Construction and Building Materials 327 (2022) 126914

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Construction and Building Materials

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Influence of design parameters on engineering properties of angular shaped

fly ash aggregates
Hrishikesh A Shahane , Satyajit Patel *
Dept. of Civil Engineering, S. V. National Institute of Technology, Surat Gujarat 395007, India

A R T I C L E I N F O A B S T R A C T

Keywords: Fly ash of thermal power plants substitute’s construction materials and can help to preserve non-renewable
Fly ash aggregate resources. In the construction industry, more particularly in concrete and road construction, a huge quantity
Impact value of aggregate is being used. Fly ash aggregate is a unique alternative for the construction industry at present.
Crushing value
However, the properties of fly ash aggregate are mostly controlled by the type and dosage of additive used
Los Angeles abrasion value
Soundness
besides the characteristics of ash and curing method adopted. In the present study, specimens from various
combinations of fly ash with hydrated lime, ground granulated blast furnace slag, and cement were prepared at
maximum dry unit weight with optimum moisture content and cured by hot water curing method. The cured
specimens were crushed to prepared angular shaped fly ash aggregates. The influence of the binding additives on
the unconfined compressive strength of mixes and aggregate impact value was studied. Measured engineering
properties were also analyzed through a micro-level study. The addition of lime enhanced the unconfined
compressive strength of mixes and impact value of aggregates, whereas, replacement of lime with the ground
granulated blast furnace slag and cement reduced the strength of the mixes. Unconfined compressive strength
value of mixes shows the inverse relationship with impact value of aggregate prepared from that mixes and a
correlation between unconfined compressive strength and aggregate impact value has been proposed. Moreover,
the effect of moisture content and pressing force on compressive strength and aggregate impact value was also
investigated on optimum mixes. From these experimentations, the optimum combinations of fly ash-additive
mixes, the optimum value for moisture content, and pressing force were chosen; and angular shaped fly ash
aggregates were produced by hot water curing method. Furthermore, the various physical properties, mechanical
properties and durability index of these fly ash aggregates are discussed and compared with the Indian standard
specifications. The leaching behavior of these aggregates was also examined in this study. The addition of lime
gives better results compared to cement and ground granulated blast furnace slag and use of lime seems to be
more cost-effective. Thus, these cold bonded fly ash aggregates with significant strength may find prospective use
in civil engineering construction sector.

1. Introduction
Disposal of fly ash represents an environmental issue, as about
70–80% of fly ash (FA) is being utilized in India [1]. On the other hand,
only around half of the FA produced worldwide is used [2]. The
remaining fly ash is either disposed of in an unrestrained manner or
landfilled. The approach of developing new eco-friendly and cost-
effective building materials that integrates numerous kinds of wastes
as a partial or full replacement of cement, sand, and aggregate has
gained considerable attention. The government of India is encouraging
the usage of fly ash in the manufacturing of building materials and
construction practices. The making of synthetic aggregates using fly ash
has a great potential for its large-scale consumption in the construction
field, and can resolve the disposal issue of fly ash and fulfill the
requirement of must desired stone aggregates in one effort. Aggregates
made from fly ash having sufficient mechanical strength can find
widespread applications in the manufacture of different building ma­
terials, concrete, construction of roads, and embankment by substituting
natural sand, gravel, and stone aggregates [3]. Also, it can be used for
filling low-lying areas, mines and as cover material for ash ponds to
protect from erosion and leaching of heavy metals [3].
For the manufacturing of fly ash aggregates, primarily, two types of

* Corresponding author.
E-mail addresses: shahane.hrishi@gmail.com (H.A. Shahane), spatel@amd.svnit.ac.in (S. Patel).

https://doi.org/10.1016/j.conbuildmat.2022.126914
Received 18 October 2021; Received in revised form 27 January 2022; Accepted 17 February 2022
Available online 23 February 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
H.A. Shahane and S. Patel
agglomeration techniques, namely, pelletization or granulations and
compaction are used for the consolidation of fly ash particles into larger
shapes. In the method of granulations agglomerates are shaped by
tumbling forces without any external compacting forces, and in the
method of compaction the desired density is achieved with external
compacting forces [4]. Whereas, for the hardening of these fly ash
granules cold bonding, autoclaving or sintering are the three approaches
commonly adopted [5].
Binder plays a vital role in the production of fly ash aggregates.
Initially, binders are used for the formation of feasible agglomerates in
the balling and pelletization processes. Required interparticle bonds of
finite strength to maintain the necessary structural integrity of the fly
ash pellets is developed through binders [4]. For the development of
these bonds, numerous binders have been tried by various researchers,
which includes bentonite, kaolinite, cement, lime, glass powder, clay,
etc. [5–11]. The use of mineral admixtures, for example, lime and
cement, exhibit excellent cost-effectiveness, however, appeared to be
incompatible if used for the higher temperature process as they disin­
tegrate during sintering [8,12]. Bentonite and kaolinite when used with
coarser fly ash, it improves the efficiency of pelletization [7]. Geetha and
Ramamurthy [13] also explain the use of low-calcium bottom ash by
adding clay binders.
In the cold bonding hardening method a reaction between additives
and fly ash takes place which forms calcium aluminosilicate hydrate (C-
A-S-H) and calcium-silicate hydrate (C-S-H) gel. Alkaline substances,
calcium sulfite, and calcium sulfate may have a constructive influence
on strength improvement [4]. Geetha and Ramamurthy [13] reported
that the formation of C-S-H gel through the pozzolanic reaction among
lime/cement, water, and bottom ash is responsible for the higher
strength of pellets at ambient temperature. Patel and Shahu [14] re­
ported that the quantity of C-A-S-H and C-S-H gels produced in the
pozzolanic reaction is the main controlling factor for strength gain of fly
ash-lime mixes. Walker [15] stated that the pellets or granules produced
with lime as a binder are much more resilient than those produced with
cement. Ramamurthy and Harikrishnan [5] concluded that the capa­
bility of fly ash to react with the binder, binder type, and dosage of
binder are the main governing aspects that influence the properties of
cold bonded fly ash aggregate. The mechanical strength of granules
made with bottom ash of incinerated municipal solid waste strongly
reliant on the type of binder [16].
Using a different combination of fly ash-additive mixes various re­
searchers have developed fly ash aggregates and its physical and me­
chanical properties are reported in the literature [12,17–23]. The
drawbacks of the above processes consist of use more energy, time-
consuming and complicated procedure to make the aggregates from
the mixture of fly ash and various additives, resulting in non-use of these
aggregates on a large scale in civil engineering applications [24–25]. An
innovative and economical four step process for the production of
angular shaped fly ash aggregates has been developed and discussed in
the patent by Patel and Shahane [24]. The effect of various curing
methods on strength development of fly ash-lime mix was investigated
by Shahane and Patel [25] and hot water curing method has been pro­
posed to be the most effective and economical process for hardening of
the fly ash-lime mix. However, a detailed study of various design pa­
rameters influencing the engineering properties of angular shaped fly
ash aggregates has not been reported yet. Consequently, the objectives
of the present paper are as follows:
1. To study the influence of additives on the unconfined compressive
strength (UCS) of fly ash-additives mixes and impact value of
aggregate produced by hot water curing method.
2. To develop the optimum combination of the fly ash-additive mix for
different types of fly ash, so that fly ash aggregate does not require
expensive additives or complicated formulations.
2
Construction and Building Materials 327 (2022) 126914
3. To investigate the influence of moisture content and pressing force
on the compressive strength of fly ash block and aggregate impact
value.
4. To study the engineering properties of angular shaped fly ash ag­
gregates that can be used as a replacement of natural aggregates.
In the present work, suitable additives, namely, hydrated lime,
ground granulated blast furnace slag (GGBS), and cement have been
added to fly ash at different proportions. A sequence of unconfined
compression tests and aggregate impact value tests were performed to
investigate the effect of additives on the strength and toughness of
different fly ash-additive mixes. Experimental test outcomes are also
described using the result of X-ray diffraction (XRD) and scanning
electron microscope (SEM) tests. The equation for the prediction of
aggregate impact value through unconfined compressive strength (UCS)
of fly ash-additive mixes is developed and presented in this paper. Be­
sides, the effect of moisture content and pressing force on the strength of
selected mixes and impact value of aggregates was also studied. Based
on these results, an optimum value of the fly ash-additive mix pro­
portions, moisture content, and pressing force were chosen for different
fly ashes, and various physical and mechanical properties of aggregates
made with these mixes are evaluated and correlated with standard
specifications.
2. Materials and mix proportion
Fly ashes are collected from Reliance Industries Limited, Surat,
Gujarat, India and Gujarat Industries Power Company Ltd., Surat,
Gujarat, India, respectively. The physical properties of the fly ashes are
given in Table 1. Based on the chemical compositions (Table 2), Fly ash-
1 is categorized as ‘Class F’ whereas Fly ash-2 is categorized as ‘Class C’
[26]. Commercially available hydrated lime (L), GGBS (G), and ordinary
Portland cement of 53 grade (C) were used as an additive throughout the
study.
Binding additives such as lime, GGBS, and cement are the sources of
calcium. In pozzolanic reaction, these calcium ions react with silica, and
alumina existing in fly ash to produce cementitious gel leading to the
strength development in the mixes. GGBS is cheaper than lime; there­
fore, in this study lime has been replaced with GGBS. Table 3 shows the
detailed description of fly ash-additives mixes tested in this study.
2.1. Laboratory tests
Initially, modified Proctor compaction tests were executed as per IS
2720 Part-VIII [27] on all fly ash-additive mixes to study the compaction
behavior of fly ashes. Next, cylinder-shaped samples of 50 mm diameter
and 100 mm height were prepared at a dry unit weight equal to the
maximum dry unit weight of the mix obtained from the compaction test.
Immediately after compaction, the samples were cured as per hot water
curing method and UCS tests were conducted on the specimens as per IS
4332 Part-V [28]. The detailed study of hot water curing method i.e.,
curing time and curing temperature has been carried out by Shahane
and Patel [25] and same has been adopted in the present study to attain
Table 1
Physical property of fly ashes.
Physical Parameters F1 F2
Color Grey Light Brown
Specific Gravity 1.28 1.64
Grain Size Distribution
0.425 mm to 2.0 mm – –
0.075–0.425 mm 9.0 12.0
less than 0.075 mm 91.0 88.0
Coefficient of uniformity (Cu) 5.79 6.00
Coefficient of curvature (Cc) 1.41 2.67
IS classification ML ML
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

Table 2
Chemical Composition of the Raw Materials.
Constituents (%) SiO2 Al2O3 Fe2O3 SO3 MgO CaO Na2O LOI

Fly Ash 1 (F1) [25] 44.45 25.30 5.92 4.49 0.598 10.64 0.57 5.84
Fly Ash 2 (F2) [25] 36.80 3.82 14.78 10.03 0.895 22.40 0.55 7.71
Lime (L) NT NT NT NT NT 63.33 NT NT
GGBS (G) 33.62 26.02 2.01 NT NT 28.15 NT NT

NT- Not Tested.

Table 3
Proportions by dry weight of different raw materials in trial mixes for F1 and F2 fly ash.
Mix-1 Mix-2 Mix-3 Mix-4

Mix Fly Lime GGBS Cement Fly Lime GGBS Cement Fly Lime GGBS Cement Fly Lime GGBS
Category Ash (%) (%) (%) Ash (%) (%) (%) Ash (%) (%) (%) Ash (%) (%)
(%) (%) (%) (%)

FL 98 2 0 0 96 4 0 0 94 6 0 0 92 8 0
FLG-1 98 1.5 0.5 0 96 3 1 0 94 4.5 1.5 0 92 6 2
FLG-2 98 1 1 0 96 2 2 0 94 3 3 0 92 4 4
FLG-3 98 0.5 1.5 0 96 1 3 0 94 1.5 4.5 0 92 2 6
FG 98 0 2 0 96 0 4 0 94 0 6 0 92 0 8
F 100 0 0 0 – – – – – – – – – –
FC 96 0 0 4 92 0 0 8 88 0 0 12 – – –

FL:Fly Ash-Lime, FLG: Fly Ash-Lime-GGBS, FG- Fly ash-GGBS, F-Fly Ash, FC:Fly ash-Cement.

maximum efficiency. In this curing method, initial hardening of the
specimens in hot air oven at a temperature of 50 ◦ C for 6 ± 1 h was
carried out. If samples are kept in hot water immediately after
compaction then it will disintegrate and it was found that minimum
50 ◦ C temperature of hot air is required for initial hardening to prevent
disintegration. Then specimens of F1 and F2 fly ashes were cured in hot
water at a temperature of 75 ◦ C and 65 ◦ C, respectively, for curing
period of 24 h. Subsequently, fragmented pieces of different fly ash-
additive mixes were collected from the failed UCS test specimens and
then broken into the required size of aggregate to perform aggregate
impact value tests. XRD and SEM measurements were carried out on
powder sample and fractured pieces of different mixes, respectively,
after completion of hot water curing. Based on unconfined compressive
strength, aggregate impact value and micro level study optimum com­
bination of fly ash-additive mixes were finalized.
For large scale manufacturing of the proposed fly ash aggregates the
fly ash brick making machines readily available in the market are most
suitable to prepare the compacted specimens of fly ash-additive mixes.
Therefore, in the present study fly ash blocks of size 20 cm × 10 cm × 8
cm were prepared for the two optimum mixes i.e., 96F1 + 4L mix and
98F2 + 2L mix. OMC values were found to be about 30% and 26% for
the mixes of 96F1 + 4L and 98F2 + 2L, respectively, and a pressing force
of about 17 tons is required to prepare the fly ash blocks with the
maximum dry unit weight determined from modified Proctor test. To
study the effect of moisture content and pressing force on strength of
mixes and impact value of aggregates, fly ash blocks were prepared with
three different moisture content (=OMC, OMC-3% and OMC-6%) and
compacted under three different pressing forces of 17 tons, 26 tons, and
35 tons. Then blocks were cured in hot water bath as explain above. The
compressive strength of the cured fly ash blocks was determined using a
compression testing machine. The impact values of aggregates prepared
from the cured blocks were also determined. Based on the test results of
compressive strength and impact value optimum combinations of
moisture content and pressing force were selected for 96F1 + 4L mix and
98F2 + 2L mix.
2.2. Synthesis of aggregates and tests on aggregates
For preparation of fly ash aggregates fly ash blocks of 96F1 + 4L mix
and 98F2 + 2L mix were prepared for the optimum combinations of
moisture content and pressing force and cured in hot water bath. Then
these blocks were kept at ambient temperature for 24 hrs. and subse­
quently crushed into different sizes of coarse aggregates.
Fly ash aggregates were oven-dried at 105 ◦ C for 24 h before the
tests. The physical properties of aggregates have been discussed through
bulk density, specific gravity, and water absorption as per IS 2386 Part-
III [29]. The toughness of aggregate was determined by the impact value
test as per IS: 5640 [30]. The behavior of aggregates under a gradually
applied compressive load is termed as crushing value. The standard
aggregate crushing test was performed on the aggregate sample of 12.5-
mm passing and retained on a 10-mm IS sieve [30]. The Los Angeles
abrasion test measures the resistance to degradation i.e. hardness of
mineral aggregates under standard test conditions. The combined effect
of impact, abrasion, and grinding in a revolving steel drum having a
quantified number of steel balls on the standard gradation of aggregates
are evaluated. The numbers of steel balls are depended upon the
gradation of the test sample. The sample is removed from the drum after
the specified number of revolutions and sieved through the 1.7 mm
standard sieve to measure the degradation as a percent loss. In this
study, grading-A having a maximum and minimum particle size of 40
mm and 10 mm, respectively, as per IS 2386 Part-IV [31] has been used.
The 12 number of abrasive charges having a total weight of 5000 ± 25g
were used.
A soundness test was conducted to study the resistance of fly ash
aggregates to weathering action and to evaluate the durability charac­
teristics. In this study, saturated solution of sodium sulphate was pre­
pared and used as a reagent. The sample of coarse aggregate having a
size of 4.75 mm to 40 mm was thoroughly washed and dried out to
constant weight at 105 ◦ C and then separated into different sizes as
given in IS 2386 Part-V [32]. For the fractions coarser than 20 mm, the
number of particles was also counted. Then samples were immersed in
the prepared reagent for 16 h of immersion period at a temperature of 27
± 1 ◦ C. After completion of the immersion time the sample was removed
from the solution and kept to drain for 15 min followed by placing in the
hot air oven at a temperature of 105 ◦ C to obtain a constant weight.
When the constant weight has been attained the samples were allowed
to cool to room temperature and then again immersed in the prepared
solution. Five numbers of alternate such cycles were performed as pre­
scribed by Ministry of Road Transport and Highway (MoRTH) [33].
The leachate test was performed to confirm the possibility of envi­
ronment pollution due to leaching of heavy metals from the proposed
cold bonded fly ash aggregates. To obtain an aqueous solution the

3
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

standard procedure for leaching of solid waste with water as described 28 37

in ASTM D-3987 [34] was followed. Leaching test was performed on the 2% Additive 4% Additive
raw fly ash as well as on the selected fly ash aggregates having maximum 6% Additive
26
particle size of 4.75 mm. The extraction fluid prepared with glacial UCS AIV 35
acetic acid (CH3COOH and NaOH diluted in distilled water) at pH of
4.93 ± 0.05 was used. The pH of the leachates was measured prior to the 24

Impact Value (%)

UCS (MPa)
test. Then analysis for various heavy metals and toxic substances was 33
carried out using the atomic adsorption spectrophotometer (AAS). 22
31
3. Results and discussion 20

3.1. Compaction characteristics 29

18
UCS of 100F2: 19.36 MPa
OMC and maximum dry unit weight values of F1-additives mixes AIV of 100F2: 36%
were found to be in the range of 29.5–30.2% and 11.1–11.3 kN/m3, 16 27
respectively. Whereas, F2-additive mixes have an OMC value of 26% 0 25 50 75 100
and maximum dry unit weight varies between 13.4 and 13.5 kN/m3. No Replacement of Lime with GGBS (%)
considerable change in OMC and dry unit weight of fly ash-additives
mixes was observed for both the fly ashes. This might be as a result of Fig. 2. Variation of UCS and AIV with the different percentage of additives
for F2.
the high lime content available in the fly ashes itself.

3.2. Effect of additive content on UCS and aggregate impact value
Unconfined compressive strength (UCS) test results of various fly
ash-Lime-GGBS mixes cured with hot water curing are given in Fig. 1
and Fig. 2. It is observed that lime has the intense effect on the
compressive strength of the FL mix. With the increase in lime, UCS
values increase; however, this rise in the strength becomes insignificant
at 6% and 4% lime for F1 and F2 fly ashes, respectively. The strength
enhancement in mixes arises owing to pozzolanic reaction between
calcium ions of lime with silica and alumina ions available in fly ash. By
the increase of lime percentage in fly ash, the amount of cementitious gel
formation due to pozzolanic reaction rises, resulting in a higher strength.
But, when lime is added beyond the optimum percentage certain lime
particles may remain unutilized because all silica and alumina particles
presented in the fly ash for the pozzolanic reaction might have already
been utilized. Therefore, a very small increase in strength was witnessed
beyond 6% and 4% lime content for F1 and F2 fly ashes, respectively.
Alternatively, Fig. 1 shows that at any percentage of additives (i.e. 2,
4, 6, and 8), UCS values decrease as the replacement of lime with GGBS
increases (FLG mix). Similar curves were also obtained for the mixes of
F2 fly ash (Fig. 2). Moreover, for 100% replacement of lime with GGBS
at 2% additive for F1 fly ash and 2%, 4%, and 6% additives for F2 fly ash
UCS values are lower than the UCS value of only fly ash without any
25 38
2% Additive 4% Additive
6% Additive 8% Additive
36
23 UCS AIV
34
Impact Value (%)
UCS (MPa)
additive (16.96 MPa for 100F1 and 19.36 MPa for 100F2). This indicates
that the pozzolanic reaction between lime and fly ash is more predom­
inant than that between fly ash and GGBS. This might be owing to fewer
amounts of calcium ions available in GGBS (Table 2) to react with silica
and alumina present in fly ash for the pozzolanic reaction. Similarly, the
usefulness of cement as an additive for the strength development of fly
ash was also studied (Fig. 3). The improvement in UCS value by the
addition of cement up to 12% was found to be lower as compared to that
for addition of lime up to 4% as an additive. This may be because of the
higher specific surface area of lime as compared with that of cement. The
larger the specific surface area of the binder, the higher will be the
chemical reactivity leading to the formation of stronger mass [35]. The
cost of cement is higher than that of lime and hence, addition of cement
as an additive for manufacturing fly ash aggregate is not recommended.
Fig. 1, Fig. 2, and Fig. 3 also show the influence of binders with
different combinations and dosages on the aggregate impact value
(AIV). The higher the UCS value, the lower will be the impact value of
aggregates. The addition of lime with different dosages caused notice­
able improvement in AIV for both the fly ashes (Fig. 1 and Fig. 2).
Aggregate impact value improves continuously as the lime content in­
creases up to 6% and 4% for F1 and F2 fly ashes, respectively, and this
rate of improvement decreases thereafter with further addition of lime.
AIV improves approximately by 1.25, 1.30 and 1.32 times with the
addition of 2%, 4% and 6% lime in F1 fly ash, respectively. Similarly, for
F2 fly ash, impact values for 2%, 4% and 6% lime content were found to
22 35
34
21

21 33
Impact Value (%)

20
UCS (MPa)

32
19 32
30 19
UCS AIV 31
17
28
UCS of 100F1: 16.96 MPa 18
30
AIV of 100F1: 38%
15 26 F1+Cement F2+Cement
0 25 50 75 100 17 29
Replacement of Lime with GGBS (%) 4 8 12
Percentage of Cement
Fig. 1. Variation of UCS and AIV with the different percentage of additives
for F1. Fig. 3. Variation of UCS and AIV for different fly ash-Cement mixes.

4
H.A. Shahane and S. Patel
be enhanced by 1.35, 1.37, and 1.37 times as compared to that for 0%
lime content. When the lime content is more than the optimum value,
the calcium irons remain unutilized because all the reactive silica and
alumina ions available in the fly ash may already be exhausted. The
unutilized calcium irons simply serve as weak filler in the mix resulting
in insignificant contribution for the improvement of impact values.
Fig. 1 and Fig. 2 show the variation of AIV for various FLG mixes.
With the replacement of lime with GGBS, AIV increase; and this value
coincides with AIV of 100% fly ash (38% for F1 and 36 % for F2) as
shown in Fig. 1 and Fig. 2. In FLG and FG mixes silica and alumina
present in fly ash may be partially utilized owing to lesser amounts of
calcium ions present in the GGBS for pozzolanic reaction. Similarly,
improvement in AIV by the addition of cement up to 12% was also found
to be lower as compared to that for addition of lime up to 6% and 4% as
an additive in F1 and F2 fly ashes, respectively (Fig. 3). This resulted in
marginal improvement in AIV when GGBS and cement were used as
additives. This shows that lime is more effective in accomplishing the
strength and impact value as compared to GGBS and cement. Based on
the test results of UCS and AIV, 96F1 + 4L mix and 98F2 + 2L mix were
selected as the optimum mixes for the production of fly ash aggregates.
3.3. The relation between UCS and impact value
In the present work, an effort has been made to develop empirical
relations for evaluation of impact value of fly ash aggregates from UCS
value of mixes. The UCS (qu) of the mixes depends on several important
factors, such as type of curing, type of fly ash, binder content, and type of
binder. Nonetheless, UCS may be used as the reference variable in
evaluating the impact value, as UCS values may signify the collective
effects of the important leading factors on the toughness.
Fig. 4 shows that the impact value obtained from standard aggregate
impact value tests can be presented as a linear function of unconfined
compressive strength (qu) of F1 and F2 fly ash stabilized with various
additives and cured by hot water curing method. Similarly, the linear
correlation between AIV and UCS (qu) of the F1 and F2 fly ash cured with
different curing methods is presented in Fig. 5 (Data from Shahane and
Patel [25]). The empirical relationships with the R2 values are given in
the figure for various curing types. However, the values of AIV for the
hot water curing method are only considered in developing the model
for the present study. It is observed from Fig. 4 and Fig. 5 that the impact
value depends upon the curing method, fly ash type, binder content, and
binder type.
With these results, a general empirical correlation for impact value is
38
98F1+L+G 96F1+L+G
94F1+L+G 98F2+L+G
36
96F2+L+G 94F2+L+G
34 F1+C F2+C
Impact Value (%)
32
30
28
F1 F2
26
15 18 21 24 27
Unconfined Compressive Strength (MPa)
Fig. 4. Relationship between AIV and UCS of different fly ash-additive mixes
cured by hot water.
5
Construction and Building Materials 327 (2022) 126914
proposed as a function of unconfined compressive strength, qu (MPa). By
multiple regression analysis [38] of the experimental outcomes of hot
water curing method, different fly ashes, and different additive mixes
the empirical correlation for impact value achieved is presented as
follows:
AIV = − 0.93qu + 51.45, R2 = 0.91 (1)
Where, AIV = aggregate impact value (%); qu = unconfined
compressive strength (MPa); and R2 = the coefficient of correlation.
The predicted AIV using Eq. (1) is plotted against the measured AIV
for the various fly ash-additive mixtures cured by hot water curing in
Fig. 6. The empirical correlation proposed above is in the simple format,
considers UCS as the independent variable capable of demonstrating the
collective effects of the factors that can affect the impact value of the fly
ash aggregates. The selection of model was established on physical
implication. However, this correlation may be refined when new sup­
plementary results become available.
3.4. Microstructure investigation
Micro level study was undertaken to find out the probable reason of
variation in the strength of hot water cured fly ash mixtures with
different additives. The XRD measurements were carried out through
Bruker D8 advanced X-ray diffractometer using CuKα radiation and the
wavelength of the X-ray was 0.154 nm. The peak intensity of various
compounds of fly ash-additive mixes was analyzed to understand the
strength and toughness of the mixes (Fig. 7 and Fig. 8). Silica, alumina,
and iron oxide of fly ash react with calcium present in lime and GGBS to
develop calcium silicate, calcium aluminate, calcium aluminosilicate,
and these compounds are accountable for the improvement in the
strength of aggregate [13].
Fig. 7a and Fig. 7b shows the XRD results of hot water cured fly ash-
lime mixes. For both the F1 and F2 fly ashes, an increase in lime dosage
leads to a decrease in the intensity of quartz peak. The intensity of the
most important phases such as dicalcium silicate, calcium silicate hy­
drate, and ettringite for 100F1 were less than that of 98F1 + 2L mix.
After the addition of 2% lime, these phases increase significantly. This
percentage of rise of three compounds is significant in the beginning but
slows down after 6% of lime content as non-reacted calcium particles in
the form of CaCO3 increase in the mixes. The compounds dicalcium
silicate and dicalcium aluminosilicate were increased by about three
times owing to the addition of 4% lime in the mix. Similar results were
also obtained for F2-lime mixes (Fig. 7b). However, the optimum results
were found at 2% lime content as higher initial lime content available in
the F2 fly ash. This represents that formation of non-reacted hydrated
product cause of the lower UCS value and higher AIV (Fig. 1 and Fig. 2)
of the mixes. Similar results were also obtained by Shahane and Patel
[25].
It was witnessed from the XRD results of fly ash-lime mixtures that
the formation of dicalcium silicate, calcium silicate hydrate, and
ettringite are responsible for strength development of the mix. The
amount of these three compounds is less in fly ash-lime-GGBS mix (not
shown here) indicating a low strength of the mix. The XRD of the ag­
gregates with GGBS and cement as additives are presented in Fig. 8a and
Fig. 8b. It is observed that the quantities of hydrated products (CSH and
C2S) are governed by the type of additive and its dose. GGBS and cement
as an additive gives a very low concentration of dicalcium silicate, cal­
cium silicate hydrate, and ettringite compounds for both the fly ashes.
XRD peak intensity of these compounds is found to be almost same for
both GGBS and cement as an additive.
The structural alterations that take place during the pozzolanic re­
action are analyzed by observing cured fly ash-additive mixes under
scanning electron microscope. Fig. 9 shows the SEM images of fly ash-
lime mixes. For the micrographs, a magnification of 4500 was used.
Many unreacted fibrous fly ash particles are present in 100F1 and 100F2
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

86.00
Sealed y = -2.35x + 73.15
76.00 Curing R² = 0.95
Open y = -1.76x + 77.29
66.00 Curing R² = 0.95
Impact Value (%)

Steam y = -1.99x + 63.92

56.00
Curing R² = 0.97

46.00 Humidity y = -1.90x + 63.53

Curing R² = 0.97
36.00
Hot Water y = -1.03x + 53.85
Curing R² = 0.97
26.00
0 3 6 9 12 15 18 21 24 27
Unconfined Compressive Strength (MPa)
Fig. 5. Relationship between AIV and UCS of fly ash-additive mixes for different curing methods.

ettringite as compared to that of fly ash-lime mix (Fig. 10) for both fly
40 ashes.
F1+L+G F2+L+G
F1+C F2+C 3.5. Effect of moisture content and compressive force on strength and
toughness of mixes
Predicted AIV (%)

35
30
Equality line
AIV (%)= -0.93qu+51.45
R2=0.91
25
25 30 35
Measured AIV (%)
Fig. 6. Measured impact value versus predicted impact value using pro­
posed equation.
(i.e. without lime) fly ash mixes. The arrangement of fly ash particles
without lime is discrete and irregular. Lack of binding gel between the
fly ash particles may be the reason for the lower strength of mixes.
Furthermore, fly ash-lime mixes having 2% to 6% lime content show
that fly ash particles are interconnected with a significant amount of
cementitious gel and ettringite. The fly ash particles are bound by a
continuous matrix of pozzolanic compounds formed by the reaction of
lime and fly ash, resulting in an increase in unconfined compressive
strength of mixes. Similar kinds of observations were recorded in the
literature [36–37]. The formation of ettringite densified the structure
and increases the density and strength of aggregate considerably [13].
However, at 6% lime content unreacted lime particles are observed in
SEM images of F1 and F2 fly ashes (Fig. 9). These unreacted lime par­
ticles act as weak filler in mixes leading to the lower strength and higher
AIV (Fig. 1 and Fig. 2).
As the lime is replaced by GGBS the formation of cementitious gel
decreases and the unreacted fibrous pore structure increases (Fig. 10).
The fly ash-GGBS mixes displayed the presence of pores that contribute
to the low strength of the mixes and higher AIV. Similarly, fly ash–ce­
ment mix gives the marginal improvement in the formation of gel and
Fig. 11 and Fig. 12 show the effect of moisture content and pressing
force on compressive strength of the mixes and impact value of aggre­
gates. An increase in pressing force results in an increase in compressive
strength of fly ash block and decrease in AIV for given moisture content
for both F1 and F2 fly ashes-additive mixes. The compressive strength
value increase by 10% and 24% with the increase in the pressing force
from 17 tons to 26 ton and 17 tons to 35 ton, respectively at OMC of 30%
for F1 (Fig. 11). Similarly, it increased by 11% and 37% with the in­
crease in the pressing force from 17 ton to 26 ton and 17 ton to 35 ton,
respectively, at a moisture content of 27%. Similar trend of observations
was also obtained for F2 fly ash specimens as shown in Fig. 12. With the
40
increase in pressing force, fly ash particles are closely packed and
interlocked with each other as a result of this diameter of capillary voids
decreases and fly ash particles get bonded more effectively by binding
gel resulting in a rise in the strength of the specimen [39].
At a given pressing force of 17 tons and 26 tons compressive strength
decreases and AIV increases with the decrease in moisture content
(Fig. 11 and Fig. 12). With the decrease in moisture content the lubri­
cation of fly ash particles decreases and the mix offers more resistance to
compaction as a result of which the void space between fly ash particles
increases resulting in a loosely compacted mix and hence, strength de­
creases. For pressing force of 17 tons and 26 tons moisture content of
30% and 26% exhibited best results for F1 and F2 fly ashes, respectively,
whereas, for 35 tons of pressing force best results were observed for
moisture content of 27% and 23% for F1 and F2 fly ashes, respectively.
With the increase in compactive effort the quantity of water required for
lubrication of the fly ash particles to achieve better compaction de­
creases. Squeezing out of fly ash slurry from the mix was observed for
the pressing force of 35 tons with moisture content of 30% and 26% for
F1 and F2 fly ashes, respectively, which indicates that these moisture
contents are on the wet side of the optimum value resulting in a lower
strength of the mix.
As expected, the trend for the variation of AIV with moisture content
and pressing force was found to be exactly opposite to that of
compressive strength (Fig. 11 and Fig. 12). The best combinations of
moisture content and pressing force for the optimum mixes of 96F1 + 4L
and 98F2 + 2L were found to be 27% and 35 tons; and 23% and 35 tons,

6
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

Q
E Q
C 2S CCS 94F1+6L
Q C 2
CSH C 2S
Q 94F2+6L

CSH
E

C 2S
C E G E C 2S
Q
E

CSH
C 2S E Q
Q 96F1+4L 96F2+4L
C 2S E CSH
E CSH C 2S Q E
C Q E

C 2S
G E C 2S

E Q Q
E
Q CSH
C 2S
98F1+2L CSH
C2S C C 2S
CSH Q E E 98F2+2L
E C
G E

C 2S
C2SE M C E C2S
Q
E Q

Q CSH
Q 100F1 E 100F2
E C 2S C
CSH G E AH
C ECS
2

10 20 30 40 50 60 10 20 30 40 50 60
2θ 2θ

a. F1+Lime b. F2+Lime
Fig. 7. X-ray diffraction pattern of fly ash-Lime mixes. Q-Quartz (SiO2), AH-Calcium Sulfate Anhydrite (CaSO4), C-Calcite (CaCO3), E-Ettringite (Ca6Al2(SO4,SiO4,
CO3)3(OH)12⋅26H2O), C2S-Dicalcium Silicate (Ca2SiO4), CSH-calcium silicate hydrate Ca3(OH)2Si16⋅4H2O, G-Dicalcium Alumosilicate (Al2Ca2SiO7),
M¡Magnetite (Fe3O4).

Q
E CSH 96F1+4C Q
C 2S
Q C E C 2S
C 2S 96F2+4C
Q E
CSH E

E Q
Q
Q CSH
C2S 96F1+4G
C 2S C E C 2S
Q E 96F2+4G
CSH E
E Q

Q
CSH
C 2S E
C 2S Q E 96F1+4L
E CSH C2S
CSH
C Q Q E 96F2+4L
E E

10 20 30 40 50 60 10 20 30 40 50 60
2θ 2θ

a. F1+Additive b. F2+Additive
Fig. 8. X-ray diffraction pattern of fly ash-Additive mixes. (Legends as in Fig. 7).

respectively. The lowest AIV of 20.15% and 19.66% was observed for F1 4. Test on aggregates and comparison of properties with
and F2 fly ashes, respectively. specification

Various engineering properties such as unconfined compressive

strength, AIV, and microscopic study of fly ash-additive mixes were
investigated, and two optimum mix proportions one each from two types

7
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

Fig. 9. SEM image of hydrated products of fly ash-lime mixes.

8
H.A. Shahane and S. Patel
Fig. 10. SEM image of hydrated products of fly ash-additive mixes.
of fly ash were adopted based on the achieved strength and AIV re­
quirements of Indian standard specifications. These optimum mix pro­
portions by dry weight are 96F1 + 4L (i.e., 96% fly ash 1 + 4% lime) and
98F2 + 2L (i.e., 98% fly ash 2 + 2% lime).
The physical and mechanical properties of the proposed fly ash ag­
gregates obtained from various laboratory tests were presented in
Table 4 along with the standard specifications. The specific gravity and
bulk density of aggregates prepared with lime as binder i.e., for 96F1 +
4L and 98F2 + 2L mixes were found to be higher than that of 100F1 and
100F2 mix aggregates. Also specific gravity of fly ash particles for F1 and
F2 fly ashes (Table 1) found to be lower than specific gravity of fly ash
aggregates. This is due to the formation of ettringite which densifies the
9
Construction and Building Materials 327 (2022) 126914
structure and increases the density of mixes as evident in XRD and SEM
results. However, these values are much lower than those of natural
aggregates. The water absorption of aggregates was found in the range
of 24% to 32% for various mixes (Table 4). But, after addition of binder
these values decreased to 15% to 25% for F1 and F2 fly ashes, respec­
tively. The high water absorption value specifies that the various
properties (e.g. workability, creep, shrinkage etc.) of concrete may be
affected by it. Therefore, fly ash aggregates in saturated surface dry
condition may be used in concrete preparation or suitable corrections for
quantity of water required during concrete mixing should be applied.
Table 4 also shows that aggregates produced from fly ash-lime mix
have better impact resistance (toughness) than the aggregates produced
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

4.1. Crushing value of aggregate

The crushing value is expressed as the ratio of the mass of fines

passed through 2.36 mm IS sieve to the overall mass of the sample. The
crushing value of aggregates decreased with addition of lime to fly ash
(Table 4). The crushing value of aggregates for F1 and F2 fly ashes were
found to be 34% and 31%, respectively, which decreased by 18% and
26% with the addition of optimum lime content to F1 and F2 fly ashes,
respectively. The reason for this is probably the same as that mentioned
earlier in UCS and impact value of aggregate. The lower strength of
100F1 and 100F2 aggregates was possibly due to the presence of many
unreacted fibrous fly ash particles in the fly ash mixes (Fig. 11).

4.2. Los Angeles abrasion value

The percentage degradation of fly ash aggregates due to rubbing with

Fig. 11. Effect of moisture content and pressing force on compressive strength
of block and AIV for F1.
steel balls was determined and the abrasion values are reported in
Table 4. Los Angeles abrasion values of all mixes are higher as compared
to that of natural stone aggregates. However, based on the requirement
of IS 383 [42] and MoRTH [33] these fly ash aggregates are found
suitable for use in non-wearing surfaces of concrete and base and sub-
base layer of flexible road pavements.

4.3. Soundness test

After 5 numbers of alternate immersion and drying cycles quantita­

tive and qualitative examination of aggregates was carried out. Fig. 13
shows the photograph of fly ash aggregates after 3rd and 5th cycle. The
fly ash aggregates shown in Fig. 13c indicates the intactness of structure
even after 5 alternate immersion and drying cycles. Very few aggregate
were disintegrated and crack on 2–3 pieces of aggregates has been
observed, however, this weight loss is well within the permissible limit.
The soundness results of the aggregates are reasonably acceptable and
satisfying the requirements of the Indian standards (Table 4). Even
though the fly ash aggregates have porous structure with water ab­
sorption of about 24% to 32% this structure has not been affected much
by sodium sulfate solution during soundness test. This may be due it
strongly bounded structure of fly ash particles. Such structure of the
proposed fly ash aggregates may exhibits good fire resistance and sound
insulation properties.
Fig. 12. Effect of moisture content and pressing force on compressive strength
of block and AIV for F2.
4.4. Leaching characteristics
from 100% fly ash. Moreover, these results fulfill AIV requirements of
The pH value of the aqueous solution of raw fly ashes F1 and F2 were
MoRTH [33] for GSB and WMM layer and also fulfill the AIV require­
11.09 and 11.36, respectively. These values decreased to 10.27 and 9.85
ment for sintered fly ash aggregates as per IS 9142: Part-II [41].
for F1 and F2 fly ashes, respectively, after hot water curing. Similarly,

Table 4
Typical physical and mechanical properties of an aggregate made with this process.
Parameters Authors Results Properties of Natural IS 383 (2016) MoRTH-2013 IS 9142
Aggregates [40] Requirements Requirements [33] (Part 2) 2018
100F1 96F1 + 100F2 98F2 +
[42] Requirements [41]
4L 2L

Specific Gravity 1.28 1.30 1.65 1.74 2.65 2.1 to 3.2 – –

Dry Loose Bulk Density 680 710 880 890 1534 – – ≤ 950
(kg/m3)
Water absorption (%) 30 26 32 24 0.7 ≤ 2% – ≤ 18%
Wet Impact value (%) 29.5 21 24 19.3 16 ≤ 30% (wearing ≤ 40% Sub-base ≤ 40%
surfaces) ≤ 30% Base Courses
≤ 45% (nonwearing
surfaces)
Crushing value (%) 34 28 31 23 22 ≤ 30% – ≤ 45%
Los Angeles Abrasion 43 35 46 36 23 ≤ 30% (wearing ≤ 40% For Base Courses ≤ 40%
Value (%) surfaces)
≤ 50% (nonwearing
surfaces)
Soundness in Na2SO4 13.5 10 12.5 9 – ≤ 12% ≤ 12% ≤ 12%
(%) (5 Cycles)

10
H.A. Shahane and S. Patel Construction and Building Materials 327 (2022) 126914

Fig. 13. Qualitative observation of Fly ash aggregate (96F1 þ 4L) (Images by H. Shahane).

96F1 + 4L and 98F2 + 2L mixes show the pH of 9.35 and 7.95, indi­
vidually, after hot water curing. The pH level shows that the aggregate
nature changed from alkaline to neutral with hot water curing and
addition of lime as binder this indicating the stabilization of fly ash. The
analysis of the concentration of heavy metals performed for various fly
ash aggregates is given in Table 5. The outcomes demonstrated that the
contagion levels of the toxic elements leached from the fly ash aggre­
gates are well within the limit of Indian drinking water standards [43]
and India Hazardous Waste Management (HWM) Rules. The concen­
tration of heavy metals in the leachate practically diminished after
addition of lime to the fly ashes and cured by hot water curing for all
samples. The non-leachable and nontoxic nature of the hot water cured
fly aggregates additionally indicates that they would neither contribute
to any composite chemical reaction affecting the durability of concrete
nor cause environmental problems leading to ground-water and land
contamination.
5. Conclusions
Engineering properties of fly ash-additive mixes are investigated for
their use to produce angular shaped fly ash aggregates and different
properties of fly ash aggregates produced with optimum mixes are
evaluated. The following conclusions are drawn:
1. An increase in the lime content of the lime-treated fly ash specimen
shows an improvement in UCS value and aggregate impact value.
However, a very small improvement in strength and AIV was wit­
nessed beyond 6% and 4% lime content for F1 and F2 fly ashes,
respectively.
2. For a given binder content compressive strength and AIV of fly ash-
lime mix was found to be the best followed by fly ash–cement mix
and fly ash-GGBS mix. This shows that lime is more effective in
accomplishing the strength and impact value as compared to cement
and GGBS. Based on the test results of UCS and AIV, 96F1 + 4L mix
and 98F2 + 2L mix were selected as the optimum mixes for F1 and F2
fly ashes, respectively.
3. The characterization studies on hot water cured fly ash-additive
mixes demonstrate that the properties of aggregates are influenced
by the type of additives, its dosage, and the type of fly ash used. A
simple empirical relation is developed with R2 value of 0.91 to es­
timate the aggregate impact value from unconfined compressive
strength of the mix.
4. XRD and SEM analyses show that the amount of binding gel forma­
tion was the maximum for fly ash-lime mix as compared to fly
ash–cement mix and fly ash-GGBS mix for a given binder content
which agrees with the laboratory test results for strength and AIV.
5. For a given moisture content strength and AIV improves with in­
crease in pressing force applied on fly ash blocks. With the increase in
compactive effort, fly ash particles are closely packed and inter­
locked with each other and the quantity of water required for
lubrication of the fly ash particles to achieve better compaction de­
creases. The best combinations of moisture content and pressing
force for the two optimum mixes were found to be 27% and 35 tons;
and 23% and 35 tons for F1 and F2 fly ashes, respectively.
6. The results shows that produced angular shaped fly ash aggregates
are sufficiently tough, strong, hard and durable. The physical and
mechanical properties of fly ash aggregates are found to be quite
satisfactory as per the required specifications of various Indian
standards for use in road and structural concrete. The specific gravity

Table 5
Heavy metal concentrations leached as a result of TCLP test.
Metal Raw Fly Ash F1 100F1 96F1 + 4L Raw Fly Ash F2 100F2 98F2 + 2L IS:10500–2012 (Max) [43] HWM Rules 2016
(mg/l) (Cured) (Cured)

pH 11.09 10.27 9.35 11.36 9.85 7.95 – –

Copper (Cu) ND ND ND ND ND ND 0.05 25
Iron (Fe) 2.1 1.2 >0.15 3.1 2.4 >0.15 0.3 NL
Zinc (Zn) 0.4 0.4 ND 0.1 0.1 ND 5 250
Cadmium (Cd) ND ND ND ND ND ND 0.003 1
Lead (Pb) ND ND ND ND ND ND 0.01 5
Nickel (Ni) ND ND ND ND ND ND 0.02 20
Total chromium (Cr) ND ND ND ND ND ND 0.05 5

Concentrations in mg/l, ND – Not detected, NL –Not listed in TCLP list.

11
H.A. Shahane and S. Patel
of the proposed fly ash aggregates is quite low as compared to that of
natural stone aggregates leading to additional benefit of reduction in
dead weight of the concrete structures.
7. The leaching characteristics of heavy metals from fly ash aggregates
concluded that bulk utilization of these aggregates in construction
industry will be safe and environmental-friendly.
CRediT authorship contribution statement
Hrishikesh A Shahane: Writing – original draft, Conceptualization,
Methodology, Data curation. Satyajit Patel: Writing – original draft,
Supervision, Writing – review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
Thanks, Center Director and Director of UGC-CSR for allowing us for
utilizing the XRD facilities. Thanks to Dr. Mukul Gupta (Scientist) and
Mr. Layanta Behera for allocating the time slot for performing the XRD
experiments and providing us raw data.
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coarse aggregate. IS 9142 Part-II, New Delhi, India, 2018 (Indian Standard).
[42] IS, Coarse and Fine Aggregate for Concrete-Specification. IS 383, New Delhi, India,
2016 (Indian Standard).
[43] IS, Drinking water- Specification, IS 10500, New Delhi, India, 2012 (Indian
Standard).