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Effect of calcium content on soil stabilisation with alkaline activation

Nuno Cristelo
a,
, Stephanie Glendinning
b
, Lisete Fernandes
c
, Amndio Teixeira Pinto
d
a
Trs-os-Montes e Alto Douro University, Portugal UTAD, Quinta de Prados, Engenharias I, 5000-801 Vila Real, Portugal
b
Reader in Environmental Geotechnics, Newcastle University, UK
c
Electronic Microscopy Unit, Trs-os-Montes e Alto Douro University, Portugal
d
Trs-os-Montes e Alto Douro University, Portugal
a r t i c l e i n f o
Article history:
Received 15 February 2011
Received in revised form 3 October 2011
Accepted 4 October 2011
Available online 26 November 2011
Keywords:
Soil stabilisation
Alkaline activation
Industrial waste
Soil cement
a b s t r a c t
This paper in concerned with the role of calcium content in y ash used to stabilise soft soils through
alkaline activation with sodium-based alkaline activators. A 10 molal sodium hydroxide solution was
used to activate y ash at solution: ash ratios of 2:1 and 4:1, and at a solution: (soil + ash) ratio of
0.40. Fly ash type C, with higher calcium content (FAC), and type F, with lower calcium content (FAF) were
used separately, and soilcement (SC) and soillime (SL) mixtures were also tested. Comparing the
strength of the FAC and FAF mixtures, the results showed that short-term compressive strength was
higher for FAC. However, after longer curing FAF mixtures achieved signicantly higher strength levels
than SC or SL mixtures. The same relative behaviour was reported when FAF strength results were com-
pared with SC or SL mixtures, i.e., the former achieved lower strength than the latter in the short term,
but for longer curing periods FAF strength was signicantly higher. XRD (X-ray diffraction), SEM (Scan-
ning Electron Microscopy) and EDS (Energy Dispersive Spectroscopy) analysis showed material modica-
tions that can be related to the strength results. The main conclusion is that low calcium y ash is a better
source for long term soft soil stabilisation with alkaline activation than high calcium y ash.
2011 Elsevier Ltd. All rights reserved.
1. Introduction
In general terms, alkaline activation is a reaction between alu-
mina-silicatematerials andalkali or alkali earthsubstances, namely:
ROH, R(OH)2), R
2
CO
3
, R
2
S, Na
2
SO
4
, CaSO
4
2H
2
O, R
2
(n)SiO
2
, in which
R represents an alkaline ion like sodium(Na) or potassium(K), or an
alkaline earth ion like Ca. It can be described as a polycondensation
process, in which the silica (SiO
2
) and alumina (AlO
4
) tetraedrics
interconnect and share the oxygen (O) ions. The process starts when
the high hydroxyl (OH

) concentration of the alkaline medium


favours the breaking of the covalent bonds SiOSi, AlOAl and
AlOSi from the vitreous phase of the raw material, transforming
the silica and alumina ions in colloids and releasing them into the
solution. The extent of dissolution depends upon the quantities
and nature of the alumina and silica sources and the pH levels. In
general, minerals with a higher extent of dissolution will result in
higher compressive strength after the process is complete.
At the same time, the alkaline cations Na
+
, K
+
or Ca
2+
act like the
building blocks of the structure, compensating the excess negative
charges associatedwiththemodicationinaluminiumcoordination
during the dissolution phase. Duxson et al. [11] demonstrated that
sodium, when used as the alkaline agent, is incorporated into geo-
polymeric binders only via a charge-balancing role with aluminium.
Several authors [8,18,13] report that the polymeric gel, formed
immediately after the activator comes in contact with the silica/
alumina source, has a Si/Al ratio of around one. Since the silica per-
centage present in the soil is signicantly higher than alumina, this
ratio can be explained by the fact that the weaker AlO bonds are
more easily broken than SiO, which means that at an early stage
of the reaction process more aluminium ions will be available. As
the reaction evolves, the aluminium source diminishes while silica
continues to be dissolved into the matrix, increasing the Si/Al ratio.
The resulting products accumulate for a period of time, forming
a high mobility ion soup. If calcium is present in the mixture in
signicant amounts the dissolved AlSi complex will diffuse from
the solid surface and produce a dominant CSH gel phase. Other-
wise a poly-condensation process occurs in which Si and Al ions
precipitate around the nuclei points, sharing all oxygen ions, and
form a SiOAl and SiOSi three-dimensional structure (the for-
mation of AlOAl is not favoured). This is a more stable structure
than those existing in the original aluminosilicate source (Granizo,
1998). The resulting polymeric AlOSi bonds are the main struc-
ture of the new material.
To enhance activation results, the source of alumina and silica
should rstly be subjected to thermal treatment in order to reduce
0950-0618/$ - see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2011.10.049

Corresponding author. Tel.: +351 966 193 212; fax: +351 259 350 356.
E-mail addresses: ncristel@utad.pt (N. Cristelo), stephanie.glendinning@
newcastle.ac.uk (S. Glendinning), ume@utad.pt (L. Fernandes), ateixeirapinto@
gmail.com (A.T. Pinto).
Construction and Building Materials 29 (2012) 167174
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the amount of crystallisation water and alter the structural order
between the aluminiumand the oxygen ions. An amorphous chem-
ical structure is created, with a very reactive chemical response.
Since y ash has already undergone thermal treatment, together
with the fact that it is an abundant waste material with few appli-
cations, makes it an ideal source of silica and alumina for alkaline
activation. However, the calcium percentage in the y ash is an
important and sometimes neglected consideration. Fly ash is ob-
tained fromthe combustion of coal, consisting of the inorganic mat-
ter that did not burn during the process. If a sub-bituminous coal is
used the resulting ash will be classied as type C due to its higher
amounts of calcium[2]. This type of ash has self-cementing proper-
ties, which means that in theory water is the only additive needed
to hydrate this material and form cementitious products similar to
those obtained from Portland cement. If a bituminous coal is used
the resulting by-product is classied as class F y ash (calciumusu-
ally not higher than 5%), with no self-cementing properties [12]. It
is clear that the calciumpercentage has a major impact on the prop-
erties of y ash as a construction material, even when no alkaline
agent is used to enhance its behaviour. Antiohos and Tsimas [1]
added quicklime to cement and y ash mixtures and concluded that
it increased both the early and long-term strengths. Temuujin et al.
[19] studied the effect of calcium compounds on the mechanical
properties of y ash based geopolymers and concluded it had a po-
sitive effect when the samples were cured at ambient temperature,
but reduced their mechanical strength when they were cured at
elevated temperatures. According to Fernandez-Jimenez et al.
[13], aluminosilicate gels formed after short reaction times are
not homogeneous, since some ash particles react earlier than
Table 1
Chemical composition of the original soil (wt.%).
Mg Al Si K Ca Fe Others
8.48 15.80 49.12 9.20 6.77 9.42 1.21
Table 2
Soil properties.
Plastic limit 19.7%
Liquid limit 51.9%
Optimum water content 18%
Maximum dry density 20.8 kN/m
3
Fines fraction 52%
UCS (optimum water content) 60100 kPa
Fig. 1. Micrograph and EDS characterisation of the y ash type C in general.
Fig. 2. Micrographof the y ashF (a) and EDS characterisationof areas A(b) and B(c).
168 N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174
others, whether because of their composition and/or size. Mechan-
ical properties depend strongly on the formation of a continuous
precipitate that surrounds unreacted y ash particles, with any dis-
continuity reducing considerably the mechanical performance.
However, the same authors also claim that the immediate coverage
of y ash particles slows down or completely stops the dissolution
of silica and alumina since it restricts the access to the rawmaterial
source.
An increasing amount of research resources are being directed
to the study of alkaline activation of y ash for many different
applications. Recently, some attention has been given to its appli-
cation to the stabilisation of soft soils [9,10]. The aim of the re-
search described herein is to clarify the effect on compressive
strength of the calcium percentage in the y ash used as a source
of silica and alumina in alkaline activation, specically when it is
used for soil stabilisation. The activator used was composed of so-
dium hydroxide and sodium silicate. Two types of y ash were
used. The samples were tested after different curing periods, and
the results compared with those obtained from similar tests on ce-
ment and lime stabilised soil. The specic objectives were to:
Compare the relative strength evolution between class C and
class F y ash over a curing period of up to 12 weeks.
Compare the mechanical properties of both y ash mixtures
with those obtained with more common additives, specically
cement and lime.
Quantify the effect of the y ash on strength gain by activating
mixtures of pure soil.
Identify the chemical and mineralogical basis for the different
strength development behaviour exhibited by the samples.
2. Methodology
The soil used was a marl or marlstone with a high calcium carbonate content
(Table 1), collected from the Portuguese region of Leiria, and was sieved down to
fractions below 1.18 mm prior to mixing. Characterisation tests were performed
in accordance with BSI British Standards [36] (Table 2). The sieve analysis showed
the presence of 52% particles smaller than 0.063 mm, based on which the soil was
classied as CH (inorganic clays of high plasticity, fat clays). The X-ray diffraction
(XRD) pattern showed the presence of quartz, kaolinite and muscovite (mica).
Type C and type F y ash were obtained from a pulp and paper company, and a
thermo-electric plant, respectively. Characterisation was carried out by Scanning
Electron Microscopy (SEM), together with chemical analysis by Energy Dispersive
Spectroscopy (EDS) (Figs. 1 and 2) and X-ray diffraction (XRD) (Fig. 3).
The alkaline activator solution used was prepared from sodium silicate and so-
dium hydroxide, both in solution form. The sodium silicate had a specic gravity of
1.5 and a SiO
2
:Na
2
Oratio of approximately 2:1 by mass. The sodiumhydroxide, orig-
inally in ake form, had a specic gravity of 2.13 at 20 C and 9599% purity, and was
solvedinwater uptoaconcentrationof 10 molal. Thesodiumsilicate/sodiumhydrox-
ide ratio by mass was 2, with an activator/solids ratio of 0.4 [10,20,14]. The cement
Fig. 3. X-ray diffraction pattern of the y ash class C (a) and class F (b).
Table 3
Mixture designation and composition (wt.%).
Designation Soil Fly ash Cement Lime Liquid phase
C F
A0 70.0 30.0 (activ.)
C10 64.3 7.1 28.6 (activ.)
C20 57.2 14.2 28.6 (activ.)
F10 64.3 7.1 28.6 (activ.)
F20 57.2 14.2 28.6 (activ.)
CEM10 83.2 8.4 8.4 (water)
CEM20 66.4 16.8 16.8 (water)
L6 72.3 4.6 23.1 (water)
L12 67.7 9.2 23.1 (water)
Fig. 4. UCS evolution with curing time.
N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174 169
used was a Portland cement Type II/B-L, class 32.5 N, prepared with a water/cement
ratio of 1. Two different soilcement mixtures of 10% and 20% cement by dry mass
were considered. Calcium hydroxide Ca(OH)
2
in powder form with 95% purity was
used to prepare two different soil/lime mixtures with 6% and 12% of the total dry
(soil + lime) mass, and in both cases the water/solids ratio was 0.30. The composition
and designation of all the mixtures prepared and tested is shown in Table 3.
A simple 600 Wsmall kitchen appliance was used for mixing. This propeller type
mixer achieves its purpose due to axial and turbulent ow, and is suitable for sus-
pensions with viscosities up to 20 Pascal-Seconds [16]. After mixing for 3 min the
samples were cast into 38 mm moulds by tapping the mould continuously for 25
30 s for each of the three layers. These were then left in a sealed container. Before
the start of the mixing process, and because the reaction between the sodiumsilicate
and the sodium hydroxide is highly exothermic, the activator temperature was al-
lowed to decrease to ambient values. This was because previous work [10] showed
that using the activator at higher temperatures has a negative effect on the strength
development of the mixtures. After 48 h the samples were removed from the
moulds, wrapped in cling lm and left at ambient temperature and humidity condi-
tions (4050% RH and 1923 C). Mixtures with y ash C had enough consistency
and strength to be de-moulded after 24 h, but y ash F mixtures were still soft,
and therefore, in order to avoid any experimental discrepancy, all samples were
de-moulded after 48 h. Similar behaviour was reported by Temuujin et al. [19].
Immediately before testing, at ages of 1, 4 and 12 weeks, the samples were
trimmed to 76 mm long and tested for UCS (unconned compressive strength)
using an Instron machine model 1125, with a 100 kN capacity [3,6]. Sufcient of
every mixture was prepared to form at least three samples, and each result here
presented is an average of three tests.
Selected samples were analysed by SEM, EDS and XRD after testing. The XRD
equipment was a PANalytical XPert Pro diffractometer, tted with an XCelerator.
Fig. 5. UCS comparison between alkaline activated and cement/lime mixtures: (a)
1 week curing and (b) 12 weeks curing.
Fig. 6. X-ray diffraction pattern of the C20 mixture at 1 and 12 weeks curing.
Fig. 7. X-ray diffraction pattern of the F20 mixture at 1 and 12 weeks curing.
170 N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174
The scans covered the range 570, with a nominal step size of 0.033 2-h and time
per step of 100 s. Radiation is Cu Ka with a wavelength of k = 1.54180 A. Phase iden-
tication was carried out using the XPert accompanying software program High
Score and the ICDD database, Sets 149 (1999).
3. Results and discussion
3.1. Compressive strength
Fig. 4 shows the evolution of compressive strength over curing
periods for the activated mixtures. Mixture A0, without y ash,
showed the lowest strength at both 4 and 12 weeks curing. This
was expected, but it is worth mentioning that there was a slight in-
crease from 4 to 12 weeks, which could only happen because the
activator was able to dissolve some silica for the reactions to occur.
Even at 4 weeks there was some improvement compared to the
raw soil whos original strength was 100 kPa. At 1 week curing
the C20 mixture developed a signicantly higher UCS than the
F20 mixture. This difference in strength was obvious since after
de-moulding the type F samples had not hardened after several
days. However, although the rate of increase in UCS in the C20
mixture is steady up to the 12 weeks curing, the rate of increase
in UCS in the F20 sample is signicantly higher. This resulted in
the UCS of the F20 mixture becoming 38% higher than the UCS of
the C20 mixture after just 4 weeks curing. This difference further
increased between the 4th and the 12th weeks, and there is reason
to believe that it would not continue for a longer period since pre-
vious research showed that the strength increase of soil improved
with y ash F is still active after 1 year [10].
This behaviour can also be seen when comparing the F10 mix-
ture with both type C mixtures C10 and C20. In fact, at 4 weeks
curing F10 has the lowest strength of all combinations (excluding
A0). However at 12 weeks it has a UCS 41% higher than both C10
and C20. Winnefeld et al. [21] compared the strength gain between
low and high calcium y ashes and concluded that low calcium y
ash mortars cured for 24 h (at both 20 C and 80 C) developed
Fig. 8. Micrograph and EDS characterisation of the C20 mixture in general at
1 week curing.
Fig. 9. Micrograph and EDS characterisation of the C20 mixture in general at
12 weeks curing.
Fig. 10. Micrograph and EDS characterisation of the F20 mixture in general at
1 week curing.
Fig. 11. Micrograph and EDS characterisation of the F20 mixture in general at
12 weeks curing.
N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174 171
higher short term strength gains than high calcium y ash mortars
cured in the same conditions.
Comparing the effect of the amount of y ash on the UCS devel-
opment for both types of y ash mixtures (C10 with C20, F10 with
F20), it is clear that this is far more important for y ash type F than
for type C. In fact, when the y ash content increases from 10% to
20% the UCS increases about 288% (4 weeks) and 207% (12 weeks)
for y ash type F and just 117% and 146% for type C.
Fig. 5a compares UCS at 1 week curing between both 20% y ash
mixtures (C20 and F20) with the 20% cement (CEM20) and 12%
lime (L12) mixtures. Although the C20 mixture has a signicantly
higher strength than the F20 mixture, it still is inferior to both
the cement and lime mixtures. This could imply that using alkaline
activation of y ash C or F for soil stabilisation is not the best op-
tion for short term strength gain when compared to more tradi-
tional binders like cement or lime. However, Fig. 5b shows that
at 12 weeks curing both alkaline activated mixtures (C20 and
F20) developed a higher strength than cement (CEM20) or lime
mixtures (L12). For this curing period (12 weeks) the type F mix-
tures achieved an UCS almost 4 times that obtained for the cement
mixtures. This gure shows also that at 12 weeks the highest
strength for the cement/lime group was obtained for CEM10 and
that is only slightly higher than the lowest strength obtained for
the alkaline activated group (C10). The fact that CEM10 achieved
better results than CEM20 is probably related to the higher water
percentage used in the CEM20 mixture, since an increase in water
content usually reduces cement strength [15]. Also, the higher lime
percentage in L12 had probably a detrimental effect on its strength
development due to carbonation [17], responsible for the lower
UCS obtained when compared with L6.
3.2. XRD analysis
XRD spectra of mixtures C20 and F20 at 1 and 12 weeks curing
were analysed in order to detect any signicant modication in its
mineralogical structure. Comparing the spectra of the C20 mix-
tures at the referred curing periods (Fig. 6) it is possible to detect
that most crystalline phases decreased with curing time, meaning
that more material was used in the development of the geopoly-
meric matrix, which is probably related with the reported strength
increase during this period. The same can be observed for the F20
mixtures (Fig. 7). A similar conclusion was reported by Villa et al.
[20].
3.3. SEMEDS characterisation
Figs. 8 and 9 show micrographs of the C20 mixture at 1 and
12 weeks curing, respectively. No intact y ash particles can be de-
tected at 1 week curing, and the precipitation gel appears evenly
distributed. Also, no signicant differences between the two curing
phases are perceptible, at least at this magnication, probably
meaning that whatever changes happened, they probably hap-
pened during the 1st week of curing. This clearly was not the case
with the F20 mixtures, as can be seen by comparing the overall
structure at 1 week curing (Fig. 10) with the more homogeneous
structure after 12 weeks (Fig. 11). In this case, intact y ash F par-
ticles are smaller at 12 weeks, with the precipitated gel covering
several areas of what appears to be ash particles. This difference
between both mixtures is probably due to the difference in their
respective dissolution/precipitation rate. As suggested by Temuu-
jin et al. [19], it is probable that the higher initial dissolution of
the C20 mixture, responsible for its initial higher strength
improvement when compared with the F20 mixture, is related to
a raised alkalinity, derived from the loss of water due to the almost
immediate formation of CSH and CAH phases. However, the
slower dissolution (and consequent lower short-term strength
gain) of the F20 mixtures allowed more time for the formation of
a well-formed SiOAl and SiOSi three-dimensional structure,
which was responsible for the higher long-term strength gain
reported.
Fig. 12. Micrograph of the C20 mixture at 40 weeks curing (a) and EDS character-
isation of areas A (b) and B (c).
172 N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174
The y ash particles still intact in the F20 mixture may be re-
lated to the relatively low ambient temperature during the curing
process. The commonly accepted model for the dissolution of the
raw material by the alkaline activator [7,13] suggests that as soon
as precipitation of the reaction products starts to occur, a layer of
gel will cover certain portions of the smaller y ash particles, pre-
venting the contact with the alkaline environment and hence any
further dissolution. Therefore, further dissolution of these intact
y ash particles is not to be expected, which prevents the forma-
tion of a more stable SiOAl and SiOSi three-dimensional struc-
ture in favour of a CSH structure.
In both mixtures some cracks can be seen at 12 weeks curing,
suggesting some shrinkage of the material, which was indeed ob-
served immediately prior to testing. The samples had smaller
height and diameter at 12 weeks curing than they did at 1 week
or when removed from the moulds.
Additional EDS analysis was made at 40 weeks curing in order
to better evaluate the effect of the chemical reactions in both mix-
tures. The change in texture of the C20 mixture from the original
y ash is clear. However not many differences are visible from pre-
vious curing periods (Fig. 12a). This can probably be correlated
with the relatively low increase in strength after 1 week curing.
However, there seems to be an increase in porosity between 12
and 40 weeks curing. The general texture of mixture F20 at
40 weeks shown in Fig. 13 is more heterogeneous than it was at
1 and 12 weeks curing, with what appears to be a signicantly
higher void area, compared to the same mixture at 12 weeks cur-
ing. In C20 (Fig. 12) and F20 (Fig. 13) mixtures a separated EDS
analysis was made for the different areas seen in each micrograph.
This analysis showed that the white areas (mark A in C20 mixture
and mark C in F20 mixture) probably correspond to geopolymeric
gel resulting from the alkaline activation process. This can be con-
cluded from the higher sodium content detected in those white
areas (Figs. 12b and 13d), when compared with the remaining
areas in both gures.
A statistical analysis based on the image constructed from sev-
eral pictures taken from the original y ash F (Fig. 14a) and the F20
mixture (Fig. 14b) at 40 weeks curing showed a reduction of 50% in
the number of round particles, whereas the average size of those
particles declined by 20%. This indicates up until the 40 weeks
mark the y ash F samples were still reacting with the activator,
which is only possible due to the slow formation of the gel. How-
ever, the slow gel formation is also responsible for the slow
strength gain at short curing periods.
Fig. 13. Micrograph of the F20 mixture at 40 weeks curing (a) and EDS characterisation of areas A (b), B (c) and C (d).
N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174 173
4. Conclusions
Results show that at 4 weeks curing the highest strength value
was obtained with the mixture containing a lower calcium per-
centage and 20% y ash. At 12 weeks curing the effect of the low
calcium content is even more evident since the mixture F10
achieved a higher strength than mixtures with C10 and C20,
CEM20 and L12. Although the activator without any source of
amorphous silica and alumina was able to increase soil initial
strength, its effect was the lowest for all the mixtures tested,
meaning that even 6% lime is a better solution to improve a clayey
soil.
XRD analysis showed dissolution of the silica/alumina phases
into the precipitated gel for both the F20 and C20 mixtures, while
SEMEDS analysis revealed a more pronounced structural evolu-
tion between 1 and 12 weeks curing for the F20 mixture than the
C20 mixture, which might explain the higher strength gain of the
former during the period. SEMEDS analysis at 40 weeks curing
accentuated the idea that low calcium mixtures continue to react
over larger periods of time, therefore achieving higher strength
levels at medium/long term. However, C20 mixture micrographs
showed a higher short term dissolution/precipitation rate of poly-
meric gel, which resulted in a higher short term strength, but at the
same time avoided the formation of well dened 3D structural
bonding. The correct development of this structure is responsible
for the higher strength gains of the F20 mixture at medium/long
term. Both C20 and F20 mixtures showed an increase in voids at
40 weeks.
Finally, it can be concluded that in the medium/long term a
lower percentage of calcium in the silica and alumina source used
for soil improvement through alkaline activation has a positive ef-
fect on mechanical behaviour, although short term strength gain is
faster in calcium-based materials like y ash C, cement or lime.
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174 N. Cristelo et al. / Construction and Building Materials 29 (2012) 167174