International Journal of Geosynthetics and Ground Engineering (2021) 7:74

https://doi.org/10.1007/s40891-021-00318-2

ORIGINAL PAPER

Mechanism of Carbonation in Lime‑Stabilized Silty Clay from Chemical

and Microstructure Perspectives
Dhanalakshmi Padmaraj1 · Dali Naidu Arnepalli1

Received: 5 May 2021 / Accepted: 25 September 2021 / Published online: 16 October 2021
© The Author(s), under exclusive licence to Springer Nature Switzerland AG 2021

Abstract
The carbonation of lime-treated soils that occurs during the short-term and long-term curing is not sufficiently explored in
the domain of lime stabilization. The present study investigates the carbonation mechanism in lime-treated silty clay treated
with two lime contents (4%, 8%) subjected to different curing periods (7, 90, 180, and 365 days). The cured samples were
exposed to accelerated carbonation, and subsequent change in the unconfined compressive strength was compared with that
of control samples tested under a nitrogen environment. The extent of carbonation was measured using phenolphthalein
solution. X-ray diffraction technique and thermogravimetric analysis were used to analyze the reaction products resulted from
carbonation. The morphology of carbonates and effects of carbonation on the pore structure were assessed using a scanning
electron microscope and mercury intrusion porosimeter, respectively. Results show that carbonation has a deleterious effect
on the performance of lime-treated clay. The strength of lime-treated soils upon carbonation decreased by 30% on average.
The fabric structure of treated clay was found to vary with lime content and curing period, which determined the extent of
carbonation. Decalcification of reaction products and cracking induced by the carbonation of residual lime contributed to the
reduction in compressive strength of treated clay. The observed strength behavior of the carbonated samples is substantiated
by quantifying the variation in pore structure characteristics.

Keywords Lime-treated soils · Pozzolanic compounds · Carbonation · Microstructure · Pore size distribution

Introduction dispersed fabric of clay then transforms into a flocculated

Rapid urbanization and industrialization have imposed the
need for utilizing problematic soils for infrastructure devel-
opment. Chemical stabilization of fine-grained soils that are
rich in clay minerals is found to be a feasible solution for
improving their engineering behavior. Lime stabilization is
an age-old conventional ground improvement method that
has been successfully adapted even in modern times by prac-
ticing engineers. When lime is added to the clayey soil, it
dissociates to form calcium ions and replaces the monova-
lent ions present in the exchangeable sites of clays. Conse-
quently, it suppresses the electrical diffused double layer
and associated charge modifications on the clay surface. The
* Dali Naidu Arnepalli
arnepalli@iitm.ac.in
Dhanalakshmi Padmaraj
dhanalakshmip93@gmail.com
1
Department of Civil Engineering, Indian Institute
of Technology Madras, Chennai 600036, India
structure and further undergoes aggregation, which reduces
the plasticity properties of clay [1, 2]. Also, the highly alka-
line nature of lime enables the dissolution of silica and alu-
mina from clays, which reacts with the calcium in the pore
solution to form various cementitious compounds. These
cementitious compounds bind the clay aggregates to modify
the engineering properties of the clay [3].
Initially, the studies on lime stabilization have primar-
ily focused on understanding stabilization mechanisms in
terms of variations in the index and engineering properties
of treated soils. The advancements in analytical tools have
helped substantiate the physicochemical mechanisms associ-
ated with lime stabilization [4–6]. However, due to the fail-
ure of various lime and cement-stabilized earthworks over
the past few decades, researchers are interested in assessing
their long-term performance by subjecting them to cycles of
wet–dry and freeze–thaw [7–9]. The two significant deleteri-
ous reactions that occur during the service life of treated soil
are carbonation and leaching of calcium from unreacted lime
and cementitious phases [10, 11]. Although considerable

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74 Page 2 of 12
research has been conducted on calcium leaching and mois-
ture susceptibility of cementitious phases [12–14], carbona-
tion has not given importance to date.
Carbonation of lime-stabilized soils refers to the inter-
action of atmospheric or microbial induced soil carbon
dioxide with the free lime and pozzolanic reaction products
to produce calcium carbonate [15]. This reaction ought to
have detrimental effects on the lime-treated soil, inhibit-
ing the progress of various pozzolanic reactions involved
in the process. Carbon dioxide competes with clay for lime
resulting in the shortage of lime for the progression of poz-
zolanic reactions. In addition to lime paucity, the carbona-
tion of lime to different polymorphs of calcite having higher
molar volume can induce tensile stress resulting in cracking
[16]. In the long term, the stability of the lime-treated soils
is compromised owing to the decalcification of reaction
products, viz., Calcium Silicate Hydrate (CSH) and Cal-
cium Aluminate Silicate Hydrate (CASH). The byproduct
of CSH carbonation is observed to be a weak silica gel,
which undergoes polymerization, and results in differential
shrinkage and formation of internal cracks [17]. To address
the above-mentioned mechanisms in cement-stabilized
soils and to quantify the variation in mechanical properties
upon carbonation, a few attempts were made in the recent
past. Nakarai and Yoshida [18] found that the strength and
stiffness of cement-treated sand increased due to lime car-
bonation. However, the observations were applicable only
to granular materials like sand, where lime carbonation
resulted in pore-filling and an overall increase in strength.
These findings were substantiated by Ho et al. [19], who
conducted carbonation studies using cement-treated clayey-
sand and confirmed that the part strength increase is due to
drying-induced suction. In addition, once the water content
reaches the hygroscopic moisture content, further drying was
stopped, and the overall strength of treated soil was reduced
due to the CSH carbonation alone.
The studies carried out in recent years to understand car-
bonation were mainly focused on cement-treated sands. The
strength changes due to carbonation alone by eliminating the
suction-induced strength have not been studied experimen-
tally by the researchers. Besides, the role of two significant
parameters, such as lime content and curing period, on the
nature and effect of carbonation has not been investigated.
Given this, the present study aims to address these gaps by
studying the changes in the mechanical behavior of com-
pacted lime-treated soil upon carbonation by considering
samples cured in a nitrogen environment as a control. Curing
under a non-reactive nitrogen environment does not initiate
carbonation as the environment is devoid of carbon dioxide.
The type of carbonates formed and the associated effects
in mineralogy and microstructure upon carbonation were
assessed for silty clay treated with two different lime con-
tents and cured for different time intervals up to 365 days.
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International Journal of Geosynthetics and Ground Engineering (2021) 7:74
Materials and Methods
Selection of Materials
Naturally occurring silty clay from a lakebed located in
the Indian Institute of Technology Madras campus, Chen-
nai, Tamilnadu, India, was chosen for the present study.
Hydrated calcium hydroxide obtained from Astrra Chemi-
cals Pvt. Ltd., Chennai, Tamilnadu, was used as an additive
in this study. An optimum lime content (OLC) of 4% was
selected based on the pH-based Eades and Grim [20] test.
To assess the effect of lime content on carbonation, the per-
centage of lime (8%) that corresponds to a maximum 28-day
unconfined compressive strength was also considered.
Basic Characterization
A detailed characterization of selected soil was carried out
by determining its physicochemical and mineralogical prop-
erties. The pH, specific gravity, consistency properties, and
grain size distribution were determined as per the ASTM
codal provisions [21–24]. To ascertain the reactivity of soil
toward lime, cation-exchange capacity and specific surface
area were determined as per the methodologies outlined in
ASTM D7503 [25] and Arnepalli et al. [26], respectively.
The chemical composition of clay and lime was evaluated
by X-ray fluorescence technique using an X-ray analytical
microscope (Horiba XGT-2700, Japan). The predominant
minerals present in the clay were identified using the powder
X-ray diffraction method (PANalytical X’PERT Pro, The
Netherlands).
Preparation and Curing of Samples
For the preparation of compacted cylindrical samples, the
air-dried soil passing through 1 mm was mixed thoroughly
with a known amount of deionized water and kept for mois-
ture equilibration for 48 h in airtight zip-lock bags. After
maturation, the moist soil was mixed with required lime
and water, and compacted dynamically to form a cylindrical
specimen of 38 mm diameter and 76 mm height by achiev-
ing the corresponding optimal conditions of the standard
Proctor test. The compacted samples were wrapped with
two layers of thin plastic film and an intermediate covering
of aluminum foil to prevent evaporation and inhibit the pos-
sibility of carbonation in the process of curing. The samples
were stored in double-decked airtight containers; the lower
deck is filled with distilled water to maintain the desired
relative humidity. These containers were then placed in a
temperature-controlled chamber maintained at 28 °C. This
procedure ensured humidity greater than 95% and constant
International Journal of Geosynthetics and Ground Engineering (2021) 7:74
temperature conditions, thereby favoring pozzolanic reac-
tions in the compacted lime-treated samples. Various curing
periods, viz., 7, 90, 180, and 365 days, were adopted for the
present study. Due to the flocculated structure, the ingress of
atmospheric gases is predominant during the initial curing
periods. Hence, the maximum period of curing was limited
to 365 days in this study.
Accelerated Carbonation
After the specified curing period, the compacted samples
were subjected to accelerated conditions of carbonation
using 3% volume/volume of ­CO2 in a carbonation cell, as
shown in Fig. 1, under a constant temperature (28ºC) and
atmospheric pressure. The literature on concrete carbonation
suggests that gas concentration up to 3% ­CO2 can mimic
the mechanism involved in natural carbonation [27, 28].
In addition, the decomposition of organic matter as low as
5% that may present in the subsoil environment can give
rise to a carbon dioxide concentration of 3%, justifying the
proposed concentration of gas used for carbonation [29].
For preparing the gas mixture containing 3% C ­ O2 and 97%
­N2, a test setup shown in the picture (Online Resource 1)
was developed, and the mixture was prepared using con-
cepts of Dalton’s partial pressure. The concentration of the
prepared gas mixture was verified to be 3 ± 0.2%, using a
gas chromatograph equipped with a thermal conductivity
detector (Agilent Technologies, USA). The carbonation cell
was purged using the gas mixture for a specified duration to
displace the existing gas inside the cell. For compensating
­CO2 consumed by the soil, gas purging was performed three
times a day. The procedure was followed for 7 consecutive
days for all lime-treated samples considered in this study.
The time for the accelerated carbonation was selected as
7 days based on the outcome of the initial trials on the extent
of carbonation. It was observed that exposure of the samples
to the carbon dioxide beyond 7 days leads to the carbonation
of the entire sample. Apart from the accelerated carbonation,
Fig. 1  Schematic diagram of the
test setup used for carbonation
Page 3 of 12 74
identical samples were subjected to the nitrogen environ-
ment by considering similar flow conditions. This procedure
was envisaged to nullify the suction-induced strength gain
from the loss of moisture during drying, which helped to
quantify the change in the strength of the lime-treated soils
due to the carbonation alone.
Mechanical and Microstructure Characterization
The variation in the mechanical behavior of lime-treated
soils due to carbonation was assessed in terms of its uncon-
fined compressive strength (UCS) as per ASTM D2166 [30].
The compacted specimens were subjected to uniaxial com-
pression at a displacement rate of 0.5 mm/min. The load
carried by the specimen and the corresponding deformation
were recorded to obtain the stress–strain characteristics and
the peak strength. For ascertaining the severity of carbona-
tion, the specimen was sliced diametrically at the mid-height
and sprayed evenly with a 1% phenolphthalein alcohol. Once
the indicator changes the color, the cross-section image of
the sample was captured using a digital camera to identify
­ O2. Furthermore, using ‘ImageJ’ soft-
the diffusion zone of C
ware, the extent of carbonation was traced, and the carbon-
ated area was calculated. The radial extent of carbonation
was irregular, and hence, percentage area under carbonation
was adopted as the parameter for comparing the extent of
carbonation.
To evaluate the severity of the carbonation, variations in
the amount of calcium carbonate and hydrated gels present
in the samples were quantified by employing the thermal
analysis technique [31]. About 15–20 mg of powdered sam-
ples were subjected to elevated temperatures using a thermo-
gravimetric analyzer (Discovery SDT650, TA Instruments,
USA) at a controlled heating rate of 10 °C/min from 30 °C to
1000 °C under a non-reactive nitrogen environment. Based
on the observed data, the variation in weight loss with the
temperature was plotted, major thermal reactions were
identified, and corresponding weight change was calculated
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74 Page 4 of 12
using ‘Trios’ software (TA Instruments, USA). The deriva-
tive of the weight loss curve was analyzed to estimate the
range of temperature at which weight loss occurred.
To substantiate the findings from thermogravimetric
analysis and to evaluate the crystalline phases and phase
transformations emanating from carbonation, powder X-ray
diffraction technique was employed. In the present study,
lime-treated samples before and after carbonation were
dried, powdered, sieved through a 75 µm sieve, and tested
using an X-ray diffractometer fitted with Cu-Kα source
(Philips X’pert PRO PANalytical, The Netherlands). The
step size used was 0.004° per second, and the counting time
was 20 s per step, over a 2θ value of 5–70°. The experi-
mentally obtained diffractograms were further analyzed to
identify various phases present in the samples, as per Inter-
national Centre for Diffraction Data database.
To visualize the morphology of pozzolanic and carbona-
tion reaction products, a high-resolution scanning electron
microscope (FEI, Quanta FEG 200F, USA) was employed.
The undisturbed sections of the samples were cut, lyophi-
lized, gold-coated, and subjected to the secondary electron
beam [32]. Besides, these undisturbed carbonated and uncar-
bonated samples were analyzed for pore size distribution
characteristics using the Pascal series mercury intrusion
porosimeter (Thermo Fisher Scientific, USA). The speci-
mens were subjected to pressure from 0 to 300 MPa at a
constant rate of 6 Pascals/min, and the intruded and extruded
volume of mercury was measured. The distribution function
dV/dlogD was used to obtain the differential pore volume
distribution to analyze and quantify the relative proportion
of various pore sizes present in the samples.
Results and Discussion
Characterization of Selected Materials
The soil has a relatively neutral pH of 7.8, with a 55% clay-
size fraction and a plasticity index of 18%. It is classified as
clays of low compressibility, as per ASTM D2487 [33]. The
physicochemical properties of untreated soil are reported in
Table 1. The cation-exchange capacity and specific surface
area are 87.1 centimol ­kg−1 and 179 ­m2 ­g−1, respectively.
These properties indicate that the soil surface is chemically
active for interaction with lime. The predominant clay min-
erals present in the soil are identified as illite and traces of
kaolinite and quartz, as shown in the X-ray diffractogram
(Online Resource 2). As per X-ray fluorescence results
reported in Table 2, the soil is rich in silica, with a silica-to-
sesquioxide ratio (SSR) of 2.30, indicating the presence of
a large amount of reactive silica for promoting pozzolanic
reactions. The chemical composition analysis performed on
hydrated lime showed 96% purity, as described in Table 2.
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International Journal of Geosynthetics and Ground Engineering (2021) 7:74
Table 1  Physical, chemical, and consistency properties of silty clay
Property Value
Specific gravity (–) 2.62
pH (–) 7.8
Cation-exchange capacity (centimol k­ g−1) 87.1
Specific surface area ­(m2 ­g−1) 179
Liquid limit (%) 44
Plastic limit (%) 26
Plasticity index (%) 18
Sand-size fraction (%) 4
Silt-size fraction (%) 41
Clay-size fraction (%) 55
USCS classification CL
Extent of Carbonation and Carbonation‑Induced
Strength Variation.
As shown in Fig. 2, the progress of carbonation does not fol-
low a uniform path as gas ingresses into the sample through
a randomly organized unsaturated network of interconnected
pores. For 4% lime-treated soil, when compared to 8%, the
carbonated area is enhanced by 40%. Also, with an increase
in the curing period up to 365 days, the zone of carbonation
in the specimen has decreased by 20% on average. For sam-
ples treated with lower lime content, the formation of insuf-
ficient and unstable cementitious gels with a low Ca/Si ratio
develops a porous and interconnected fabric structure that
favors easy permeation of gas through the gels [34]. Also,
with the progress of curing, time-dependent dissolution of
silica and alumina and subsequent precipitation of pozzo-
lanic reaction products fill the capillary pores and block the
pathway for ingress of C­ O2 gas [35]. Overall, it is observed
that the carbonation rate is mainly governed by lime content
than the curing period.
The mechanical characteristics of carbonated and uncar-
bonated specimens are illustrated in Online Resource 3.
The strength of uncarbonated samples was assessed after
subjecting them to a high-purity nitrogen environment
for 7 days. The samples cured in ­CO2/N2-rich atmosphere
have exhibited the same water contents with a variation
of ± 0.4%. Hence, the contribution of suction-induced
strength is expected to be similar in both carbonated and
uncarbonated samples. For a compacted lime-treated soil,
both unreacted lime and cementitious gels can undergo
carbonation. Carbonation of unreacted lime can either
enhance the strength of the soil by pore-filling or reduce
the strength by the phenomenon of cracking due to tensile
stresses induced by the precipitation of calcium carbon-
ate. Hence, the initial fabric developed upon curing deter-
mines the consequence of lime carbonation. Carbonation
of cementitious gels results in decalcification and loss of
International Journal of Geosynthetics and Ground Engineering (2021) 7:74 Page 5 of 12 74

Table 2  Chemical composition Material Chemical oxide constituents (%) SSR

(% by weight) of materials used
in the study SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O TiO2 P2O5

Silty clay 62.26 14.76 12.28 1.28 0.21 2.05 5.46 0.96 0.11 2.30
Hydrated lime 1.65 0.06 0.07 96.1 0.46 - - 0.01 0.02 NA

SSR silica-to-sesquioxide ratio - less than detectable limit of the equipment, NA not applicable

Fig. 2  Variation in the area (or

depth) of carbonation with lime
content and curing period

cohesion which reduces the overall strength of treated

materials [16]. To address the role of lime content and
curing period on the mechanical performance upon car-
bonation, the ratio of unconfined compressive strengths
of carbonated specimens and uncarbonated specimens was
considered. UCS of carbonated and uncarbonated samples
were assessed using the identical samples cured under sim-
ilar conditions, including the curing time. Figure 3 shows
that the UCS ratio (­ UCScarbonated/UCSuncarbonated) for both
lime contents follows an increasing trend with the curing
period. Also, the UCS ratio is comparatively lesser for 4%
lime-treated soil. During curing, continuous precipitation
of reaction products within the stabilized fabric can block
gas permeation and hence the carbonation, as observed in
Fig. 2. Also, the susceptibility of unstable cementitious
gels developed in the 4% lime-treated soil facilitates easy
decalcification giving rise to a lower strength ratio. As a
whole, the type of carbonation and the fabric of treated
soil determine the degree of variation in the mechanical Fig. 3  Variation in the compressive strength ratio of lime-treated soils
performance of lime-treated soils. It warrants the need for upon carbonation

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74 Page 6 of 12
chemical, mineralogical, and microstructure analysis of
the carbonated samples.
Variation in the Chemical and Mineralogical
Properties upon Carbonation
The weight loss curve obtained from the thermal analysis
was assessed to identify various phases from the respec-
tive range of decomposition temperature (Online Resource
4). The calcium carbonates formed upon carbonation of
residual lime and hydrated gels were quantified using the
observed thermograms. Figure 4a and b shows the weight
change and the derivative of weight change for 90 days cured
lime-treated soils upon carbonation. The peaks correspond-
ing to hydrated gels (240–300 °C) indicate the presence of
residual pozzolanic compounds. Figure 4b shows two peaks
in the temperature range of 550–710 °C. Though pure cal-
cites have a decomposition temperature of 898 °C, when
adulterated with silicate minerals like clays, their decompo-
sition temperature reduces [36]. To ascertain the nature of
carbonated compounds, the gas emanated from thermogravi-
metric analyzer was analyzed using Fourier transform infra-
red spectrometer with the help of a TGA-IR hyphenation
Fig. 4  Thermogravimetric response and infrared absorbance spectra of carbonated lime-treated soil cured for 90 days
13
International Journal of Geosynthetics and Ground Engineering (2021) 7:74
module (Thermo Fischer Scientific, USA). As shown in
Fig. 4c, the absorbance region of C ­ O2 coincides with the
first peak after 550 °C and ends at 710 °C, confirming the
decomposed compounds in the temperature range to carbon-
ates. Moreover, the study conducted by Villain et al. [37]
suggests that the primary peak (550–650 °C) is due to the
decomposition of amorphous carbonates and the secondary
peak (650–710 °C) is related to the crystalline polymorphs
of calcium carbonate.
The weight loss corresponding to hydrated gels in both
carbonated and uncarbonated specimens was calculated, as
shown in Fig. 5a, b. It can be observed that with the increase
in curing time, the amount of hydrated gels increased due
to the progressive pozzolanic reactions. Whereas upon car-
bonation, it was reduced in all lime-treated soils. These
observations suggest that hydrated gels underwent decal-
cification from carbonation to reduce the cohesion and
overall UCS. The relative amounts of different types of
carbonates, Type I carbonates (550–650 °C) and type II
carbonates (650–710 °C) in all samples, are quantified and
presented in Fig. 5c, d. The 7-day cured lime-treated soils
show maximum carbonation indicating the presence of a sig-
nificant fraction of unreacted lime and unstable cementitious
International Journal of Geosynthetics and Ground Engineering (2021) 7:74
Fig. 5  Variations in the weight
loss of a, b hydrated phases
[240–300 °C] and c, d carbon-
ates [550–710 °C] formed upon
carbonation
products. The percentage of type I carbonates is lowest for
7-day cured samples, whereas it is highest in the carbonated
samples that are cured for the long term. These observations
strongly indicate that type I and Type II carbonates have
evolved from hydrated gels and unreacted lime, respectively.
From 90 days of curing, the quantity of type I carbonates
increased with curing in 4% lime-treated soils, whereas it
decreased in 8% lime-treated soils. In the case of 4% lime-
treated soils, progressive lime consumption with curing
leads to the formation of excess cementitious gels with a
low Ca/Si ratio, which favored easy carbonation [38]. On
the contrary, higher lime content favors the dissolution of
silica and contributes to the formation of dense cementitious
gels, which crystallize and prevents the permeation of gases
through the lime-treated soil [39, 40].
Furthermore, the changes in the intensity of cementitious
phases and the various polymorphs of calcium carbonates
formed upon carbonation were identified using X-ray dif-
fractograms of uncarbonated and carbonated soils, as shown
Page 7 of 12 74
in Fig. 6. The presence of peaks (Fig. 6b) corresponding to
reaction products, denoted as CSH and CASH (21.9° and
28.02°, respectively), indicates the progress of pozzolanic
reaction of lime and clay [41, 42]. However, upon carbon-
ation, the intensity of these peaks (Fig. 6c) reduced with
the formation of peaks corresponding to calcites (29.31°,
43.01°) and vaterites (22.94, 43.84°). The intensity of
peaks corresponding to carbonates decreased as the curing
period increased. The observed trend can be attributed to the
enhanced durability of treated soil to carbonation with time.
Variation in Microstructure and Pore Size
Distribution Properties upon Carbonation
The microstructure of reaction products precipitated via
pozzolanic and carbonation processes is presented in
Fig. 7. Nodule-like structures of CASH are observed in the
uncarbonated specimens (Fig. 7a), which indicate pozzo-
lanic reactions between clay and lime. Figure 7b shows the
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74 Page 8 of 12 International Journal of Geosynthetics and Ground Engineering (2021) 7:74

Fig. 6  X-ray diffractograms of

lime (8%)-treated soils cured
for a 7 days and carbonated,
b 90 days and uncarbonated,
c 90 days and carbonated, d
180 days and carbonated, and e
365 days and carbonated

Fig. 7  a Formation of CASH precipitates, b micro-crack formed after carbonation, c, d rhombohedra calcite structures, and e, f nano-sized car-
bonates

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International Journal of Geosynthetics and Ground Engineering (2021) 7:74
formations of micro-cracks, and Fig. 7c and d shows rhom-
bohedral calcite structures in carbonated samples treated
with 4% lime. The formation of calcium carbonates with
molar volume higher than lime gives rise to the expansion
of the soil–lime composite resulting in micro-cracks. Also,
Fig. 7e and f shows irregular, nano-sized amorphous struc-
tures of calcium carbonates formed in carbonated 180-day
cured clays similar to that observed by Cizer et al. [43],
indicating CSH carbonation.
In addition to morphological characterization, the effects
of curing and carbonation on the porosity and pore size dis-
tribution of samples considered in the study were examined.
The pores present in the lime-treated soils belong to three
different categories, viz., large capillary pores (3–100 µm),
Fig. 8  Variation in the pore size
distribution of lime-treated soil
upon carbonation
Page 9 of 12 74
medium capillary pores (0.1–3 µm), and small capillary
pores or gel pores (0.005–0.1 µm), as shown in Online
Resource 5. Based on the experimentally observed pore
size distribution characteristics, the different pores present
in the carbonated and uncarbonated samples were quantified,
as depicted in Fig. 8. It can be observed that the total pore
volume is higher for 8% compared to 4% lime-treated soils.
This must be due to increased flocculation and improved
pozzolanic reactions, increasing the fraction of large capil-
lary pores and gel pores, respectively [44]. However, with
the increase of curing period, in 4% lime-treated soils, large
and medium capillary pores increased by 60%, whereas, in
8% lime, it decreased by 30%. Also, gel pores of reaction
products are higher for higher lime content and extended
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74 Page 10 of 12
curing periods. Hence, it is understood that higher dissolu-
tion of silica and alumina in 8% lime-treated soil resulted
in enhanced precipitation of pozzolanic reaction products
with curing, which eventually contributes to filling of large
capillary pores and decrease in the total porosity [45, 46].
Lime-treated soils upon carbonation exhibited an over-
all reduction in the proportion of gel pores (Fig. 8) and an
increase in the proportion of large and medium capillary
pores. The decrease in the gel pores is related to the car-
bonation of CSH, as observed in thermal analysis (Fig. 5a,
b). The carbonated CSH with reduced cohesion fails to bind
the soil matrix and results in pore coarsening. Also, the for-
mation of polymorphs of calcium carbonate (Fig. 6) like
vaterite having higher molar volume than lime can result
in micro-cracks (Fig. 7b) which increases the porosity of
the stabilized matrix. [47]. The initial porosity of 4% lime-
treated soil is relatively less (Fig. 8), and precipitation of cal-
cium carbonate can initiate tensile stress and cracks. In addi-
tion, the percentage reduction of gel pores upon carbonation
is more for 4% lime-treated soil, which is in accordance with
the UCS ratio reported in Fig. 3.
Summary and Conclusions
The effects of carbonation on the mechanical and micro-
structure aspects of lime-treated silty clays were studied by
exposing the treated soil to 7 days of accelerated carbona-
tion. The performance of carbonated lime-treated samples
was assessed, considering the control samples purged with
nitrogen. Based on the inferences made in this study, the
following conclusions are drawn.
• The extent of carbonation was observed to be nonuniform
due to the unsaturated network of interconnected pores
in the lime-treated soil. The percentage area of carbona-
tion was significantly higher for 4% lime-treated soil than
the soil amended with 8% lime. Also, the areal extent of
carbonation was slightly reduced with the curing period.
The soils treated with higher lime content and subjected
to extended curing periods have precipitated significant
quantities of cementitious products and reduced overall
porosity due to the pore-filling process. Consequently,
this phenomenon enhanced the resistance against carbon
dioxide ingression into the lime-treated samples.
• The thermal analysis revealed that the carbonation of
lime-treated soils produced two types of carbonates
with a distinct range of decomposition temperatures. The
varying quantities of each type of carbonate with curing
suggest that carbonation of hydrated gels and unreacted
lime produced carbonates with lower and higher decom-
position temperatures, respectively. Furthermore, X-ray
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International Journal of Geosynthetics and Ground Engineering (2021) 7:74
diffraction studies revealed crystalline polymorphs, cal-
cite, and vaterite in the carbonated lime-treated soils.
• The microstructure characterization of lime-treated soils
revealed different morphology of calcium carbonate pro-
duced upon carbonation. The presence of rhombohedral
calcite structures and micro-cracks confirmed that lime
carbonation is significant during the early stages of the
curing period. Furthermore, carbonation increased large
capillary pores and reduced gel pores, substantiating
CSH decalcification and loss of particle to particle bond-
ing in the treated soil.
• The unconfined compressive strength decreased with
carbonation, especially for soils treated with lower lime
content, due to the decalcification of CSH and alteration
in the pore structure characteristics. For both lime con-
tents, the UCS ratio of carbonated and control samples
increased with the curing period owing to the progression
of pozzolanic reactions and enhanced durability.
The pertinent role of lime content and curing period is
comprehended in terms of carbonation mechanisms and
their effects on chemico-mineralogical, pore structure, and
mechanical characteristics of lime-treated soils. Overall, the
study contributed toward enhancing the current understand-
ing of the carbonation mechanism in lime-treated soils.
Supplementary Information The online version contains supplemen-
tary material available at https://​doi.​org/​10.​1007/​s40891-​021-​00318-2.
Author Contributions DP: methodology, data curation, formal analysis
and investigation, and original draft preparation. DNA: conceptualiza-
tion, supervision, validation, visualization, and writing—review and
editing.
Funding No funding was received for conducting this study.
Data Availability All data used in the study are included in the submit-
ted article.
Declarations
Conflict of Interest The authors declare that there is no conflict of in-
terest concerning the content of this manuscript.
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