Effect of Temperature on Strength

and Microstructure of Lime Stabilized Flyash

Aparupa Pani(&) and S.P. Singh

Department of Civil Engineering, National Institute of Technology,

Rourkela, India
aparupapani@gmail.com, spsingh@nitrkl.ac.in

Abstract. Production of extensive amount of flyash from Coal-Based thermal

power plants occupies huge areas of highly serviceable land which covers a
massive area in measurement and it also creates enormous environmental haz-
ards. Utilization of fly-ash in geotechnical constructions like highway and
railway embankments, landfill, road base and sub bases etc. is gaining
momentum as it proves to be an effective and effectual mean of bulk utilization
of these kinds of materials. For increasing use of flyash as a construction
material, it is a requisite to amplify the geotechnical properties of flyash with a
suitable stabilizing agent like lime. This paper describes the effect of curing
temperature on strength properties and microstructural changes of compacted
flyash treated with lime. Specimens are prepared with different percentages of
lime compacted to densities corresponding to light and heavy compaction
energies at their respective OMC. These specimens are cured at different tem-
peratures such as 10 °C, 25 °C, 45 °C and 90 °C and the unconfined com-
pressive strength are determined after curing periods of 0, 7, 15, 30 and 60 days.
The test result showed that an increase of either lime content or curing period
results in increase in the strength. The elevated temperature is found to influence
both the early and later age strengths. Samples cured at low temperature show
rising trends of strength even up to 60 days of curing whereas the strength of
high temperature cured specimens stabilize much earlier. A crossover effect of
strength is noticed between low and high temperature cured specimens. Also it
is found that the incorporation of lime significantly increases the compressive
strength of compacted flyash. From the microstructural study it was found that
the addition of lime along with curing temperature might generate more
amorphous hydration products and accelerate the reaction rate of raw materials.

1 Introduction

Rapid growth of industrialization; scarceness in power and electricity is the leading

cause of exculpate huge amount of fly ash by thermal power plants where coal is used as
fuel. The class-F fly ash generates major environmental complications such as leaching
and dusting of atmospheric air. To mitigate these problems, fly ash can be transformed to
a construction worthy material (Subbarao and Ghosh 1997). Stabilization of the low
lime fly ash with lime and gypsum gives effective control over hydraulic conductivity
and leachate characteristics (Ghosh and Subbarao 2007). The strength enhancement
depends on the pozzolanic reaction occuring between lime and flyash (Joshi et al. 1975).

© Springer International Publishing AG 2018

D.N. Singh and A. Galaa (eds.), Contemporary Issues in
Geoenvironmental Engineering, Sustainable Civil Infrastructures,
DOI 10.1007/978-3-319-61612-4_8
102 A. Pani and S.P. Singh

Gray and Lin (1972) studied the gain in strength and the ultimate strength of lime-treated
fly ash and showed that it is sensitive to curing temperature. The lime-pozzolana
reaction required very long curing period to attain appreciable strength under ambient
temperature conditions (Reddy and Gourav 2011). The rate and mechanism of poz-
zolanic reaction of fly ash vary with curing temperature. Elevated curing temperatures
accelerate the rate of main reaction linearly (Narmluk and Nawa 2014). Formation of
‘calcium silicate hydrate’ as a result of reaction product of lime-rice husk ash was shown
by Ali et al. (1992) through XRD analysis. Ghosh and Subbarao (2001) studied the
surface morphology of lime stabilized flyash specimen and found that formation of gel
like substance of C-S-H and C-A-H found at higher doses of lime. Also, needle like
structures of ettringite is visible at long curing period. X-ray diffraction (XRD) studies
are generally employed to distinguish the crystalline phases in the stabilized fly ash.
Croft (1964) observed the appearance of gel-like varieties of CSH and CAH.
In the present analysis, an effort has been made to study the effect of elevated
curing temperature on the lime-stabilized flyash. This paper elucidates the reason of
improvement in properties of lime-stabilized fly ash through mechanical and
microstructural studies.

2 Materials
Fly ash used for this investigation was obtained from captive power plant of Rourkela
steel plant (RSP), India in dry condition. The chemical composition of the flyash is
given in Table 1. The major elements of this fly ash are silica, alumina and iron oxide.

Table 1. Chemical composition of flyash

Elements SiO2 Al2O3 Fe2O3 CaO MgO SO4 Unburnt carbon Others
Composition (%) 59.2 17.9 9.5 3.2 1.3 1.2 7.0 0.7

Fig. 1. Grain size distribution curve of fly ash

 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 103

Calcium present in the fly ash is less than 20%. So, according to ASTM specification C
618-89 (1992), this fly ash belongs to a Class-F category. The specific gravity of flyash
was found to be 2.38. The grain size distribution of the fly ash showed that it contained
88% fines (<75 lm). The Cu and Cc values were found to be 8.34 & 2.08 respectively;
indicating uniform gradation of the sample. Its gradation curve is given in Fig. 1.
Commercial grade hydrated lime of 90.2% purity was used in this study.

3 Methodology

The raw flyash blended with different percentages of lime content such as (0%, 2%,
4%, 8% and 12%) of its dry weight. These samples were condensed with two different
compactive energies i.e. 593 kJ/m3 and 2483 kJ/m3. The lime stabilized flyash
(FA) specimens prepared at compaction energy of 593 kJ/m3 were designated as L0,
L2, L4, L8, L12 and at compaction energy of 2483 kJ/m3 were designated as H0, H2,
H4, H8, H12.
Laboratory compaction tests the moisture content, dry density relationships were
found as per IS: 2720 (Part VII) 1980. From the dry density and moisture content
relationship, optimum moisture content (OMC) and maximum dry density
(MDD) were determined for both compaction energies with varying percentage of lime
are reported in Table 2.

Table 2. OMC and MDD of lime treated fly ash

Lime Compactive effort: 593 kJ/m3 Compactive effort: 2483 kJ/m3
content Maximum Dry Optimum Maximum Dry Optimum
(%) Density, MDD Moisture Density, MDD Moisture
(g/cc) Content, OMC (g/cc) Content, OMC
(%) (%)
0 1.12 40.5 1.236 33
2 1.085 43 1.206 35.8
4 1.089 42 1.237 35
8 1.097 41.5 1.244 34.8
12 1.108 41.3 1.25 34.5

Unconfined samples were prepared in sealed condition at compaction energy of

2483 kJ/m3 to their corresponding MDD at OMC. Sealed specimens were made to
maintain the actual moisture content during the course of curing. Samples were wax
coated for 10 °C, 25 °C, 45 °C temperature and covered with heat resistant wrapper for
90 °C temperature and cured for 0, 7, 15, 30, and 60 days in a temperature controller
unit as shown in Fig. 2. These test specimens (50 mm in diameter and 100 mm in
height) were cured at a temperature of 10 °C, 25 °C, 45 °C and 90 °C and sheared at
an axial strain rate of 1.25 mm/min till failure of the sample after specified curing
periods. Three identical specimens were tested for each condition and the average value
was specified.
104 A. Pani and S.P. Singh

Fig. 2. Curing of unconfined samples in temperature controlled chamber

For CBR study the test specimens were prepared for both soaked and unsoaked
condition according to IS: 2720(Part XVI)-1987 in a rigid metallic cylindrical mould
having diameter of 150 mm and a height of 175 mm. The samples were prepared for
both the compactive energies with separate percentage of lime at their respective MDD
and OMC cured for 7 and 30 days (4 days of soaking before testing for soaked
samples) before testing. Furthermore, the specimens were tested after specified curing
periods in a mechanical loading machine equipped with a movable base that moves at a
uniform rate of 1.2 mm/min.
The X-ray diffraction tests were used to determine the hydration product appeared
in the lime treated specimen after specified curing periods by using Philips X’PERT
high score. The samples were prepared from the fractured unconfined specimens and
soaked in an anhydrous ethanol to stop further hydration. Microscopic study were
undertaken to examine the morphology and microstructure of hydrated specimens.
These were done by a JEOL 6480 LV scanning electron microscope.

4 Results and Discussions

4.1 Moisture Content and Dry Density Relationship

The variation of maximum dry density with their respective optimum moisture content
at different compactive energy and lime content are presented in Figs. 3 and 4. Initially
with increase in compaction energy and lime content maximum dry density decreases
and optimum moisture content increases but after certain point of deflection the
maximum dry density increases and optimum moisture content decreases. Formerly,
illustrated that in Fig. 1 the fly ash mostly comprises of fine sand to silt size particles
with uniform gradation therefore, the particle-particle inter connectivity pores gets
filled by lime water and minor flocculation occurs resulting higher initial dry density
and lower optimum moisture content.
 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 105

Fig. 3. Variation of MDD with lime content

Fig. 4. Variation of OMC with lime content

4.2 Unconfined Compressive Strength

4.2.1 Effects of Compaction Energy
Unconfined compressive strength tests were carried out on treated flyash specimens
compacted to their corresponding maximum dry density at optimum moisture content
with both the compaction energy. The relation between compactive energy and strength
are directly proportional to each other. The increase in unconfined compressive strength
106 A. Pani and S.P. Singh

of specimen with increase in compactive effort is ascribed to the closer packing of

particles, resulting in increased interlocking among particles. A closer packing is also
responsible in increasing the cohesion component in the sample resulting in gain in
strength. Additionally, the unconfined compressive strength depends on the doses of
lime as well as the curing period. From Fig. 5 it is seen that as the curing period
increases from 7 days to 60 days at 2% lime there is not much gain in strength observed
at both compaction energies. Furthermore, at 2483 kJ/m3 compaction energy with 8%
lime content the achieved strength gives better result than 12% lime at 595 kJ/m3 with
longer curing period.

Fig. 5. Comparisons between different compaction energy at different lime content and curing
period

4.2.2 Effects of Curing Temperature

The UCS value is found to change from 300 to 520.5 kPa with change in lime content
from 0 to 2% indicating that the gain in strength is not so remarkable with smaller
amount of lime; the strength enhancement is practically insignificant, even if cured for
longer period of time. But a higher dose of lime that is beyond 2% enhances the
unconfined strength by many folds. This conveys that about 2% of lime is used for
colloidal type of reaction and lime in excess to this amount is utilized for pozzolanic
reaction. As the lime percentage and curing period increases this facilitates the poz-
zolanic reaction that form cementitious gel of CSH and CASH that binds the particles.
The process of pozzolanic reaction is improved with longer curing period which results
higher strength.
The elevated temperature is very much susceptible to unconfined compressive
strength; it is found to influence the sealed unconfined specimens. At higher temper-
ature with additional percentage of lime the UCS shows a remarkable increase in
 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 107

strength. However, flyash added with lower percentage of lime does not show this
trend. This indicates that higher temperature favors a better pozzolanic reaction than a
lower temperature especially when the lime content is high. Higher curing temperature
(90 °C) favours an early strength gain, but the strength at a later age is found to be
lower than the samples cured at moderate temperatures like 25 °C and 45 °C. Samples

Fig. 6. Unconfined compressive strength of specimens cured at 10 °C

Fig. 7. Unconfined compressive strength of specimens cured at 25 °C

108 A. Pani and S.P. Singh

cured at low temperature such as at 10 °C shows rising trends of strength even up to 60

days of curing whereas the strength of high temperature cured specimens stabilize
much earlier. A crossover effect of strength is noticed between low and high temper-
ature cured specimens. This indicates that more the lime content more the water needed
to complete the pozzolanic reaction. Hence it is recommended that ash samples sta-
bilized with higher amount of lime should either be compacted wet of OMC or suf-
ficient water be added subsequently for proper curing. Shows in Figs. 6, 7, 8 and 9.

Fig. 8. Unconfined compressive strength of specimens cured at 45 °C

Fig. 9. Unconfined compressive strength of specimens cured at 90 °C

 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 109

4.3 California Bearing Ratio

4.3.1 Effects of Curing Period and Lime Content
The variation of CBR value due to increase in lime content and curing period with both
the compactive energy are presented in Figs. 10, 11, 12 and 13. It is clearly visible that
CBR value increases with increase in compaction energy. The unsoaked and soaked

Fig. 10. Variation of soaked CBR with lime content for 7 days cured specimen

Fig. 11. Variation of unsoaked CBR with lime content for 7 days cured specimens
110 A. Pani and S.P. Singh

Fig. 12. Variation of soaked CBR with lime content for 30 days cured specimens

Fig. 13. Variation of unsoaked CBR with lime content for 30 days cured specimens

CBR values are found to increase with increase in lime content beyond 4% which gives
marginal strength. Also, the Soaked and unsoaked CBR value gives lesser value when
cured for 7 days; as curing period increase up to 30 days these values are slightly
increased due to presence of some short of cementing material (free lime). So, higher
doses of lime treatment needed for better strength.
 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 111

The soaked CBR value of flyash is relatively low ranging from 1.3% to 5.8% as
compaction energy increases from 595 to 2483 kJ/m3. However, the flyash treated with
12% lime gives comparatively higher CBR value of 44.2% after 7 days in soaked
condition. When the sample subjected to a curing period of 26 days and a soaking period
of 4 days, CBR value considerably increases due to pozzolanic reaction of lime. This
phenomenon occur mainly because fly ash, a fine-grained material, when placed at 95%
of Proctor maximum dry density and corresponding water content, exhibits capillary
forces, in addition to friction resisting the penetration of the plunger and thus high values
of CBR are obtained. On the contrary, when the same fly ash samples are soaked for 24 h
maintaining the same placement conditions, they exhibited very low values of CBR. This
can be attributed to the destruction of capillary forces under soaked conditions.

Fig. 14. X-ray diffraction pattern of lime stabilized flyash specimens cured at different
temperature (Q – Quartz, E – Ettringite, C – Calcium carbonate, CASH – Calcium aluminium
silicate hydrate, CSH – Calcium silicate hydrate)
112 A. Pani and S.P. Singh

4.4 Chemical Composition and Micro-Structure

The X-ray diffractographs and scanning electron micrographs of fly ash specimen treated
with 8% lime cured at 10 °C, 25 °C, 45 °C and 90 °C for 30 days are presented in
Figs. 14 and 15. It is observed that the samples stabilized at lower temperature i.e. 10 °C
give more number of ettringite peaks at (2H = 33.2°, 40.37° and d-spacing = 2.696Å,
2.23 Å) and calcium aluminum silicate hydrate (2H = 47.55° and d-spacing = 1.912Å).
Increasing the curing temperature from 25 °C to 45 °C resulted supplementary peaks
of low intensity of ettringite. Those peaks of ettringite get disappeared when the
treated specimen cured at 90 °C and more CSH/CASH peaks were appeared
(d-spacing = 1.541Å, 2H = 60.003).
An analysis of the micrographs showed that an interlocking network of the poz-
zolanic reaction products has been formed in the specimens containing 8% lime cured
at 90 °C shown in Fig. 15(d). The needle-like crystals of ettringite exist in the
hydration product at lower temperature of 10 °C which get gradually disappeared with
increase in temperature from 25 °C to 45 °C and then 90 °C. At higher curing tem-
perature the ettringite get wrapped with a cementitious substance of calcium silicate

(a) 10°C+8%Lime+30Days (b) 25°C+8%Lime+30Days

(c) 45°C+8%Lime+30Days (d) 90°C+8%Lime+30Days

Fig. 15. Microstructure of lime treated flyash specimens cured at different temperatures
 Effect of Temperature on Strength and Microstructure of Lime Stabilized Flyash 113

hydrate or calcium aluminium silicate hydrate gel which gives early gain in strength.
These compounds are already found in texture analysis. Extension of the curing
temperature enhanced the pozzolanic reaction and formation of hydration products.

5 Conclusions
• Maximum dry density of compacted specimens is found to change from 1.12 to
1.236 g/cc with change in compaction energy from 595 kJ/m3 to 2483 kJ/m3,
whereas the OMC is found to decrease from 40.5 to 33%. This shows that fly ash
sample responds very poorly to the compaction energy.
• Increase in curing period of lime treated fly ash specimen shows improvement in the
unconfined compressive strength. But with smaller amount of lime that is 1%–2%
the strength improvement is practically insignificant, even if cured for long time.
This is similar to the colloidal reaction with lime, which is mainly responsible in
modifying the physical properties not the mechanical strength. As the lime per-
centage increases this facilitates the pozzolanic reaction that form cementitious gel
that binds the particles. The process of pozzolanic reaction is improved with curing
period which results higher strength.
• The unconfined compressive strength of flyash added with higher percentage of
lime show a remarkable increase in strength with increase curing temperature.
However flyash added with lower percentage of lime does not show this trend. This
indicates that a higher temperature favours early strength gain and better pozzolanic
reaction than a lower temperature especially when the lime content is high.
• Both the unsoaked and soaked CBR values are found to increase with lime content
up to 4% beyond which the increment is marginal. This trend is observed for
specimens cured for 7 days. However specimens cured for 30 days showed a
continuous increase in CBR value with lime content. This indicates that the reaction
of lime with flyash is slow and a higher curing period is needed to complete the
pozzolanic reaction.
• From the diffraction study the new amorphous humps of calcium aluminium silicate
hydrate, calcium silicate hydrate and ettringite with low intensity are detected.
Abundance of needle-like structures of ettringite is found in the specimen at lower
temperature. As curing temperature proceeds up to 90 °C the needle shaped crystals
are seen wrapped with gel like substances of calcium silicate hydrate (CSH) and
calcium aluminium silicate hydrate (CASH) gel which takes a major role in strength
enhancement.

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