1 EFFECT OF REDUCED MIXING TIME ON FRESH, MECHANICAL AND

2 MICROSTRUCTURAL BEHAVIOR OF CLASS C FLY ASH BASED ALKALI

3 ACTIVATED PASTE, MORTAR AND CONCRETE
4
5
6 Md. Mashfiqul Islam, Corresponding Author
7 Graduate student, Department of Civil, Architectural & Environmental Engineering,
8 Missouri University of Science and Technology, 1401, N. Pine Street, Rolla, MO, USA;
9 Email: mashfiq@mst.edu
10
11 Ahmed A. Gheni
12 Postdoctoral Fellow, Department of Civil, Architectural & Environmental Engineering,
13 Missouri University of Science and Technology, 1401, N. Pine Street, Rolla, MO, USA;
14 Email: aagmr6@mst.edu
15
16 Mohamed A. ElGawady
17 Professor, Department of Civil, Architectural & Environmental Engineering,
18 Missouri University of Science and Technology, 1401, N. Pine Street, Rolla, MO, USA;
19 Email: elgawadym@mst.edu
20
21 AUTHOR CONTRIBUTION STATEMENT
22 The authors confirm contribution to the paper as follows: study conception and design: Md.
23 Mashfiqul Islam, Ahmed A. Gheni, Mohamed A. ElGawady; data collection: Md. Mashfiqul
24 Islam; analysis and interpretation of results: Md. Mashfiqul Islam, Mohamed A. ElGawady; draft
25 manuscript preparation: Md. Mashfiqul Islam, Ahmed A. Gheni, Mohamed A. ElGawady. All
26 authors reviewed the results and approved the final version of the manuscript.

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30 Word count: 4164 words text + (2 tables) x 250 words = 4,664 words
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32 Submission Date: Aug. 01, 2019
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 Islam, Gheni, ElGawady

1 ABSTRACT
2
3 In this paper, the effect of reduced mixing time on the fresh and mechanical properties of fly ash
4 based alkali activated pastes, mortar and concrete (AAP, AAM and AAC) specimens are critically
5 investigated. The specimens are prepared from five different sources of Class C fly ash (FA)
6 collected from five coal based power plant in Missouri State, USA, consists of different chemical
7 compositions and physical properties. The calcium oxide content of the FAs varied from 21-37%
8 by mass. In this study, varying mixing time from three to twelve minutes; three mixing procedures
9 and three different curing methods, e.g. ambient, oven and steam curing are employed to prepare
10 the specimens. Liquid alkaline activators were used to prepare the alkali activated specimens. The
11 activators used in this study are 10 M sodium hydroxide (SH) solution and sodium silicate (SS)
12 soluiton. The ratio of alkaline activators to FA and SS to SH was maintained 0.275 and 1.0 in the
13 mixes. The workability and the setting times are measured to determine the fresh properties. A
14 satisfactory level of workability and setting time as well as mechanical performance was achieved
15 employing MM-8 mixing procedure. The effect of reduced mixing time on microstructural
16 behaviors are explained by employing x-ray diffraction (XRD) spectroscopy, scanning electron
17 microscope (SEM) imaging and isothermal calorimeter analysis.
18
19 Keywords: Alkali activated concrete, alkali activated mortar, alkali activated pastes, geopolymer,
20 fly ash, class C fly ash, mixing time, microstructural behaviour.
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 Islam, Gheni, ElGawady

1 INTRODUCTION
2 To meet the demand of sustainable development of the human civilization, the popularity of fly ash
3 (FA) based alkali activated concrete (AAC) is increasing day by day in the construction industries
4 as the FA is a sustainable as well as eco-friendly green material which is available as a by-product
5 from the coal based power plants. Moreover, the use of AAC instead of conventional ordinary
6 Portland cement (OPC) are getting popular for their proven enhanced mechanical and durability
7 properties (Natali et al. 2011). Alkali activated materials or geopolymers are inorganic polymers
8 developed by decomposition of aluminoslicate precursors, such as, ground granulated
9 blast-furnace slag (GGBS) (Cheng and Chiu, 2003), red mud (Ke et al. 2015, Ye et al. 2016),
10 metakaolin (Wang et al. 2005), rice husk ash (He et al. 2013, Detphan and Chindaprasirt, 2009),
11 class F FA (Palomo et al. 1999, Okoye et al. 2015), and class C FA (Chindaprasirt et al. 2007,
12 Gomaa et al. 2018, Guo et al. 2010, Kotwal et al. 2015) using alkaline activators such as sodium or
13 potassium hydroxides producing Si4+ and Al3+ products. This is followed by polycondensation of
14 inorganic oxides by exothermic reaction (Davidovits 1991). The polycondensation includes
15 nucleation, oligomerization, and polymerization, which lead to aluminoslicate-based polymer
16 having three-dimensional structural system (Davidovits 1991, Zhuang et al 2016). One of the
17 relatively new applications for FA is AAC. Throughout this paper, AAC is used as a synonym for
18 FA based geopolymer concrete.
19
20 The mixing process of different ingredients of alkali activated (AA) system is still a lengthy and
21 complex process which require safety precaution from chemical hazard and highly skilled and
22 experienced worker, to be applied practically at the construction yard maintaining the desirable
23 fresh properties to achieve expected mechanical performances. The mixing processes of AA
24 materials could be difficult for general contractors and construction companies who have a long
25 experience to work with OPC for producing concrete. In addition, dealing with hazardous
26 chemicals (liquid alkali activators) is not an easy task if the mixing process is complicated to
27 conduct in the construction yard repetitively. Previous researchers have produced geopolymer
28 mortars with a mixing time of seven to twenty minutes in three to five mixing steps and achieved
29 20 to 40 MPa by ambient curing and 40 to 80 MPa by curing at an elevated temperature (Hardjito
30 and Rangan, 2005; Chindaprasirt et al. 2012; Rattanasak and Chindaprasirt, 2009; Kotwal et al.
31 2015, Sargon et al. 2018, Gomaa et al. 2018). The promotion of the sustainable AA technology
32 over the traditional OPC is only possible when researchers can offer a comparatively simpler
33 mixing process in a shorter time. To this end, this current study investigates the effect of reduced
34 mixing time, curing methods and mixing processes on the fresh, mechanical and microstructural
35 behavior of alkali activated pastes, mortars and concrete from Class C FA consists of high calcium
36 oxide (CaO) content. The fresh properties are evaluated by workability and setting time. The
37 mechanical properties are investigated by compressive strength test of AAM and AAC specimens,
38 splitting tensile strength and flexural strength test of AAC specimens. The fresh and mechanical
39 behavior are explained by employing x-ray diffraction (XRD) spectroscopy, scanning electron
40 microscope (SEM) imaging and isothermal calorimeter analysis of AAP samples.
41
42 EXPERIMENTAL PROGRAM
43 This work investigates the effects of mixing time and procedure on the fresh and mechanical
44 properties of alkali activated mortar (AAM) and alkali activated concrete (AAC). AAP samples
45 are also prepared for microstructural analysis. Five class C FAs sourced from Labadie, Jeffery
46 Energy Center, Kansas City, Thomas Hill, and Sikeston power plants were used to synthesized
47 AAM mixtures. Hereinafter, the different FAs will be called FA37, FA29, FA26, FA24, and FA21,

3
 Islam, Gheni, ElGawady

1 respectively, refereeing to the CaO content in the FA precursor used in in study. The objective of
2 this study is to investigate and explain the effects of reduced mixing time on fresh and mechanical
3 performance of AA products. The nomenclature of fly ash, AAP, AAM and AAC specimens
4 consisted the letter FA, P, M and C respectively followed by a two-digit integer representing the
5 the calcium oxide (CaO) content of the respective FA.
6
7 Material properties
8 All the FAs used in this study were categorized as class C FA per the ASTM C618 (2019). The
9 surface area (BET) of the FA37, FA29, FA26, FA24, and FA21 (Figure 1a) were 2560, 3925, 1406,
10 2858, and 2921 m2/kg, respectively, and the specific gravity of these FAs were 2.97, 2.89, 2.70,
11 2.89, and 2.82, respectively. The chemical compositions of each FA are presented in Table 1. Oven
12 dry Missouri river sand with specific gravity of 2.7 passing through sieve #8 was used to prepare
13 the mortar mixtures. Liquid sodium hydroxide (SH) and sodium silicate (SS) were used as
14 activators. The concentration of the SH was 10 M and the amount of Na 2SiO3 in SS solution was
15 43.5% (w/w) while the water content was 56.5% (w/w).
16
17
18 Mix design, procedures, and time
19 The AAM mixes used sand-to-binder ratio (sand/FA) of 2.75, alkali activators-to-FA ratio
20 (Alk/FA) of 0.38, and SS/SH of 1.0 following the mix design by Gomaa et al. (2018). Mixing was
21 performed using a Hobart N50 mixer (Figure 1b). The ratio of water-to-FA (W/FA) was different
22 for different FAs to achieve the same workability for all mixtures used in this study. Table 2
23 presents the design of the different mixes used during this study.
24
25 Table 1 Chemical Composition of the Used FAs Determined by XRF Test
Chemical composition FA type
FA37 FA29 FA26 FA24 FA21
SiO2 (%) 36.9 37.9 42.3 40.4 43.9
Al2O3 (%) 13.9 17.4 17.9 17.5 20.1
Fe2O3 (%) 3.52 3.67 4.73 4.72 4.96
CaO (%) 36.9 28.8 25.9 24.1 21.2
MgO (%) 4.80 8.00 4.74 9.39 4.29
Na2O (%) 1.62 1.85 1.58 1.17 2.87
K2O (%) 0.62 0.39 0.56 0.48 0.70
TiO2 (%) 0.87 1.17 1.44 1.40 1.36
P2O5 (%) 0.70 0.71 0.89 0.79 0.51
MnO (%) 0.03 0.04 0.04 0.02 0.05
LOI (%) 0.50 0.82 0.12 0.62 0.40
MC (%) 0.07 0.02 0.04 0.10 0.01
26 Note: LOI= loss on ignition, MC= moisture content.
27
28 This study investigated three mixing procedures along with different mixing times ranged from
29 three to twelve minutes for preparing the AAM specimens. The first mixing procedure was the
30 mixing procedure developed by Gomaa et al. (2018) where the sand and FA were mixed for one
31 minute at a speed of 136 rpm in a Hobert mortar mixture. Then, water was added over one minute
32 and mixing continued, adding the liquid alkali activators over five minutes and mixing continued
33 with the same speed and then mixing continued for five more minutes at a speed of 281 rpm. The

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 Islam, Gheni, ElGawady

1 total mixing time was twelve minutes in four steps as well as two mixing speeds.The specimens
2 prepared following this procedure were considered as control specimens. To delay the reaction of
3 the FA with the alkaline activators, modified mixing (MM) procedure was introduced. During this
4 mixing procedure, water was added to the sand and mixed for one minute at a speed of 136 rpm,
5 followed by adding of alkali activators and mixing for one more minute. Finally, adding the FA and
6 mixing continued for one minute, three minutes, or six minutes for mixing procedures MM-3,
7 MM-5, and MM-8, respectively. Therefore, this approach utilized short mixing time and one
8 mixing speed. The third mixing procedure (ALL) included mixing all ingredients, i.e., water, alkali
9 activators, sand, and FA for one minute and the mixing continued upto five, or eight minutes for
10 ALL-5, and ALL-8 process, respectively, with a mixing speed of 136 rpm.
11
12 Table Error! No text of specified style in document.2 Mix design of mortar and concrete
Mix design AAP mix AAM mix AAC mix
parameters
and quantities FA37 FA21 FA37 FA29 FA26 FA24 FA21 FA37 FA21
Alk/FA 0.28 0.28 0.28 0.28 0.28 0.28 0.28 0.28 0.28
W/FA 0.39 0.38 0.39 0.38 0.34 0.38 0.38 0.39 0.38
SS/SH 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00
SH (kg/m3) 75 75 75 75 75 75 75 75 75
SS (kg/m3) 75 75 75 75 75 75 75 75 75
W (kg/m3) 120 114 120 114 91 114 114 131 131
FA (kg/m3) 541 541 541 541 541 541 541 541 541
Sand (kg/m3) - - 1487 1487 1487 1487 1487 935 935
CA (kg/m3) - - - - - - - 1122 1122
13 Note. Alk= alkaline activator, FA= fly ash, SS= sodium silicate, SH= sodium hydroxide, W= water, CA= coarse
14 aggregate.
15
16 For each mixture, the workability was measured using a flow table (Figure 1c) per ASTM C230
17 (2014). The initial and final setting times of the fresh mortar were measured also using a modified
18 Vicat needle having a diameter of 2 mm per ASTM C191 (2013). After mixing, the fresh AAM
19 was casted in 50 mm cube molds as per ASTM C109 (2016) (Figure 1d). Three curing regiems
20 were employed in this study for AAM samples: ambient curing at 23º+2ºC while the specimens
21 were within plastic bags for seven days, curing of the specimens in electrical ovens at 70ºC for 24
22 hours, and steam curing at 70ºC for 24 hours following Gomaa et al. (2018). For each mix, nine
23 specimens were prepared; three cubes for each curing systems. The compressive strengths of the
24 cubes were determined using a Tinius Olsen universal testing machine (UTM) and the average
25 compressive strength for each mixture and curing regiem was determined. To observe effect of
26 mixing time on the microstrucrual behaviour x-ray diffraction (XRD) spectroscopy and scanning
27 electron microscope (SEM) imaging was performed on alkali activated paste (AAP) samples from
28 FA37 and FA21 which has the highest and lowest CaO content respectively. The XRD analyses
29 were performed in PANalytical Multipurpose Diffractometer utilizing a Cu source and a PIXcel
30 detector and the diffraction patterns of the present crystalline phases in each sample reflected in the
31 form of sharp peaks appearing at different 2Ɵ locations were determined and analyzed. The SEM
32 imaging were performed in Hitachi S-4700 Field Emission Scanning Electron Microscope. The
33 change in the heat of hydration temperature of AAP samples were also investigated using the
34 Humboldt Digital Cement Calorimeter (isothermal) to better understand the effect of mixing time
35 on hydration reaction and geopolymerization. The AAC samples of 100 mm x 200 mm cylinder
36 and 90 mm x 90 mm 270 mm beams were also prepared for compressive strength, splitting tensile

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 Islam, Gheni, ElGawady

1 strength, and flexural strength evaluation using FA37 and FA21 employing steam curing for 24
2 hours and compared the results with AAC prepared by Gomaa et al. (2018).
3

(a) (b)

(c) (d)

(e) (f)

(g) (h)
4 Figure 1. (a) Different types of FA used in this study, (b) mixing of AAM in Hobart mortar mixture,
5 (c) workability testing of AAM, (d) AAM cube specimens, (e) AAC samples, (f) compression test
6 of AAC cylinder, (g) splitting tensile test of ACC, (h) flexural strength test of AAC.

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 Islam, Gheni, ElGawady

1
2 RESULTS AND DISCUSSION
3 Effect of mixing time and mixing procedure on workability of AAM
4 There is no minimum workability requirements for mortar per ASTM but it is a common practice
5 to consider a minimum workability of 40% as a good workability. The effect of mixing time on the
6 workability of AAM mixed following MM and ALL procedures are shown in Figure 2(a) and
7 Figure 2(b), respectively. Also the workability for AAM mixed using Gomaa et al. (2018)
8 procedure shown in the figures. As shown in Figure 2(a), the workability increased with increasing
9 the mixing time up to five to eight minutes depending on the used FA; that was followed by
10 reduced workability. MM-5 and MM-8 generally showed higher workability compared to Gomaa
11 et al. (2018)’s mixing procedure except for M26.
12
13 For ALL mixing procedure, increasing the mixing time from five to eight minutes generally
14 decreased the workability except for M21. Furthermore, the workability of all mixtures mixed
15 using ALL-5 except M21 displayed workability at least equivalent to those displayed by the
16 counterpart mixtures mixed using Gomaa et al. 2018’s procedure. Therefore, using MM-5, MM-8,
17 ALL-5, and ALL-8 it is possible to reduce the mixing time from twelve minutes to five to eight
18 minutes while displaying better workability. This is a significant cut ranging from 33% to 58% in
19 the mixing time which would significantly increase the AAC productivity and reducing its
20 production cost.
21
150 150
M37 R² = 0.974 M37
M29 M29
120 M26 120 M26 R² = 1
M24 M24 R² = 1
Workability (%)
Workability (%)

M21 R² = 0.870 M21

90 90
R² = 1
R² = 0.763
60 60
R² = 1
R² = 0.948
30 30 R² = 1
R² = 0.995
Gomaa et al. (2018) Gomaa et al. (2018)
0 0
2 3 4 5 6 7 8 9 10 11 12 13 4 5 6 7 8 9 10 11 12 13
Mixing time (minute) Mixing time (minute)
(a) (b)
22 Figure 2. Effect of mixing time on the workability of AAM mixed using: (a) MM, and (b) ALL
23 procedures (Note. Results from Gomaa et al. 2018 mixing procedure are shown for comparison
24 purpose).
25
26 Effect of mixing procedures on setting time of AAM
27 All mixtures prepared using MM-8 initial and final setting times similar to those of mixtures
28 prepared using Gomaa et al. (2008)’s mixing procedure (Figure 3). However, mixtures prepared
29 using MM-3 and MM-5 displayed lower initial and final setting times. The short mixing time led
30 to non-uniform mixing and agglomeration of particles and hence rapid setting. Furthermore,
31 mixtures prepared using ALL-5 and ALL-8 displayed lower initial and final setting
32 timescompared to those prepared using Gomaa et al. 2018’s mixing procedure (Figure 4).
33 Dollimore and Mangabhai (1985) proved that increasing mixing time of OPC paste, the induction
34 period decreases along with the increase of heat evolution and hydration reaction. Similar

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 Islam, Gheni, ElGawady

1 hydration reaction occurs in the AAM mixes (Chindaprasirt et al. 2007) prepared from FA with
2 high CaO content (specially class C FA) which also hinder the geopolymerization reaction. Hence
3 the longer mixing time increase the hydration reaction and reduce geopolymerization process and
4 as a results setting time increases. Careful examination of the effects of mixing time and procedure
5 on the setting times of each mixture (Figures 3 and 4) showed that MM-8 displayed equal or longer
6 setting times than mixtures prepare using using Gomaa et al. (2018)’s mixing procedure except for
7 M26.
450 450
M21 M21 R² = 0.855
400 M24 400 M24
R² = 0.998

Final etting time (minute)

Initial setting time (minute)

350 M26 350 M26 R² = 0.846

300 M29 300 M29
M37 R² = 1 M37 R² = 0.822
250 250
200 R² = 0.765 200
R² = 0.997
150 150
R² = 0.994 R² = 0.996
100 100
R² = 0.486
50 50 Gomaa et al. (2018)
Gomaa et al. (2018)
0 0
2 3 4 5 6 7 8 9 10 11 12 13 2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes) Mixing time (minutes)

(a) (b)
8 Figure 3. Effect of mixing time on initial (I) and final (F) setting times of AAM mixed using MM
9 procedure: (a) M21, (b) M24, (c) M26, (d) M29, and (e) M37 (Note. Results from Gomaa et al.
10 2018 mixing procedure are shown for comparison purpose).
11
450 450
M21 M21 Gomaa et al. (2018)
400 Gomaa et al. (2018) 400 M24
M24
Initial setting time (minute)

Final setting time (minute)

350 M26 350 M26

R² = 1
300 M29 300 M29
R² = 1 M37
M37 R² = 1
250 250
200 R² = 1 200
150 150
R² = 1 R² = 1
100 100
50 R² = 1 50 R² = 1 R² = 1
R² = 1
0 0
2 3 4 5 6 7 8 9 10 11 12 13 2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes) Mixing time (minutes)

(a) (b)
12 Figure 4. Effect of mixing time on initial (I) and final (F) setting times of AAM mixed using ALL
13 procedure: (a) M21, (b) M24, (c) M26, (d) M29, and (e) M37 (Note. Results from Gomaa et al.
14 2018 mixing procedure are shown for comparison purpose).
15
16 Effect of mixing time and procedure on compressive strength of AAM
17 Figure 5 presents the effect of mixing time on the compressive strength of AAM specimens
18 prepared using MM procedure and Gomaa et al.(2018) as a reference mixing procedure. It is
19 observed from Figure 5 that, in the case of AAM synthesized using FAs having lower CaO content,
20 i.e., FA21 and FA24, the compressive strength decreased with increasing the mixing time. In case
21 of high CaO content, i.e., FA37, the compressive strength of the ambient cured specimen increased
22 with increasing the mixing time. In the case of ALL mixing procedure (Figure 6), similar response
23 was also observed. Furthermore, specimens prepared using the MM-8 procedure displayed
24 approximately equal or higher compressive strengths compared to those prepared using Gomaa et

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 Islam, Gheni, ElGawady

1 al. (2018). It is worth noting that with increasing the mixing time of ordinary Portland cement
2 paste, the induction period decreases with increasing the hydration reaction which contributes to
3 the strength gain of cement (Dollimore and Mangabhai, 1985). Similar hydration process occurs
4 also in the AAM synthesized using high CaO content FA. This was the reason that AAM
5 synthesized using FA37 displayed lower compressive strength when mixed for a short period.
6
70 70
Ambient curing Oven curing
Compressive strength (MPa)

Compressive strength (MPa)

60 60
R² = 0.596 R² = 0.437 R² = 0.954 R² = 0.979
50 50

40 40 R² = 0.968
R² = 0.932 R² = 0.966
R² = 0.951 30
30
R² = 0.438
20 M37 20 M37
M29 R² = 0.933 M29
M26 M26
10 M24 10 M24
Gomaa et al. (2018) M21 Gomaa et al. (2018)
M21
0 0
2 3 4 5 6 7 8 9 10 11 12 13 2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes) Mixing time (minutes)
(a) (b)
70
R² = 0.697 Steam curing
R² = 0.289
Compressive strength (MPa)

60 R² = 0.928
50
R² = 0.989
40 R² = 0.826
30

20 M37
M29 Gomaa et al. (2018)
M26
10 M24
M21
0
2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes)
(c)
Figure 5. Effect of mixing time onthecompressive strength of AAM prepared by MM
procedure and Gomaa et al. (2018): (a) FA21, (b) FA24, (c) FA26, (d) FA29, and (e) FA37
(Note. Results from Gomaa et al. 2018 mixing procedure are shown for comparison purpose).
7

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 Islam, Gheni, ElGawady

70 70
Ambient curing Oven curing

Compressive strength (MPa)

Compressive strength (MPa) 60 60
R² = 1
R² = 1
50 R² = 1 50 R² = 1
R² = 1
40 R² = 1 40

30 R² = 1 30 R² = 1 R² = 1
M37 20 M37
20 R² = 1 M29
M29
M26 M26
10 10 M24
M24 Gomaa et al. (2018) Gomaa et al. (2018)
M21 M21
0 0
2 3 4 5 6 7 8 9 10 11 12 13 2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes) Mixing time (minutes)
(a) (b)
70
R² = 1 R² = 1
R² = 1
Compressive strength (MPa)

60
R² = 1
50

40 R² = 1

30

20 M37
M29 Gomaa et al. (2018)
M26
10 M24
M21 Steam curing
0
2 3 4 5 6 7 8 9 10 11 12 13
Mixing time (minutes)
(c)
Figure 6. Effect of mixing time on the compressive strength of AAM prepared by ALL procedures
and Gomaa et al. (2018) procedure using different FAs (a) C21, (b) C24, (c) C26, (d) C29, and (e)
C37. (Note. Results from Gomaa et al. 2018 mixing procedure are shown for comparison purpose).
1
2 Effect of mixing time on microstructural behavior of AAP
3 Figure 7a and 7b shows the XRD pattern of the P37 and P21 samples prepared with varying
4 mixing time. The peak of quartz at 26°-2Ɵ was found smaller for both AAP samples prepared by
5 12 minutes mixing time and larger peak is seen for AAP samples for three minutes mixing time
6 and also for unreacted FA samples. This phenomenon indicates that higher dissolution of FA
7 crystalline phases occurs with longer mixing time. Again, as explained by Dollimore and
8 Mangabhai (1985), longer mixing time of AAP shows higher hydration reaction as OPC as seen in
9 Figure 8a and 8b. Figure 8a and 8b present the change of temperature with time for AAP mixes
10 prepared in varying mixing times employing MM and Gomaa et at. (2018) procedures and
11 measured in Humboldt Digital Cement Calorimeter (isothermal). The AAP mixes are prepared
12 outside the calorimeter so AAP prepared in twelve minute mixing time showed lower peak in
13 temperature-time curve, but in case of the temperature loss with time (as geopolymerization is a
14 endothermic reaction), i.e. the post peak slope of the temperature-time curve is lower compared to
15 the response of other mixing times which indicate the event of hydration reaction in the both
16 mixes. The post peak slope temperature-time curve of the AAP samples prepared in three minute
17 mixing time is the steepest which indicate the rapid ending of hydration reaction as described by

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 Islam, Gheni, ElGawady

1 Dollimore and Mangabhai (1985). As stated above, the hydration reaction is a hinder for the
2 geopolymerization process so AAM samples prepared in eight minutes mixing time showed
3 higher workability as well as compressive strength compared to Gomaa et al. (2018) in which the
4 mixing time is twelve minutes. For other other lower mixing times the reduction in strength was
5 due to non-uniform mixing and less dissolution of FA particles.
6
7 Figure 9 shows the SEM micrographs of un-reacted FA and AAP samples prepared in different
8 mixing time. There are a lot of un-reacted FA particles are seen in the SEM micrographs of the
9 AAP mixes prepared in three minutes (Figure 9b) and five minutes (Figure 9c) which indicate the
10 non-uniform mixing, weak microstructural bonding as well as lower compressive strength. In case
11 of the AAP samples prepared in eight minutes (Figure 9d) showed no un-reacted FA particle and a
12 lot of formed products of hydration and geopolymerization process which ensures higher
13 molecular packing and higher compressive strength. The AAP sample prepared in twelve minutes
14 (Figure 9e) shows no un-reacted particles but fewer formed products compared to AAP misex in
15 eight minutes. The AAP and AAM eight minute mixing was found to have stronger microstructure
16 compared to the specimens prepared in higher and lower mixing time for these FA types.
17
18 Effect of mixing time on mechanical behavior of AAC
19 With the experience of above investigations, AAC samples are prepared using F37 and FA21
20 employing MM-8 and Gomaa et al. (2018). Mixing procedure and the effect of mixing time on
21 mechanical behaviors are evaluated. Figure 10 presents the fresh and mechanical properties of
22 AAC specimens prepared employing MM-8 and Gomaa et al. (2018) procedures. The slump of the
23 C37 prepared using MM-8 procedure was higher compared to respective Gomaa et al. (2018) but
24 the slump for C21 was slightly lower than Gomaa et al (2018). AAC samples prepared using
25 MM-8 procedure shower higher compressive, splitting tensile and flexural strength compared to
26 Gomaa et al.(2018) procedure except flexural strength for C21 specimen. This study reveals the
27 optimum eight minute mixing time for the AAP, AAM and AAC prepared using class C FA which
28 surely increase the productivity as well the reduce the complexity of AAC construction industry.
29
30
31
32
33
34

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 Islam, Gheni, ElGawady

Q Q T
C T C C CC C C
T T P37 (12 min)

P37 (8 min)

P37 (5 min)

P37 (3 min)

H
H
HH
H HH
2 FA37

0 10 20 30 40 50 60 70 80 90 100

(a)
T

Q T
Q T
C Q C CC Q C C T T P21 (12 min)

P21 (8 min)

P21 (5 min)

P21 (3 min)

H
H
2 H H FA21

0 10 20 30 40 50 60 70 80 90 100

(b)
1 Figure 7. XRD patterns of FA and AAP samples prepared using MM and Gomaa et al. (2018) procedures
2 (a) P37 and FA 37 (b) P21 and FA 21. (Note. Q= Quartz, C= calcium silicate hydrate (CSH), H= Hatrurite,
3 T= TiO2, reference material).
4

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 Islam, Gheni, ElGawady

32 32
P21 (3 min)
30 P37 (8 min) 30 P21 (8 min)
P21 (5 min)

Temperature (C)
P37 (5 min)
Temperature (C)

28 P37 (3 min) 28

26 26

24 P37 (12 min) 24 P21 (12 min)

22 22

20 20
0 4 8 12 16 20 24 0 4 8 12 16 20 24
Time (hours) Time (hours)
(a) (b)
1 Figure 8. Change of temperature in AAP mixes for different mixing time prepared using MM and
2 Gomaa et al. (2018) procedure (a) P37, (b) P21.
3
4

(a) (b) (c)

(d) (e)
5 Figure 9. SEM micrographs (a) un-reacted FA37, (b) P37 prepared in 3 minutes, (c) P37 prepared
6 in 5 minutes, (d) P37 prepared in 8 minutes and (e) P37 prepared in 12 minutes.
7

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 Islam, Gheni, ElGawady

300 100
Gomaa et al. (2018) MM-8 Gomaa et al. (2018) MM-8

Compressive strength (MPa)

250
210 203 75
200 191 191
Slump (mm)

51.0
50 45.9
150 41.4
34.5
100
25
50

0 0
C37 C21 C37 C21
FA type FA type
(a) (b)
10 10
Gomaa et al. (2018) MM-8 Gomaa et al. (2018) MM-8
Splitting tensile strength (MPa)

Flexural strength (MPa)

7.5 7.5

5 5 4.6 4.5
4.2
3.4 3.1 3.3 3.2
2.8
2.5 2.5

0 0
C37 C21 C37 C21
FA type FA type
(c)
1 Figure 10. Fresh and mechanical properties of AAC specimens from FA37 and FA21 (a) slump, (b)
2 compressive strength, (c) splitting tensile strength and (d) flexural strength.
3
4 CONCLUSIONS
5 This paper investigates the fresh, mechanical and microstructural properties of AAP, AAM and
6 AAC specimens prepared using three different mixing procedures. The workability of all mixtures
7 prepared using MM-8 displayed higher workability than those prepared using Gomaa et al. (2018)
8 mixing procedure. There exists a strong correlation between the workability, mechanical and
9 microstructural properties of AAP and AAM with mixing time and mixing procedure. This study
10 reveals the optimum mixing time for AA materials prepared from class C FA with CaO content
11 ranges from 21-37% . Higher mixing time as well as very short mixing time for class C FA AA
12 materials had shown lower fresh and mechanical properties. The XRD patterns, SEM micrographs
13 and temperature-time analysis from calorimeter reveal that there exists strong correlation between
14 mixing time and mocrostructural behavior of AA materials. The MM-8 mixing procedure and the
15 eight minutes of mixing time showed higher fresh and mechanical properties of AAP, AAM and
16 AAC specimens which is a significant cut ranging from 33% to 58% in the mixing time which
17 would significantly increase the AAC productivity and reducing its production cost in the AAC
18 construction industry for class C FA.
19
20
21
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