Cement & Concrete Composites 30 (2008) 848–853

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Cement & Concrete Composites

journal homepage: www.elsevier.com/locate/cemconcomp

Effect of curing method on characteristics of cold bonded fly ash aggregates

R. Manikandan, K. Ramamurthy *
Building Technology and Construction Management Division, Department of Civil Engineering, Indian Institute of Technology Madras, Chennai 600 036, India

a r t i c l e i n f o a b s t r a c t

Article history: This paper discusses the influence of normal water curing, autoclaving and steam curing on the proper-
Received 27 June 2007 ties of a typical class-C fly ash aggregate. The 10% fines value, water absorption, and porosity of aggre-
Received in revised form 18 November 2007 gates are correlated with SEM and XRD results to understand the influence of various factors and
Accepted 14 June 2008
material characteristics. An increase in duration of normal water curing significantly improved the aggre-
Available online 20 June 2008
gate properties. Autoclaving and steam curing resulted in relatively lower enhancement in the properties
as compared to normal water cured aggregate. Between the accelerated curing methods, autoclaved
Keywords:
aggregate possessed properties closer to the normal water cured aggregate due to the dense microstruc-
High calcium fly ash
Cold bonded fly ash aggregate
ture formation. Continuation of normal water curing, after initially subjecting the aggregates to acceler-
Normal water curing ated curing, exhibited only a marginal improvement in the properties.
Autoclaving Ó 2008 Elsevier Ltd. All rights reserved.
Steam curing
Aggregate properties

1. Introduction ature up to 1080 °C for sintered sewage sludge ash aggregate.

Addition of binders like cement and lime along with increase in
As aggregates occupy large volume in concrete, conversion of fly duration of normal water curing (i.e., cold bonding) was reported
ash into aggregate facilitates high-volume utilization of fly ash and to significantly improve the properties of fly ash aggregate
saves depleting natural aggregates. Incorporation of sintered and [5,7,12] and requires minimum energy as compared to sintered
cold bonded fly ash aggregates in concrete not only reduces the fly ash aggregate. However, the properties of cold bonded fly ash
density of concrete [1,2] but also increases the thermal and acous- aggregate were observed to be comparatively lower than those of
tical insulation [3,4] and reduces the autogenous shrinkage [5]. sintered fly ash aggregate. This is because of use of low calcium
Bijen [6] presented an overview of the manufacturing process of (class-F) fly ash, which requires higher binder content and acceler-
artificial fly ash aggregates. Baykal and Doven [7] have investigated ated curing methods for enhancing strength and reducing water
the parameters influencing pelletization of fly ash and reported absorption. Limited studies have been reported on use of high cal-
that the angle and speed of the disc considerably influenced the cium fly ash in the production of cold bonded fly ash aggregates.
density and strength of the fly ash aggregate. Harikrishnan and
Ramamurthy [8] have reported that the speed of disc has signifi- 2. Research significance
cant influence on strength and water absorption of aggregate
followed by the angle of disc, while moisture content was an The properties of cold bonded fly ash aggregate were reported
important factor influencing the size growth of aggregate. to be comparatively lower than those of sintered fly ash aggregate
In order to improve the properties of fly ash aggregates due to the use of low calcium fly ash and only limited studies have
(strength and water absorption) various hardening methods viz., been carried out on high calcium fly ash. Preliminary investigation
sintering, normal water curing, autoclaving and steam curing, on pelletization of class-C fly ash showed that almost all the mate-
and binders like cement, lime, bentonite and chemical admixtures rials were converted into aggregates of size greater than 4.75 mm
have been used [9]. Show et al. [10] have reported that an increase without any binders. Further, statistically designed two level frac-
in sintering temperature up to 1300 °C along with increase in pro- tional factorial experiments showed that angle and speed of the
portion of marine clay from 0% to 30% significantly reduced the disc significantly influence the pelletization of class-C fly ash while
density and water absorption of industrial sludge aggregate. the other factors, moisture content and duration were insignificant
Cheeseman et al. [11] also reported similar behaviour of reduction due to the narrow range of the factors [13]. As sintering of Class-C
in density and water absorption with increase in sintering temper- fly ash causes aggregate disintegration, cold bonding is the appro-
priate technique. Such cold bonded aggregates require curing. This
* Corresponding author. Tel.: +91 44 22574265; fax: +91 44 22574252. study is mainly directed towards exploring the influence of various
E-mail address: [email protected] (K. Ramamurthy). hardening methods (i.e., normal water curing, autoclaving and

0958-9465/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.cemconcomp.2008.06.006
 R. Manikandan, K. Ramamurthy / Cement & Concrete Composites 30 (2008) 848–853 849

steam curing) on the properties of cold bonded fly ash aggregate oven-dried mass. The pore system of lightweight aggregate is con-
made from class-C fly ash. The 10% fines value, water absorption, ventionally classified as open and closed pores [15]. The perme-
and porosity of aggregates cured under various curing conditions able/open porosity was determined using the below mentioned
were determined. Differences in performance of the aggregates formulae after subjecting the aggregate samples under vacuum
were discussed with the support of SEM imaging and X-ray Diffrac- saturation as per ASTM C 1202-97 [16]
tion (XRD) results.
Open porosity ðOPÞ ¼ 100  ðW sat  W dry Þ=ðW sat  W wat ÞÞ
Total porosity ðTPÞ ¼ 100  ðqt  qd Þ=qt Þ
3. Materials and methodology
where, (Wsat) and (Wwat) are the weight of vacuum saturated aggre-
Fly ash conforming to class-C as per ASTM C 618 [14] (collected gates in air and water respectively (in gram), Wdry is weight of oven-
from a nearby thermal power station) having Blaine’s fineness of dried sample (in gram), qt is the true specific gravity of fly ash
414 m2/kg and specific gravity of 2.64 and chemical composition aggregate (g/cm3) measured by pycnometer method using pow-
as shown in Table 1 was used. Pelletization of fly ash was carried dered sample passing 75 lm
out on a disc pelletizer of 560 mm diameter and 250 mm depth,
which has a provision for controlling the angle, speed and moisture Dry particle density qd ¼ ððW dry =VÞ  100Þin g=cm3 ;
content. The optimum levels of these pelletization parameters where V is volume of particles
(angle-55°, speed-55 rpm and moisture content-31%) were deter- ¼ ðW sat —W wat Þ in cm :
3

mined through a systematic experimental design to achieve maxi-

mum pelletization efficiency [13]. SEM micrographs were taken on a fractured surface of 12.5–
10 mm oven-dried aggregate. Oven-dried samples were mounted
3.1. Methods of curing on metal stubs and sputtered with gold under vacuum, before
subjecting to the electron beam from a JEOL–JSM 840A Scanning
Green pellets or raw pelletized fly ash aggregate, due to its low- Electron Microscope.
er strength, was inadequate for its use in concrete or any other
application, and hence the relative effectiveness of various curing 3.2.2. Mechanical properties
methods has been studied. The variation in properties of fly ash For aggregates whose crushing value is above 25% (Neville,
aggregates with age of normal water curing (at 24 °C) has been 2000), 10% fines value (TPFV) is recommended by BS 812-110
studied by soaking aggregates packed in jute bag for 3, 7, 14 and [17] for relative measure of strength. Hence the strength of fly
28 days before testing. Adoption of normal water curing of aggre- ash aggregate was determined through 10% fines value as per BS
gate requires large curing/stocking facility within the production 812-110 [17], on 12.5–10 mm size aggregates. TPFV was deter-
premises. If some form of accelerated curing method can be em- mined using 75 mm crushing cylinder with depth of penetration
ployed to meet the performance requirements, then the aggregates of 8 mm on 12.5–10 mm size aggregate [17].
can be produced and marketed quickly thereby saving the space
requirement even though additional energy requirement is higher. 3.2.3. Chemical properties (XRD)
Hence the influence of accelerated curing methods such as auto- Powder diffractometer using Cu Ka radiation at 40 KV and
claving and steam curing were employed to reduce the period of 30 mA was used for recording the XRD data with a range of mea-
curing. Autoclaving of fly ash aggregates was done at a pressure surement (2h) 5–60°. Powdered sample passing 75 lm was used
of 1 MPa with 2 h pressure built-up period and steam curing at in XRD analysis.
70 °C with 90 min temperature rise period. After the pressure
built-up and temperature rise period, duration of autoclaving and 4. Results and discussion
steam curing was varied from 5 h to 10 h with 1 h interval and than
cooled for 5 h. 4.1. Influence of curing methods on the properties of fly ash aggregates

3.2. Properties evaluated 4.1.1. Normal water curing

Figs. 1a and 1b shows the influence of normal water curing on
The influences of above-mentioned curing methods on the 10% fines value, water absorption and porosity. An increase in
properties of aggregates have been discussed through (i) physical the duration of normal water curing (NWC) resulted in significant
(porosity, and water absorption) (ii) mechanical (strength) and increase in 10% fines value (1.63–2.8 tonne) (Fig. 1a) and reduction
(iii) chemical (XRD) properties. The variation in properties of
aggregates with change in curing period was also supported with
3.0
microstructural studies like SEM. The properties of fly ash aggre-
Ten percent fines value, tonne

gates were measured on an oven-dried aggregate at 105 °C for 2.8

24 h, after the prescribed curing period.
2.6
3.2.1. Physical properties
2.4
Water absorption: 500 g of 12.5–10 mm size oven-dried aggre-
gate was immersed in water for 24 h and then the increased mass 2.2
of saturated surface dry aggregate was measured. The water
absorption is expressed as increase in mass as a percentage of 2.0

Table 1 1.8
Chemical characteristics of class-C fly ash
1.6
Chemical content (% by mass) 0 5 10 15 20 25 30
SiO2 CaO Al2O3 Fe2O3 MgO Na2O MnO K2O SO3 LoI Age of normal water curing, days
31.62 17.17 30.11 8.94 3.71 0.74 0.02 0.10 5.72 3.18
Fig. 1a. Variation of 10% fines value with age of normal water curing.
850 R. Manikandan, K. Ramamurthy / Cement & Concrete Composites 30 (2008) 848–853

in water absorption (21–14%) (Fig. 1b). This is attributed to the sig- hydration products (calcium silicate hydrate, calcium hydroxide
nificant reduction in open and total porosity of NWC aggregate and ettringite) from the enhanced hydration of fly ash as seen in
(i.e., 52% total porosity and 43.5% open porosity at 3 days reduced the XRD pattern (Fig. 2) and SEM (Figs. 3a and b).
to 46% and 38.5% at 28 days, respectively) as shown in Fig. 1b. When the duration of normal water curing was increased to 7
These enhancements in properties were due to the formation of days, phases like anhydrite and di-calcium silicate present in the
raw fly ash were converted into the hydration products like ettring-
ite, gypsum and calcium silicate hydrate (Fig. 2), resulting in refine-
55 55 ment of pores. The presence of unhydrated fly ash particles along
50 50 with the voids in between the fly ash particles for aggregate cured
45 at 7 days (Fig. 3a) are responsible for higher water absorption and
Water absorption, %

45
lower 10% fines values. As the duration of curing is further increased
40
40 to 28 days, maximum 10% fines value of 2.8 tonne was obtained.

Porosity, %
35 This is attributed to the formation of strength giving hydration
35
30 Water absorption products such as calcium silicate hydrate and needle shaped
30 ettringite as shown in scanning electron micrograph Fig. 3b.
25 Total porosity
20 Open porosity 25
20 4.1.2. Autoclaving and steam curing
15
An increase in duration of autoclaving from 5 h to 10 h
10 15 increased the 10% fines value from 1.85 to 2.4 tonne (Fig. 4a) and
2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
reduced the water absorption from 21% to 18.5% (Fig. 4b). For a
Age of normal water curing, days
similar increase in the same period of steam curing (between 5
Fig. 1b. Variation of water absorption and porosity with age of normal water and 10 h), an increase in 10% fines value (from 1.63 tonne to 1.92
curing. tonne) and reduction in water absorption (from 24% to 20.5%) were
observed (Fig. 4b). This behaviour is attributed to the reduction in
percentage of total and open porosity (Fig. 4c) as result of forma-
q Normal water cured tion of hydration products like calcium silicate hydrate and
e, g q zcalcium hydroxide from the enhanced lime-silica reaction [18]
ch csh c2s
c2s mr as seen in XRD pattern Figs. 5a and b. The presence of unhydrated
Intensity (arbitrary units)

28-day cured
fly ash particles and interconnected pores (Figs. 6a and c) are
q responsible for higher porosity and water absorption and lower
e, g q cshc s 10% fines value for aggregates autoclaved and steam cured at 5 h.
ch 2c s mr
2 7-day cured

q 2.50
Ten percent fines value, tonne

Steam curing
Autoclaving
2.25
ah
q c2s mr
c2s
Raw fly ash 2.00

0 10 20 30 40 50 60
1.75
2 theta
q - quartz (SiO2), ah - anhydrite (CaSO4), c2s - di calcium silicate ( Ca2SiO4)
csh - calcium silicate hydrate (Ca5(OH)2Si6O16.4H2O), mr - merwinite (Ca3mg(SiO4)2)
1.50
e - ettringite (Ca6Al2(SO4,SiO4,CO3)3(OH)12.26H2O), g - gypsum (CaSO4.2H2O), 5 6 7 8 9 10
ch - calcium hydroxide (Ca(OH)2) Duration, hours

Fig. 2. XRD pattern for raw Class-C fly ash and aggregate cured at different age. Fig. 4a. Variation of TPFV with duration of autoclaving and steam curing.

Fig. 3. Micrographs of normal water-cured aggregate at different ages.

 R. Manikandan, K. Ramamurthy / Cement & Concrete Composites 30 (2008) 848–853 851

25 Even though the XRD pattern exhibits the presence of strength

Steam curing giving hydration products (Fig. 5b), due to the formation of large
24 hydration crystals (Figs. 6c and d) along with large interconnected
Autoclaving
Water absorption, %

23 pores, the 10% fines value of steam cured aggregate was lower than
the autoclaved aggregate. As compared to the steam cured
22 aggregate, autoclaved aggregate has 25% higher 10% fines value
and 10% lower water absorption due to its dense microstructure
21
formation (Fig. 6b).
20 It is interesting to note that even though the microstructure for
autoclaved and steam cured fly ash aggregate showed the presence
19 of calcium silicate hydrate, the change in shape of hydration prod-
18 ucts along with interconnected pores (Figs. 6a–d) can be attributed
5 6 7 8 9 10 as the reason for possessing inferior properties as compared to
Duration, hours normal water cured class-C fly ash aggregate.
In order to ascertain the variation in properties of fly ash aggre-
Fig. 4b. Variation of water absorption with duration of autoclaving and steam
gate after autoclaving and steam curing, the accelerated cured fly
curing.
ash aggregate were further subjected to normal water curing up
to 28 days. The properties were determined on the aggregate after
the specified period of normal water curing and presented in Figs.
58 7a–c. An increase in duration of normal water curing of autoclaved
Solid line - Total porosity Dotted line - Open porosity and steam cured fly ash aggregates exhibit only marginal increase
56 Steam curing Autoclaving
in 10% fines value (2.4 tonne to 2.55 tonne and 1.92 tonne to 2.12
54
tonne) (Fig. 7a) and reduction in water absorption (18.5–17.5% and
52 20–19%) (Fig. 7b). This is attributed to the marginal reduction in
Porosity, %

50 porosity of aggregate as shown in Fig. 7c.

48
46 4.2. Comparison of different curing methods
44
42 A comparison of the properties of aggregates subjected to dif-
ferent curing conditions is presented in Table 2. As compared to
40
28 day normal water cured aggregate, the properties of autoclaved
38
5 6 7 8 9 10 and steam cured fly ash aggregate have relatively higher water
absorption and lower 10% fines value. However, aggregates auto-
Duration of curing, hours
claved for 10 h possessed properties closer to the normal water
Fig. 4c. Variation of porosity with duration of autoclaving and steam curing. cured aggregate (i.e., 10% fines value approximately 86% of 28 days

q q
Autoclaved Steam cured

q cshc2s csh
Intensity (arbitrary units)

Intensity (arbitrary units)

ah
10 hours
c2s csh
q csh 10 hours
mr q

q q
csh
ch c2s csh
ah c s 7 hours
q csh 2 csh mr 7 hours q
q q csh
ch c2s mr
5 hours
ah
cs
q csh 2c scsh mr q
2 5 hours
q

ah
q c2s mr
q ah c2s mr c2s
c2s Fly ash-C
Fly ash-C

0 10 20 30 40 50 60 0 10 20 30 40 50 60
2 theta 2 theta
(a) Autoclaved (b) Steam cured
Fig. 5. XRD pattern for autoclaved and steam cured aggregate.
852 R. Manikandan, K. Ramamurthy / Cement & Concrete Composites 30 (2008) 848–853

Fig. 6. Scanning electron micrograph for autoclaved and steam cured aggregate.

2.75 54
Steam curing Autoclaving Solid line - Total porosity Dotted line - Open porosity
Ten percent fines value, tonne

52 Steam curing Autoclaving

2.50 50
48
Porosity, %

46
2.25
44
42
2.00
40
38
1.75
0 5 10 15 20 25 30 36
0 5 10 15 20 25 30
Age of normal water curing, days
Age of normal water curing, days
Fig. 7a. Variation in 10% fines value of accelerated cured aggregates with further
normal water curing. Fig. 7c. Variation in porosity of accelerated cured aggregates with further normal
water curing.
21.0
Steam curing Autoclaving
20.5 Table 2
Properties of fly ash aggregates cured under various conditions
Water absorption, %

20.0
Types of curing Properties of aggregates subjected to different curing methods
19.5 Water 10% fines Total Open Saturated
absorption value porosity porosity surface dry
19.0 (%) (tonne) (%) (%) specific gravity
18.5 28 days NWC 17.0 2.8 45.9 38.6 1.95
Steam curing 20.0 1.9 51.6 42.8 1.87
18.0 for 10 h
Steam cured 19.0 2.1 50.0 41.7 1.89
17.5 aggregate after
28 days NWC
17.0
Autoclaving 18.5 2.4 49.0 40.2 1.91
0 5 10 15 20 25 30
for 10 h
Age of normal water curing, days Autoclaved 17.5 2.5 47.4 39.0 1.92
aggregate after
Fig. 7b. Variation in water absorption of accelerated cured aggregates with further 28 days NWC
normal water curing.
 R. Manikandan, K. Ramamurthy / Cement & Concrete Composites 30 (2008) 848–853 853

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