; Fang et al., 2018; Nath
and Sarker, 2014) [31], [40], [81]. The accelerated reaction of Ca and the angular shape of slag
could be responsible for the reduction in workability (Deb et al., 2014) [31]. The flow value of
M6, M2 and M7 was decreased by 2.61%, 8.99% and 10.14% respectively as compared to M5.
The results showed that the effect on workability appeared to be most significant on M2 (slag
replacement level of 25%).
47
Figure 31. Flow value of AAFS mortars with different slag content
Generally, the effect of slag on the workability of AAFS with and without SAP is similar.
Comparing with the flow values reported by Fang et al. (2018) [40], who investigated the flow
value of AAFS pastes which has no internal curing agent, the decrement in workability for the
slag content from 15% to 30% is 5%, 8% and 2% respectively. These results are similar to the
present study that the decrement of workability due to the same increment of slag is 4.5%, 11.0%
and 2% respectively. It is noted that both studies have the same SS/SH ratio, AL/B ratio and
molarity of SH.
4.2. Setting Time
Figure 32 shows the change of penetration depth of different AAFS mortars in series ‘S’. Using
the results, the corresponding initial and final setting time were identified according to ASTM
C191-13. Results demonstrated that specimens with higher SAP content experienced a delay in
setting, which is in line with the observation made by Song et al. (2016) [104]. The initial and
final setting time of AAFS mortars increased from 36 mins to 57 mins and from 46 mins to 67
mins respectively when the content of SAP is increased from 0% to 0.5%. The initial setting time
48
of M1, M2, M3 and M4 was increased by 25.00%, 33.30%, 44.44% and 58.33%, and the final
setting time was increased by 19.57%, 26.09%, 34.78% and 45.65% as compared to that of M0,
respectively. The results revealed that M1 (0.2% of SAP) exhibited a relatively higher increasing
percentage in setting time than the rest of the specimens. The longer setting time is likely due to
the additional water released from the swollen SAP during the early hydration process, which
retards the setting. Therefore, higher SAP content could effectively prolong the setting time of
the mixture.
Figure 32. Setting time of AAFS with different SAP content
Figure 33 illustrates the relation between the setting time and slag content of AAFS mortars. This
figure reveals that for a higher slag content, the initial and final setting time declines. The initial
setting time dropped from 66 mins to 32 mins, while the final setting time dropped from 86 mins
to 52 mins when the slag content varied from 15% to 30%. Comparing to M5 (15% slag content),
the initial setting time of M6, M2 and M7 was decreased by 50.00%, 56.25% and 106.25%,
while the final setting time was decreased by 11.54%, 15.38% and 65.38% respectively. It can be
seen that the effect of 30% slag content appeared to be most significant. These results coincide
with other previous studies that also identified that the addition of slag would lead to the
49
acceleration of the setting (Jang et al., 2014; Fang et al., 2018; Lee and Lee, 2015) [50], [39],
[65]. Higher replacement level of slag for FA would increase the CaO content resulting to the
extra release of calcium from the dissolution of slag and thus, facilitate the formation of C-A-S-H
gel and N-A-S-H gel (Lee and Lee, 2015) [65]. As the formation of C-A-S-H gel is likely to
accelerate the chemical reactions, it leads to rapid setting.
Figure 33. Setting time of AAFS mortars with different slag content
Comparing with the setting time of AAFS pastes measured by Hojati and Radlińska (2017), the
overall setting time of AAFS mortar is relatively short in the present study. This can be attributed
to the type and concentration of alkaline activator. According to Oh and Choi (2018) [84], the
setting time of mixtures activated by NaOH and SS are much shorter than those activated by
sodium carbonate. Besides, according to Fang et al. (2018) [39], the fluid-solid transition of
AAFS mortars is strongly affected by the slag content. It was reported that higher slag content
would lead to a significant drop in the transition time between initial and final setting. However,
due to the relatively short setting time of AAFS mortar in the present study, this behaviour is not
clearly shown.
50
Oh, S. and Choi, Y. (2018) [84] studied the internal curing effects and shrinkage reduction of
AAS mortar and concrete. They reported that the AAS mixture which has the SAP concentration
of 0.3 wt% of binder, was having an initial setting time of 14 minutes. Meanwhile, the initial
setting time of M7 in this study, which has the FA/GGBS ratio of 70/30 and same mix
proportions, is 32 minutes. This illustrates the benefit of using both FA and GGBS as the binder,
rather than only using GGBS, although the increase of slag content could improve mechanical
properties.
To have a more comprehensive idea about the early age reaction and setting process of AAFS
mortars, ICC and chemical shrinkage are two primary indications. Fang et al. (2018) [39] and Tu
and Zhu (2018) [108] have investigated the relationship between mix proportions, ICC results,
chemical reactions and chemical shrinkages of AAFS pastes. The reaction of AAFS pastes at
early 48 hours was determined with an isothermal calorimetry, together with the volumetric
method measurements of chemical shrinkage according to ASTM-12. The following
observations were made by Tu and Zhu (2018) [108]:
- Higher SAP content would 1) lead to a longer induction period (i.e. the peak-valley
between first dissolution peak and second later acceleration peak – fluid-solid transition
time) because it delays the chemical reactions; 2) retard the formation of reaction
products, which cause shallower accelerated peak; 3) cause slower setting.
And the following observations were made by Fang et al. (2018) [39]:
- Higher slag content would 1) lead to a shorter induction period; 2) accelerate the
formation of reaction products (i.e. N-A-S-H and C-A-S-H), which cause a steeper
accelerated peak; 3) cause quicker setting.
51
In the present study, it has been observed that setting time increases with the increase of SAP or
the decrease of slag content, which is same as the observation made by Tu and Zhu (2018) [108]
and Fang et al. (2018) [39] respectively. Figure 34, Figure 35, Figure 36 and Figure 37 show the
heat evolution and chemical shrinkage of AAFS pastes with different SAP content and slag
content in the first 48 hours respectively, conducted by Tu and Zhu (2018) [108]. Although ICC
and chemical shrinkage test were not performed in this study, using results reported by Tu and
Zhu (2018) [108] and Fang et al. (2018) [39], it can be concluded that the increase of SAP
content could indeed retard the chemical reactions (as shown in Figure 34 that the second
acceleration peak is being shifted toward to the right-hand-side of the chart when SAP content
increases), and hence, causing more extended setting and reduced chemical shrinkage (as shown
in Figure 35) while the increase of slag content would bring the exact opposite effect.
The inclusion of SAP in AAFS mortars not only could mitigate shrinkage problems, but also
benefits its engineering application due to more extended setting. On the other hand, although the
addition of slag in AAFS mortars could improve its mechanical properties, the amount has to be
carefully designed for the sake of setting and shrinkages.
Figure 34. Heat evolution of AAFS pastes with different SAP content (Source: Tu and Zhu, 2018) [108]
52
Figure 35. Chemical shrinkage of AAFS pastes with different SAP content (Source: Tu and Zhu, 2018) [108]
Figure 36. Heat evolution of AAFS pastes with different slag content (Source: Tu and Zhu, 2018) [108]
53
Figure 37. Chemical shrinkage of AAFS pastes with differrent slag content (Source: Tu and Zhu, 2018)
[108]
4.3. Ultrasonic Pulse Velocity (UPV) Test
Many previous works have been using UPV method to predict the compressive strength of
conventional concrete (S. Al-Nu’man et al., 2015; Lin et al., 2007; Tanigawa et al., 1984; Sturrup
et al., 1984) [92], [68], [106], [105]. However, there are limited researches on the use of UPV for
geopolymer concrete. Figure 38 illustrates the relationship between the UPV and compressive
strength of all AAFS mortars. In general, the UPV increased with curing age in all samples and
follows an exponential trend.. Two previous studies by Ghosh et al. (2018) [42] and Omer et al.
(2015) [85] also observed a similar trend, who studied the estimation of geopolymer concrete and
mortar strength in the use of UPV. The gradual increase of UPV shows the gradual development
of pore structure within specimens, as the density of specimens are getting higher and higher.
However, the rate of increase in velocity is different for all the samples at different curing ages
because the growth rate is significantly affected by mix proportions (Lin et al., 2007) [68]. Such
behaviour is also in line with findings of Hardjito and Wallah (2004) [44] and Bungey (1980)
54
[20]. M0 which has no SAP content, is the sample that achieved the highest UPV, which
coincides with its highest compressive strength among all the mixtures, as shown in Figure 39. A
relationship between UPV and compressive strength is somehow identified in the present study.
The wide spread of data is likely due to the effect from the addition of SAP which affects the
development of pore structure and the slight changes of the curing room condition. A past study
by Neville (2012) [82] reported that UPV travels quicker through water-filled voids than air-
filled voids. Thus, the humidity difference in the curing room may responsible for the wide
spread of the UPV results.
According to Tharmaratnam and Tan (1990) [107] and Demirboga (2004) [34], the compressive
strength and UPV can be related using the following equation:
𝑓𝑐 = 𝑎𝑒 𝑏𝑉
Where fc is the compressive strenth; a and b are constant and V is the UPV value
Using the experimental results, the relationship between compressive strength and UPV values
can be represented approximately with:
𝑓𝑐 = 4.0638𝑒 0.599𝑉
Figure 38. Relationship between compressive strength and UPV for all AAFS mortars
55
The correlation coefficient (R2 value) was around 0.35, which shows that although an
exponential relationship between UPV and compressive strength has been identified, the
approximation in the present study may not be adequate. However, it can be concluded that the
correlation between UPV and compressive strength for conventional concrete can also be applied
on geopolymer mortar which includes internal curing. It is understood that there is no unique
relationship which covers all conventional and geopolymer concrete because UPV values could
be influenced by many factors.
4.4. Compressive Strength
The compressive strength of AAFS mortars at 1, 7, 14 and 28 days, along with standard
deviation is shown in Figure 39. Overall, the compressive strength decreased with the increase of
SAP content. The 28-days compressive strength decreased from 57.213 MPa to 37.160 MPa
when the SAP content was increased from 0% to 0.5%. These results indicate that increasing
SAP content could negatively affect compressive strength which are consistent with other studies
(Liu et al. ,2017; Oh and Choi, 2018; Riyazi et al., 2017) [69], [84], [90]. This is likely due to the
water absorption from the swollen SAP during the hydration process, resulting in the formation
of voids in the materials. The 28-days compressive strength of AAFS mortar decreased by
8.99%, 40.48%*, 23.07% and 35.05% with every 0.1% increment of SAP content from 0.2% to
0.5% when compared to M0 (0% SAP content). This reveals that the compressive strength
decreased by 35.05% at most when SAP content varies from 0% to 0.5% and the effect of M4
(0.5% SAP content) on the decrease of compressive strength is the most pronounced. As shown
in Figure 39 and Figure 41, however, the measured 28-days compressive strength of M2 was
unexpectedly low, this error is due to the improper setting of compression machine, extra
samples have been prepared and will be tested in the future.
56
Figure 39. Compressive strength of AAFS mortars with differernt SAP content
Figure 40 shows the compressive strength development of the AAFS mortars with different SAP
content at 1, 7, 14 and 28 days. Changes in strength development was observed when SAP is
added into the mixture. Comparing with reference mortar, the strength development of SAP
mortars are slightly higher at the early age (1 day, 7 days) and lower at medium age (14 days), as
shown in Figure 40. For instance, the strength development rate at day-1 of M4 was 0.47%
higher than that of M0, while at day-14, the development rate of M4 was 5.28% lower than that
of M0. This shows the curing effect of SAP at the early age due to the supplement of additional
water for hydration and its adverse impact on compressive strength at medium age because of the
formation of voids. This behaviour from SAP was also observed by Dang et al. (2017) [29].
57
Figure 40. Compressive strength development of AAFS mortars with differernt SAP content
As shown in Figure 40, it is observed that the development of strength of SAP mortar started to
catch up after medium age and the decrease in strength at medium age may be similar to the
increase in strength caused by the internal curing at the early age. Several studies, including
Hasholt et al. (2012) [45] and Snoeck et al. (2014) [100], also claimed the addition of SAP could
bring both positive and negative effects on the strength development in the mixture.
Figure 41 shows the compressive strength of series ‘G’ AAFS mortars at 1, 7, 14 and 28 days
along with standard deviation. As shown in Figure 41, the 28- days compressive strength was
raised from 30.827 MPa to 49.587 MPa when the slag content varies from 15% to 30%. This
observation coincides with the results of previous studies by Kovler and Jensen (2005) [62], Lee
et al. (2014) [66] and Zhao et al. (2007) [115]. The 28-days compressive strength of mortars was
increased by 33.91%, 10.46%* and 60.856% with every 5% increment of slag content from 15%
to 30% as compared to M5 (slag content of 15%), showing the effect of 20% slag content looks
to be more prominent. When more slag is added, significant increase in strength was observed
because it would contribute to the formation of C-A-S-H type gel, which could densify the
microstructure of the material (Kumar et al., 2009; Lloyd et al., 2009) [63], [71].
58
Figure 41. Compressive strength of AAFS mortars with differernt slag content
Figure 42 demonstrates the effects from the addition of slag on the strength development of
AAFS mortars. As mentioned before, the strength development of AAFS mortars was facilitated
by the inclusion of SAP. However, it is revealed that the slag content also affects the strength
development of mortars. As shown in Figure 42, strength development in the early-age was
improved with the increase of slag content, which agrees with the findings observed by Nath and
Sarker (2014) [81]. For instance, M7 (30% slag replacement) showed the highest strength
development compared with M5 and M6 in the early age because of higher slag content,
resulting in additional calcium bearing compound in slag, and thus, facilitating the strength
development at early age.
59
Figure 42. Compressive strength development of AAFS mortars with differernt slag content
According to ACI 318M-05 (2005) [1], the 28-days compressive strength of concrete should be
at least 28 MPa for basic engineering application. Therefore, it can be concluded that all
designed AAFS mortars in this study are applicable for wide range of engineering usages. For
instance, the 28-days compressive strength of M0 reaches 57.213 MPa which is close to the
result reported by Zhao et al. (2007) [115], who claimed the 28-days compressive strength of
AAFS mortars with the same mix proportion as the present study, can reach up to 49 MPa.
Moreover, it is noted that the 28-days compressive strength of SAP mortar, such as M1 , M3 and
M7, are higher that of concrete made with OPC 43 at the same curing age. It reveals that the
mechanical properties of AAFS with SAP can be comparable to OPC concrete.
4.5. Autogenous Shrinkage
Figure 43 shows the autogenous shrinkage measurements of AAFS mortars with different SAP
content at the first 48 hours after casting. It is realised that the growth of autogenous shrinkage
for all specimens exhibits a similar trend but with different magnitude, they all had rapid
development of shrinkage in the first two hours. Mortar without SAP (M0) exhibited the greatest
amount of autogenous shrinkage. The ultimate autogenous shrinkage of M0, M1, M2, M3 and
M4 were approximately 3400 x 10-6, 3000 x 10-6, 2200 x 10-6, 1830 x 10-6 and 1800 x 10-6
60
respectively, which shows autogenous shrinkage is considerably reduced when more SAP is
added. Song et al. (2016) [104] who investigated the internal curing effect of SAP on AAS
mortars, has the same observation as the present study. The lower autogenous shrinkage by
addition of SAP can be attributed to the additional water available to compensate the water loss
during hydration, which could sustain the saturation within pores, and thus, reducing internal
pressure and autogenous shrinkage.
Moreover, it is can be seen that the reduction of autogenous shrinkage was not linearly
proportional to the increment of SAP content from 0% to 0.5%. Comparing all samples, the
effect of 0.3% SAP content is said to have the most significant reduction of autogenous
shrinkage in which the shrinkage is reduced by 26.67% than that of M1 (0.2% SAP content). It
can be concluded that internal curing effect from SAP could mitigate autogenous shrinkage of
AAFS.
Figure 43. Autogenous shinakge of AAFS mortars with differernt SAP content
Figure 44 reveals the autogenous shrinkage of AAFS mortars with different amount of slag
ranges between 15% to 30% at the first 48 hours after casting. Comparing with mixtures in series
‘S’, the autogenous shrinkages development of M5, M6, M2 and M7 are having similar trends.
61
For 15% to 30% slag content, the ultimate autogenous shrinkage was between approximately
1300 x 10-6 and 2100 x 10-6 . The higher slag content the greater is autogenous shrinkage. This
can be attributed to the densification of the microstructure by the addition of slag, which is also
discussed in some previous studies (Ye and Radlińska, 2016; Hojati and Radlińska, 2017) [114],
[47]. The densification of microstructure results the increase of capillary pressure, causing higher
autogenous shrinkage. Furthermore, it can be seen that M6 (20% slag content) has the most
prominent effect, that the ultimate shrinkage was increased by 47.79% as compared to M5 (15%
slag content).
Figure 44. Autogenous shrinkage of AAFS mortars with differernt slag content
Moreover, autogenous shrinkage kinetics of AAFS mortars are influenced by the SAP and slag
content. According to Figure 43 and Figure 44, it is observed that the highest autogenous
shrinkage rate of M0 and M7 happens about 30 minutes after casting. Meanwhile, the highest
autogenous shrinkage rate of M5 occurs an hour after casting. As mentioned before, the degree
of reaction of AAFS mortars increased with the drop in SAP content or increase of slag content.
The kinetics of autogenous shrinkage showed a great relationship with chemical reaction of the
62
mixture. For instance, M0 which has no SAP content, exhibited the highest chemical shrinkage,
quickest setting, and thus achieving the highest autogenous shrinkage rate at the earliest.
When the slag content varies from 10% to 30%, the ultimate autogenous shrinkage of AAFS
mortars is between 1300 x 10 -6 and 2100 x 10-6 which is similar to the results reported by Fang et
al. (2018) [39] who examined the autogenous shrinkage of AAFS pastes without internal curing.
As the autogenous shrinkage data of M7 should be higher than that of M2, extra autogenous
shrinkage data will be collected in the future for better results. This error may be related to the
disturbance of apparatus during the record period.
4.6. Drying Shrinkage
The drying shrinkage is one of the crucial parameters which influence the structural properties
and durability of the material. As shown in Figure 45 and Figure 47, the change in length of all
specimens increases with curing ages. It revealed a similar trend for all specimens which the rate
of change is rapid at the early age, followed by an almost constant behaviour. In agreement with
a previous study by Lee et al. (2014) [66], most of the total drying shrinkage took place in the
first few days after casting, and the drying shrinkage differences between specimens with
different SAP and slag content also occurred during this period, as shown in Figure 45 and
Figure 47. Afterwards, the amount of drying shrinkage for all specimens was almost identical.
Figure 45 and Figure 46 show the drying shrinkage and change in mass of AAFS mortars
respectively when the SAP content varies from 0% to 0.5%. It is observed that drying shrinkage
decreases with the increase of SAP content, which corresponds with the results shown in
autogenous shrinkage. With the SAP content from 0% to 0.5%, the ultimate drying shrinkage
decreases from 1.11% to 0.71%. This illustrates that the addition of SAP to AAFS mortars could
better improve the shrinkage of AAFS mortar. Furthermore, M2 (SAP content of 0.3 %) shows
the most significant reduction in volume change as compared to other specimens, that the
ultimate drying shrinkage of M2 is 0.2 % lower than that of M1. Figure 46 shows a rapid change
63
of mass in the early age, followed by a gradual increase afterwards, which is a similar trend as
the drying shrinkage results and coincides with the degree of volume reduction of the AAFS
mortars. For instance, M0 experienced the highest ultimate drying shrinkage, also had the highest
mass change in overall. The decrement of shrinkage and mass loss from the variation of SAP
content are very similar, as shown in Figure 45 and Figure 46. The change in mass varies from
8.70% to 6.70% with the increase of SAP content from 0% to 0.5%.
Figure 45. Drying shrinkage of AAFS mortars with differernt SAP content
Figure 46. Change in mass of AAFS mortars with differernt SAP content
64
Figure 47 and Figure 48 show the drying shrinkage and change in mass of AAFS mortars with
different amount of slag respectively. The ultimate drying shrinkage of M5, M6, M2 and M7, are
in the ascending order, from 0.63% to 0.98%, which reveals that the drying shrinkage rises with
the increase of slag content, in agreement with a previous study by Lee et al. (2014) [66]. AAFS
mortars with higher slag content are experiencing greater degree of drying shrinkage; this may be
related to the higher mesopore volume. According to Collins and Sanjayan (2000) [24] and Jiang
et al. (2005) [58], higher volume of mesopores would lead to higher drying shrinkage due to
higher capillary pressure induced by the meniscus developed in the pores. As shown in Figure
47, the effect of 30% slag content appeared to be more significant as compared to other
specimens. On the other hand, the mass change of mortars increased from 6.20% to 7.90% when
the slag content increases from 15% to 30% which follows a similar trend as drying shrinkage
results as shown in Figure 47.
Figure 47. Drying shrinkage of AAFS mortars with differernt slag content
65
Figure 48. Change in mass of AAFS mortars with differernt slag content
In the present study, the ultimate change in mass of M6 (20% slag content) is approximately 7%,
as shown in Figure 48. Considering the results reported by Lee et al. (2014) [66], who studied the
drying shrinkage of AAFS pastes, MS20 which has no SAP content but the same FA/GGBS
ratio, had a similar ultimate drying shrinkage and change in mass to M6. The ultimate shrinkage
of M6 does not lower than that of MS20 because the concentration of alkaline solution is higher
in the present study, as high alkaline activator concentration would cause higher shrinkages (Lee
et al. 2014) [66].
As shown in Figure 49, obvious curvature was observed for some samples, which includes M0
sample 3, M3 sample 1 and M6 sample 1. As the change in linear measurement no longer only
involves longitudinal displacement, this has a minor effect on the corresponding drying
shrinkage measurements. The curvature of samples may be related to the assemble of drying
shrinkage moulds which create differential contraction within the samples.
66
Figure 49. Samples with curvature
4.7. Internal Relative Humidity (IRH)
The IRH of AAFS mortars with different SAP content and slag content are shown in Figure 50
and Figure 51 respectively. A general development trend of IRH was found for all mixtures that
in the first two hours, there is a rapid increase in the IRH followed by a gradual increase.
Moreover, it is noted that the IRH of AAFS mortars would not decrease during early age
autogenous shrinkage.
Figure 50 shows the variation of IRH in the samples over time when different dosage of SAP
was added. It is observed that the IRH of specimens increases with the rise of SAP content,
which is due to the internal curing effect by SAP. This outcome is in line with the findings of
Song et al. (2016) [104]. M0 which has no SAP content exhibits much lower IRH compared to
other mixtures which contain SAP. The IRH of M0, M1, M2, M3 and M4 were 90.50%, 92.53%,
92.62%, 92.80% and 92.96%, respectively, which in turns indicate that the increase of SAP
content could sustain and even promote the moisture within mixtures. The IRH of M1 to M4 was
sustained at approximately 92.70%, which indicating that self-desiccation in the specimens was
considerably reduced. It is concluded that SAP can effectively supplement the moisture loss of
the specimens at early ages, which is in agreement with the observation made by previous studies
(Craeye et al., 2011; Snoeck et al. 2015) [27], [99].
67
Figure 50. IRH of AAFS mortars with different SAP content
Figure 51 shows the variations of IRH in the specimens over time when different slag
replacement level was incorporated. As shown in the figure, the IRH of the mixtures drops with
the rise of slag content, which can be attributed to the accelerated hydration, resulting in the
decrease of IRH. The IRH of M5, M6, M2 and M7 were 94.52%, 94.49%, 92.62% and 91.39%,
respectively. In particular, M7 exhibited the most significant effect of slag on the decrease of
IRH. It is noted that although M7 has the slag replacement level of 30%, the IRH of M7 is about
0.90% higher than that of M0, which verifies the influence of internal curing. Such difference is
also consistent with the drying shrinkage and autogenous shrinkage results of M0 and M7 as
shown in Figure 43, Figure 44, Figure 45 and Figure 47 respectively.
68
Figure 51. IRH of AAFS mortars with different slag content
Moreover, mixture FS20 (20% slag replacement level) in a previous study by Fang et al. (2018)
[39] and M6 in the present study, are the two mixtures with the same mix proportions and
alkaline activator. The only difference between them is the presence of SAP. It can be seen that
the IRH of M6 is about 94.490%, which is higher than that of FS20, which has the IRH of 86%.
This further verifies the effectiveness of internal curing on AAFS mortars.
4.8. Relationship between Autogenous Shrinkage, Pore Structure and IRH
IRH is a dominant factor in autogenous shrinkage. Water is gradually consumed during
continuous hydration, resulting in gradual decrease in IRH. When more water is consumed, the
saturation of moisture in the pores reduces, and many pores are formed in the specimen.
Eventually, the internal pressure starts to build up, causing autogenous shrinkage.
In the present study, when the IRH in the mixtures drops, the absorbed water in SAP is gradually
released into the matrix to compensate the water consumption due to hydration. As a result, the
IRH within the mixture can be maintained at a high level. In other words, the saturation of water
in capillary pores are maintained, and the internal pressure will be low. According to the
69
autogenous shrinkage and IRH results in as shown in Figure 43 and Figure 50, respectively, it is
proven that the addition of SAP can suppresses self-desiccation and autogenous shrinkage can be
effectively reduced. It can be seen that the results of autogenous shrinkage were consistent with
the results of IRH. For instance, M0 which has no SAP content, exhibits the lowest IRH and the
highest degree of autogenous shrinkage, while M4 which has the highest SAP content, is having
the highest IRH and lowest autogenous shrinkage. This is because when more SAP is added,
more water is available to compensate for the water loss due to hydration.
On the other hand, the increase of slag content could accelerate hydration, where water
consumption is more significant, causing low saturation in pores (i.e. lower IRH), higher internal
pressure and thus, greater autogenous shrinkage. This is evidenced according to the autogenous
shrinkage and IRH results, as shown in Figure 44 and Figure 51 respectively.
5. CONCLUSION
5.1. Concluding Remarks
The present study evaluated the effect of internal curing by SAP on mitigating shrinkages of
AAFS mortar. A series of AAFS samples incorporating different dosage of SAP and FA/GGBS
ratio were prepared and their fresh and hardened properties, IRH, drying shrinkage, autogenous
shrinkage were investigated. By varying the SAPs content, i.e. 0%, 0.2%, 0.3%, 0.4% and 0.5%,
the effect of internal curing by SAP was evaluated and compared. Through the examinations of
four different slag replacement level, i.e. 15%, 20%, 25% and 30%, the effect of slag content
were also evaluated. The main conclusions of this study are summarised as follows:
1. Workability, setting time and compressive strength of AAFS mortar were significantly
affected by the SAP and slag content. Higher SAP content increased the workability and
setting time, but reduced the compressive strength of AAFS mortar. On the other hand,
higher slag content improved compressive strength but caused rapid setting and low
workability.
70
2. In general, the compressive strength of AAFS mortars is comparable to concrete
produced with OPC. With an increase of SAPs dosage, the strength of specimens
decreased. However, it was realised that the rate strength development in the early-age
was more significant than the specimen without SAP. It is believed that the inclusion of
SAP improved the hydration of the specimens by releasing the absorbed water.
3. The relationship between UPV and compressive strength of AAFS mortar with internal
curing was identified, however, the relationship may not be adequate due to the wide
spread of UPV results.
4. Regarding shrinkages, it was observed that AAFS mortars with higher slag content
experienced a higher degree of volume reduction in overall, including autogenous and
drying shrinkage. However, by examining AAFS mortars with different SAP content, it
can be concluded that the inclusion of SAP as an internal curing agent can significantly
reduce the shrinkages, and the internal curing effect becomes more significant with high
SAP content.
5. The effect of internal curing increased with the rise of SAP content. This sustains the
moisture within the specimens and promotes sustainable hydration process. However, as
the addition of SAP could negatively affect compressive strength, it is necessary to
consider such benefit and limitation when determining the appropriate SAP content.
6. Internal curing reduces the drying shrinkage that the specimens experienced because it
sustains the moisture within the specimens. This can be attributed to the water
supplement from SAP. Absorbed water from SAP is released into the matrix to
compensate for the water loss due to evaporation.
71
7. Autogenous shrinkage, chemical shrinkage, degree of hydration, setting time, IRH and
pore structure are closely related. The inclusion of internal curing retards chemical
reactions, resulting less water consumption during hydration process, while promotes the
saturation of water within pores (i.e. IRH), which helps to reduce the internal pressure,
thus, reduce the autogenous shrinkage.
5.2. Future work
Due to time limitation, only one set of autogenous shrinkage data was collected for each mixture
in this study. More autogenous shrinkage data will be further collected in the future to ensure a
more characterisation of shrinkage behaviour. Regarding the issue with M2 day-28 compressive
strength, extra samples have already been prepared, and they will be tested in the future to
provide better results. Furthermore, properties of cement-based materials, such as concretes and
mortars, are highly connected to their pore structure which includes pore size, connectivity and
porosity and so on. Moreover, it is noted that the SAP content, binder composition and curing
age could directly affect the resultant air voids sizes and distribution in mortars. Therefore,
representative pieces of specimens were collected to carry out further microstructure analysis in
the future to evaluate how internal curing affects the pore structure of AAFS mortars using SEM
and MIP.
5.3. Prospectus
AAFS system is an exciting alternative for OPC which has a high potential to be further
developed and widely used in the future. This study evaluated the effect of internal curing and
the addition of slag on AAFS, and it can be concluded that internal curing could mitigate the
shrinkage of AAFS. It is believed that the use of internal curing could facilitate the application of
AAFS in the construction industry. Under the scope of mix proportion in the present study, it is
suggested that the slag replacement level of between 20 to 30% along with SAP content of 0.2%
could be the optimal proportion to produce AAFS mortar with decent engineering properties and
relatively low shrinkages.
72
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END
86
7. APPENDICES
7.1. Appendix A – Example of Mix Proportion Calculation – M1
- Binder
Unit weight of total binder = 400 kg/m3
With 25% slag replacement level, i.e. FA/GGBS = 75/25
Therefore, unit weight of FA = 400 kg/m3 x 75% = 300 kg/m3;

unit weight of GGBS = 400 kg/m3 x 25% = 100 kg/m3
- Alkali activator
As alkali activator occupies 40% of total binder
Therefore, unit weight of alkali activator = 400 kg/m3 x 40% = 160 kg/m3
As SS/SH = 2.0, i.e. SS:SH = 2:1
Therefore, unit weight of SS = 160 kg/m3 x 2/3 = 106.5 kg/m3

unit weight of SH = 160 kg/m3 x 1/3 = 53.5 kg/m3
- Fine aggregate
As sand-to-binder ratio is 2.0
Therefore, unit weight of sand = 400 kg/m3 x 2.0 = 800 kg/m3
- SPs
As SPs occupies 1% of total binder
Therefore, unit weight of SPs = 400 kg/m3 x 1% = 4 kg/m3
- SAPs
As SAPs occupies 0.2% of binder
Unit weight of SAP = 400 kg/m3 x 0.2% = 0.8 kg/m3
87
- Additional water
Unit weight of SAP = 0.8 kg/m3
As 12.5 gram of water is required per gram of SAP
Amount of additional water = 0.8 kg/m3 x 12.5 = 10 kg/m3
88

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UCL DEPARTMENT OF CIVIL, ENVIRONMENTAL &

MSc DISSERTATION SUBMISSION

Student Name: ____________LOK WAI YU AARON_________ (BLOCK CAPITALS)

Programme: ___________MSc Civil Engineering______________ (e.g. MSc GIS)

Supervisor: ___________Dr. Mingzhong Zhang__________________

Internal Curing of Cement Free Geopolymer Mortar Using Superabsorbent Polymer

• I have submitted an electronic copy of the project report through turnitin.

Signature: Lok Wai Yu Aaron Date: 12th September 2018

Internal Curing of Cement Free Geopolymer Mortar Using

Submitted in partial fulfilment of requirement for the Degree of Master of

Department of Civil, Environmental and Geomatic Engineering

University College London (UCL)

12th September 2018

observations made on conventional concrete.

with less shrinkages.

I would like to express sincere appreciation to my project supervisor, Dr Mingzhong Zheng,

and obstacles throughout my research.

fascinated in. It is a great honour to work under his supervision.

and advice are influential throughout the project.

1.1. Background ………………….………………….……………………......………….11

2.1. Alkali-Activated (AA) Materials ………………….………………..………...….….17

3.1. Materials ………………….………………….………………………..…………….32

3.2. Mix Proportions ………………….………………….……………………...……….35

4. DISCUSSION AND RESULTS …………………………………………...….……………46

4.1. Workability ………………….………………….…………………...………...…….46

5.1. Concluding Remarks ………………….…………………...…………..……………70

7.1. Appendix A – Example of Mix Proportion Calculation – M1………………..…..…87

A-S-H Amorphous aluminosilicate gel

AL/B Alkaline activator to binder ratio

AAC Alkali-activated concrete

AAF Alkali-activated fly ash

AAFS Alkali-activated fly ash/ slag

AAS Alkali-activated slag

ASTM American Society for Testing and Materials

CaCO3 Calcium carbonate

CaO Calcium oxide

CO2 Carbon dioxide

C-S-H Calcium silicate hydrate gel

FRC Fibre reinforced composite

GGBS Ground granulated blast-furnace slag

IRH Internal relative humidity

LCA Life cycle analysis

LVDT Linear variable differential transformer

MIP Mercury Intrusion Porosimetry

Na2SiO3 Sodium silicate (water glass)

NaOH Sodium hydroxide powder

NWA Normal weight aggregate

OPC Ordinary Portland cement

PWLA Pre-wetted lightweight aggregate

SAP Superabsorbent polymer

SEM Scanning Electron Microscopy

SH Sodium hydroxide solution

SS Sodium silicate solution

SSD Saturated surface-dry

S/B Sand to binder ratio

UPV Ultrasonic pulse velocity

Figure 1 Fly Ash (FA) (Source: Lizmar, 2016) [70]

Ground Granulated Blast-furnace Slag (GGBS) (Source:

Five aspects of investigation of AAFS mortars involved in

Figure 4 Tests involved in the present study

Visual illustration of external curing (conventional Curing)

Figure 6 Microstructure of SAPs

SAP particles in dry condition (left) and after absorption of

Student Name: ____LOK WAI YU AARON_ (BLOCK CAPITALS)

Programme: _MSc Civil Engineering____ (e.g. MSc GIS)

Supervisor: _Dr. Mingzhong Zhang________