Construction and Building Materials 157 (2017) 83–95

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Construction and Building Materials

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Characterization and use of an untreated Mexican sugarcane bagasse ash

as supplementary material for the preparation of ternary concretes
Venustiano Ríos-Parada a, Víctor Guillermo Jiménez-Quero b, Pedro Leobardo Valdez-Tamez c,
Pedro Montes-García b,⇑
a
Instituto Politécnico Nacional, CIIDIR-Oaxaca, Hornos 1003, Col. Noche Buena, Sta. Cruz Xoxocotlán C. P. 71230, Oaxaca, Mexico
b
Instituto Politécnico Nacional, CIIDIR Unidad Oaxaca, Grupo de Materiales y Construcción, Mexico
c
Universidad Autónoma de Nuevo León (UANL), FIC, Cd Universitaria S/N, C. P. 66451 San Nicolás de los Garza, Nuevo León, Mexico

h i g h l i g h t s

 The addition of untreated sugarcane bagasse ash (UtSCBA) was studied in ternary concretes.
 Microstructure characteristics of ternary concretes containing UtSCBA and fly ash were analyzed.
 Mechanical properties of those ternary concretes were obtained and discussed.

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

Article history: The effects of the addition of a Mexican sugarcane bagasse ash to binary concrete prepared with blended
Received 6 March 2017 Portland cement (CPC) and fly ash (FA) were studied. The sugarcane bagasse ash was used practically as
Received in revised form 11 September received (UtSCBA), with the only post-treatment application sieving through a No. 75 mm (ASTM) mesh
2017
for four minutes. The characterization of the materials used for the concrete preparation was carried
Accepted 13 September 2017
out using RXFE, XRD and SEM/EDS, and the BET methods. Besides the control mixture, three ternary con-
crete mixtures were prepared: the control mixture (C) with 100% CPC; a mixture with 80% CPC, 20% FA
and 0% UtSCBA (T0); a mixture with 70% CPC, 20% FA and 10% UtSCBA (T1); and a mixture with 60% CPC,
Keywords:
Agricultural waste
20% FA and 20% UtSCBA (T2). The properties of the concretes in fresh and hardened states were studied. In
Ecological concrete the fresh state, slump, volumetric weight, air content and temperature were estimated, while in the hard-
Fly ash ened state microstructure, mineral phases, compressive strength, moduli of elasticity and Poisson ratios
Untreated Sugarcane Bagasse Ash were investigated. The results indicate that UtSCBA can be considered as a pozzolan even though the LOI
content is higher than the maximum allowed in the Standard. UtSCBA particles are heterogeneous (in
shape and size) with a specific surface area similar to that of the CPC. Because it has a larger volume
of total pores, the use of UtSCBA leads to a reduction of workability and volumetric weight; however,
the air content and the temperature in the fresh state are not affected. The results of XRD and SEM/
EDS suggest that at early ages both a physical effect of dilution of the CPC and the high carbon content
in the SCBA negatively affect the compressive strength of the concretes. However, the pozzolanic reaction
of the SCBA is beneficial at later ages. The combination of 10% UtSCBA plus 20% FA did not affect either the
development of the strength of the concrete or its modulus of elasticity. On the other hand, the addition
of 20% UtSCBA decreased the strength of the concrete at early ages, but after 90 days it was similar to the
strength of the control mixture.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction Portland cement production has a negative impact on the environ-

ment. Studies report that its production is responsible for generat-
The demand for Portland cement is increasing with the world- ing approximately 7% of the world’s total CO2 emissions [1].
wide expansion of urbanization and industrialization; however, One strategy to reduce this problem is to use supplementary
cementing materials (SCMs) [2], which is not only an effective
⇑ Corresponding author. measure to protect the environment but also allows for saving
E-mail addresses: pmontesgarcia@gmail.com, montes@ipn.mx resources and energy required in cement production [3,4]. Over
(P. Montes-García). the past 30 years important research has been carried out on the

https://doi.org/10.1016/j.conbuildmat.2017.09.060
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
84 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
use of industrial SCMs as a partial replacement for Portland
cement; for example, fly ash (FA), silica fume (SF), and blast fur-
nace ground slag (BFGS). With the addition of these materials,
the mechanical and durability properties of concrete have been
improved [5,6]. Chief among the SCMs, FA is the most-used SCM
in the production of binary and ternary concretes, not only for its
low cost but also because it is the most characterized and
production-controlled material in the construction industry.
It has been demonstrated that despite its slow rate of reaction,
when FA is added to concrete it generally provides a significant
improvement in the workability of fresh concrete, a higher
mechanical strength at later ages and a superior performance
when exposed to aggressive media [7,8]. Consequently, the use of
FA in concrete increased from 19% in 2010 to 27% in 2013 [9].
Despite the proven benefits of adding FA to concrete, actual
trends indicate a significant reduction in its production due to
the reduction in the use of coal, the regulatory uncertainties about
its use, and the economic slowdown [10]. As a result, the supply of
FA is not guaranteed in the near future and the use of alternative
SCMs, such as agricultural waste combined with FA, to replace a
large percentage of Portland cement has yet been investigated.
In this context, a promising agricultural waste that can be used
as a pozzolanic material is sugarcane bagasse ash (SCBA). SCBA is
obtained as a by-product of the combustion of the bagasse in boil-
ers and is improperly deposited at open dumps, causing pollution
problems [11]. Because SCBA has a high content of SiO2, it can be
used as a supplementary pozzolanic material to partially replace
Portland cement in mortars and concretes. However, it has been
reported that the addition of SCBA in concrete leads to a significant
workability problem during the mixing and placing of the concrete.
The solution to this problem has been addressed in several
ways; first, using a large dosage of a high-range superplasticizer
(SP) in the mixture [12]; second, by subjecting the SCBA to one
or several post-treatments; third, by the combination of SCBA with
another SCM; and fourth, by the combination of some the previous
options.
The implementation of several post-treatments to improve the
properties of the SCBA has been the subject of current research
projects [13]. Despite all this research, most of the post-
treatments evaluated require a significant amount of energy to
operate, causing additional emissions of pollutants to the atmo-
sphere. Among the most common post-treatments applied to the
SCBA are re-calcining, grinding, sieving, floating, electrostatic pre-
cipitation, and their combination [14,15]. To select a suitable
method to post-treat the SCBA and improve its pozzolanicity prior
to its use as a SCM in concrete, it is necessary to carry out an exten-
sive study on the availability of low-energy-consuming post-
treatments [16]. Studies carried out in Brazil, India, Cuba, Colombia
and Thailand suggest that used as a SCM, post-treated SCBA can
improve the properties of concrete [17,18]. Additional research
has found that the efficiency of the method used to post-treat
the ash and its resulting pozzolanic properties are highly depen-
dent on the physical properties of the original ash [19].
Another option to decrease the negative effects on workability
caused by using untreated SCBA as a SCM in concrete is its use in
combination with FA to prepare ternary concretes, although stud-
ies addressing this subject are scarce. Cordeiro et al. [20] investi-
gated the effect of the SCBA in combination with rice husk ash
(RHA) on the properties of fresh and hardened concretes. In that
study, the SCBA and RHA were ground for 120 min using a vibrat-
ing grinder. After grinding, the average particle-sizes of 2.7 mm for
the SCBA and 4.3 mm for the RHA were obtained by the authors.
They concluded that the combination of the 20% SCBA and 20%
RHA in the concrete mixture caused workability problems, while
the compressive strength of the concretes was similar to the
control mixture using only Portland cement. Jiménez et al. [21]
investigated the effect of SCBA in combination with FA on the
workability of ternary pastes and mortars. The SCBA was only
sieved using the 75 mm ASTM sieve for four minutes. Because of
the low-energy post-treatment applied to the ash, the authors
decided to name it Untreated Sugarcane Bagasse Ash (UtSCBA).
In that study, the authors reported that the addition of UtSCBA pro-
duced an increase in the yield stress and viscosity of pastes. In a
similar manner, the inclusion of UtSCBA in mortar mixes increased
both yield stress and viscosity, which caused a lower percentage of
fluidity and a greater consumption of SP than in the simple mor-
tars. The addition of FA in mortars containing UtSCBA has a bene-
ficial effect on workability as FA hinders the negative effects of
UtSCBA, yielding a mortar with flow properties like those required
to the proper mixing and placing. Results from this research show
that the combination of FA and UtSCBA fulfill the necessary
requirements for pastes and mortars to be workable; however,
there is a need for on-going research which addresses the study
of the properties of these concretes in the hardened state.
The main objective of this research then is to investigate the
effects of the addition of a ‘‘practically as received” sugarcane
bagasse ash (UtSCBA) in combination with FA on the properties
in the hardened state of ternary concretes.
2. Materials
Sugarcane bagasse ash, FA and blended Portland cement CPC 30R (CPC), accord-
ing to the Mexican Standard [22], were used in the preparation of the concrete mix-
tures. The sugarcane bagasse ash was collected from an open dump at the sugar mill
‘‘Constancia,” which belongs to Grupo Beta San Miguel, located in Tezonapa, Ver-
acruz, México. The ash was collected and sieved through a No. 200 ASTM (75 mm)
sieve for four minutes. Because of the low-energy method used to post-treat the
ash, it was decided to refer to it as ‘‘untreated” (UtSCBA). The fly ash used was Type
F (FA), which is available in the American market under the brand AdmixTechÒ.
As well, both calcareous crushed coarse aggregate and river sand were used in
the preparation of the concrete mixtures. The coarse aggregate, with a maximum
size of 19 mm, was obtained from a bank of material located in Santa Maria el Tule,
Oaxaca, Mexico. Volumetric weight, specific gravity, and adsorption of the coarse
and fine aggregates were respectively 1624 kg/m3, 2.66 and 0.47%, and 1596 kg/
m3, 2.78 and 1.74%. The fineness modulus of the sand was 2.97.
Bi-distilled water and a polycarboxylate-based superplasticizer with a gravity
density of 1.07, pH of 6 and a solid content of 30% (PLASTOL 4000)Ò, which fulfills
the ASTM-494 requirements, were used.
2.1. Chemical and mineralogical analysis of the cementitious materials
A chemical analysis of the cementing materials was carried out using X-ray flu-
orescence spectroscopy (XRF) with an Epsilon 3 XL energy dispersive X-ray spec-
trometer. In addition, the loss on ignition (LOI) of the cement was estimated at
950 °C in accordance with the ASTM C114-10, whereas the LOIs of the UtSCBA
and FA were at 750 °C in accordance with the ASTM D7348-13. The identification
of the mineral phases was carried out by X-ray diffraction (XRD) using a Bruker
D8 AdvanceÒ diffractometer. The equipment, which uses a Cu anode, Ni filter and
high-speed detector, was operated at a voltage of 40 kV and a current of 40 mA.
The XRD patterns were obtained at a scanning speed of 0.5 s, with an increment
of 0.05° in a range between 10 and 70°. For the analysis and interpretation of the
results, the software EVA 11.0.0.3Ò and the ICSD, PDF-maint data base were used.
2.2. Physical properties of the cementitious materials
The density of the UtSCBA and FA was determined in accordance with the ASTM
C 188-09. The morphology and texture of the particles of the materials were studied
using a high vacuum JEOLÒ Scanning Electron Microscope (SEM) Model JSM-6490LV
in the secondary electron mode which has attached an EDS microanalysis system.
The operating voltage of acceleration was 20 kV. The EDS system consists of a
WAFER detector built with Lithium-doped Silicon with a 3.5–6 mm diameter and
3 mm thickness, which is controlled by OXFORD’s INCA-sight InstrumentsÒ soft-
ware. The particle-size distribution of the materials was estimated using a MICRO-
TRAC S3500Ò. The equipment was operated in the wet mode using isopropyl
alcohol as a dispersant and applying ultrasonic energy by 40 Watts during 60 s.
The specific surface area was determined by fisisorcion of nitrogen, a technique also
known as the BET method. Equipment from Quantachrome InstrumentsÒ (Nova
2000e) was used to obtain adsorption-desorption isotherms.
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
3. Methods
3.1. Design of the concrete mixtures
Four concrete mixtures were designed in accordance with the
absolute volume method issued by the American Concrete Institute
(ACI 211.1). All concrete mixtures had a 0.5 water/cementitious
materials ratio. The control mixture (C) was designed to reach
25 MPa compressive strength at 28 days and to reach a slump
value of 75 ± 20 mm. The T0 mixture included 0% UtSCBA, 20% FA
and 80% CPC; the T1 mixture had 10% UtSCBa, 20% FA and 70%
CPC; the mixture T2 had 20% UtSCBA, 20% FA and 60% CPC. In T0,
T1 and T2 the percentage of FA was kept constant because previous
studies had reported that 20% FA as replacement for cement is an
optimum value [23]. In Table 1 a summary of the mixture propor-
tioning for 1 m3 is presented.
3.2. Preparation and characterization of the concrete mixtures
The concrete mixtures were prepared under laboratory condi-
tions using a mixer with a capacity of 255 L. The fresh concrete
was characterized by means of a series of tests including slump
(ASTM C143/C143M-10), temperature (ASTM C1064/C1064M-08),
volumetric weight (ASTM C138/C138M-09) and air content (ASTM
C231/C231M-09b). Then 42 cylinders (100/  200 mm) for each
mixture were cast, giving a total of 168 specimens. The cylinders
were demolded after 24 h and cured by immersion in a Ca(OH)2
saturated solution at 23.0 ± 2.0 °C until the time of the test (ASTM
C31/C31M-09). Three cylinders were used for the microstructural
examination and mineral phase identification, six for the compres-
sive strength determination, and three for the modulus of elasticity
and Poisson ratios estimation.
3.3. Determination of mineral phases and microstructural analysis of
the hydrated pastes of the concrete mixtures
Analyses of the mineral phases of the concrete mixtures at 7, 28,
90 and 120 days were carried out with the purpose of identifying
the major crystalline phases. Disks 8.0 ± 2.0 mm thick were sawn
from some of the 100/  200 mm cylinders prepared for this pur-
pose in the previous section. The disks were kept at room temper-
ature and immersed in acetone to stop the hydration of the
cementitious paste in accordance with the recommendations of
the solvent-exchange method using ACS acetone [24]. At the
required ages of testing, the concrete disks were crushed to remove
large aggregate particles; in this manner, cementing paste was
mostly obtained. Subsequently the paste was manually ground
until converted into a powder which passed through the ASTM
75 mm sieve. The resulting powder was used for the determination
of the mineral phases of the different concretes at the evaluated
ages using the same equipment and operating conditions as those
used to characterize the mineral phases of the cementitious
materials.
The analysis to identify the morphology of the Hydrated
Cement Paste (HCP) at 7, 28, 90 and 120 days was also performed
from disks 8.0 ± 2.0 mm thick obtained from the same concrete
cylinders prepared for this purpose in the previous section. The
Table 1
Mixture proportioning for 1 m3 of concrete, kg.
Mixture CPC FA UtSCBA
C 410 – –
T0 328 82 – 727
T1 287 82 41
T2 246 82 82
85
concrete disks were also kept in acetone until the test date and
stored at room temperature. In this case, the disks were crushed
in order to obtain small fragments (approximately 10 mm3) to be
analyzed using SEM/EDS. The fragments were dried in an oven at
40 °C for 24 hours to eliminate the acetone. Then a thin layer of
Palladium Gold (Au-Pd) was placed for three minutes on the place
of the fracture using a Denton Vaccum Desk IVÒ with a working
pressure in the range of 30–100 mtorr. Finally, the samples were
placed on the sample supporter and the test was performed. The
equipment and operating conditions were the same as those used
to characterize the morphology of the cementitious materials.
3.4. Mechanical properties of the concrete mixtures
The compressive strengths of the concrete mixtures at 7, 28, 56,
90 and 120 days were obtained. Six replicates were considered for
each mixture and age of testing. The specimens were tested in a
wet condition, prepared according to the ASTM C1231/C1231M-
10 standard and tested using neoprene disks with a hardness Shore
60 and 100 mm in diameter. The compressive strength was esti-
mated in accordance with the ASTM C39/C39M-09ª using an
ELVECÒ model E659-5 compression machine. The moduli of elas-
ticity of the concretes were determined in accordance with the
ASTM C469-02e1 at 28, 56 y 90 days of age. For this test, three
replicates were considered and a compressometer-extensometer
by ELVECÒ was used.
4. Analysis and discussion of results
4.1. Analysis of the chemical composition of the cementitious materials
In Table 2 the results of the chemical composition of the SCMs
and cement are presented. The sum of the major oxides (SiO2 + Al2-
O3 + Fe2O3) for the UtSCBA was 88.28%, with 2.57% CaO and 9% LOI.
Only the latter parameter does not fulfill the requirements to be
considered as a material with pozzolanic potential (ASTM 618-
05). The high LOI value can be the result of incomplete burning
of the bagasse, a low calcining temperature, or a long calcining per-
iod [25]. Nevertheless, it is in the interest of this research to use the
material ‘‘practically as collected,” and thus avoid the use of a high-
energy demanding post-treatment (as, for example, a thermal
treatment at 550 °C) to decrease the LOI as used by others [26].
The sum of the major oxides for the FA was 89.55% with a CaO
content of 4% and 2.6% of LOI; therefore, the FA used can be classi-
fied as a Type F pozzolan (ASTM 618-05).
Regarding the chemical composition of the CPC, the sum of CaO
+ SiO2 + Al2O3 + Fe2O3 was 89.14% (which is within 50–90%) estab-
lished in the NMX-C-414-ONNCCE-2004; however, the LOI, 8.4%, is
higher than the allowed value. The high LOI value is the result of
the presence of calcium carbonate, mostly resulting from the car-
bonation of calcareous additions to the cement. Because the decar-
bonation of CaCO3 occurs at 700–900 °C [27], the high LOI value
can be associated with the presence of this compound. CPC 30R
cement was used in this research for several reasons. This cement
has a lesser amount of pozzolans than the other cements available
in this region of Mexico. Also, this cement is locally available in
Fine aggregate Coarse aggregate Water SP
727 1015 205 2.7
1015 205 1.6
727 1015 205 3.1
727 1015 205 4.9
86 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95

Table 2
Chemical analysis of the used materials, % s.

Element/Compound UtSCBA FA CPC

Aluminium Oxide (Al2O3) 15.00 20.01 4.87
Calcium Oxide (CaO) 2.57 4.00 60.03
Iron Oxide (Fe2O3) 7.16 5.42 3.57
Potassium Oxide (K2O) 3.52 0.96 0.85
Magnesium Oxide (MgO) 1.19 0.63 1.50
Magnesium Oxide (MnO) 0.22 0.10 0.08
Sodium Oxide (Na2O) 0.54 0.19 0.52
Phosphorous Oxide (P2O5) 1.14 0.38 0.19
Silicon Dioxide (SiO2) 66.12 64.12 20.67
Titanium Oxide (TiO2) 1.13 1.12 0.58
Sulphur Oxide (SO3) 0.26 0.86 4.95
LOI at 950 °C for the CPC and 750 °C 9.0 2.6 8.4
for the FA and UtSCBA
Equivalent Na2O 2.86 0.82 1.08
*
SiO2 + Al2O3 + Fe2O3 88.28 89.55 –
*
The sum of the three major oxides must be higher than 70% in order to consider
that a material has pozzolanic potential (ASTM 618-05).

southeastern Mexico, whereas ordinary Portland cement is not

available. This is somehow convenient because the findings from Fig. 1. XRD pattern of UtSCBA.
this research can readily be adopted in practice. Furthermore, this
cement has been previously characterized and used in other phases
of a long-term investigation. The first phase of that investigation
deals with the study of the rheological properties of binary and
ternary pastes and mortars prepared with the same materials used
in the present research [21]. The second is the subject of the pre-
sent paper regarding the analysis of the microstructural and
mechanical properties of ternary concretes prepared with the same
ingredients. Finally, the last part of this long-term project is the
evaluation of the durability of such concretes, part of ongoing
research which will be reported later on.
It is worth noticing that despite the high LOI value of the
cement used for the concrete preparation, results indicate that
the additions originally incorporated into the cement do not mask
the findings about the influence of the addition of FA or the com-
bination of UtSCBA plus FA on the concrete’s final properties. This
fact can help the authors draw sound and univocal conclusions.

4.2. Mineralogical analysis of the cementitious materials

The XRD pattern obtained for the UtSCBA is characteristic of a

semi-crystalline material (Fig. 1). A wide band of dispersion (halo)
is observed between a 12 and 38° 2h angle, which implies the pres-
ence of amorphous compounds in the ash. The presence of quartz-
a and cristobalite-b as major crystalline phases is readily evident.
Other amorphous compounds detected were graphite, maghemite,
aluminium oxide and calcium, which indicate the possibility of a
pozzolanic reaction.
The XRD pattern for the FA (Fig. 2) shows quartz and mullite as
the two main crystalline phases, while weak peaks of hematite
were identified. Similar to the UtSCBA, FA shows an amorphous
halo between 15 and 30 °C 2h angle, which is characteristic of vit-
reous silicoaluminates.
The XRD pattern for the CPC (Fig. 3) shows the C3S, C2S, C3A and
C4AF main phases present in Portland cement [27,28]. The pres-
ence of minor quantities of gypsum and calcium carbonate is
observed. Calcium carbonate is characteristic of Portland cements
with calcareous filler [29].
4.3. Analysis of the physical properties of the cementitious materials
UtSCBA contains heterogeneous particles with different shapes
and sizes. The following three particle shapes are observed: solid
prismatic [Fig. 4(a)]; porous irregular [Fig. 4(b)]; and long porous
Fig. 2. XRD pattern of FA.
cylindrical [Fig. 4(c)]. FA generally contains vitreous solid spherical
particles and an agglomeration of fine particles is observed [Fig. 4
(d)]. Cenospheres and plenospheres were also identified [Fig. 4(e)].
Similar to the UtSCBA, in the CPC irregular angular solid particles
with different sizes are observed [Fig. 4(f)]. In this case, the differ-
ent shapes and sizes are the result of the pulverization of the clin-
ker during the grinding process [30].
Fig. 5 shows the particle-size distribution of the materials. The
average sizes for the UtSCBA, FA and CPC were 48.4, 34.0 and
17.1 mm, respectively. It is worth noticing that the Laser Diffraction
technique is based on the assumption that the particles in the
material are hard and spherical in shape; however, as shown in
the previous section, the particles in the materials under study
have a variety of shapes and textures, especially those from the
UtSCBA. The density distribution curve shows a monodisperse dis-
tribution for the UtSCBA, which is characteristic of sieved materials
[31]; a polidisperse distribution ranging between 5.5 and 37 mm
was observed for the FA, which is the result of the recollection pro-
cess using an electrostatic precipitator. The CPC shows a bimodal
distribution at 5.5 and 22 mm, which can be attributed to the
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
Fig. 3. XRD pattern of CPC.
presence of different mineralogical components, the grinding pro-
cess, and the fact that small particles tend to cluster.
The specific surface areas of the materials are presented in
Table 3. The UtSCBA has the largest total pore volume of the three
materials, indicating that this material has both internal and exter-
nal porous structures. Nevertheless, FA presents a lower pore vol-
ume than UtSCBA, which indicates the predominance of vitreous
solid particles. The CPC has a particle system with a lower porosity
than UtSCBA and its surface area is related mainly to the fineness
of the material, as demonstrated in the previous results on the dis-
tribution and average sizes of the particles of the materials.
It is well known that the size and shape of particles have a sig-
nificant effect on the workability of Portland cement-based mate-
rials [32]. Consequently, it is necessary to carry out tests on the
fresh state of concrete prepared with the combination of these
three materials.
(a)
(d)
Fig. 4. Morphology of the used materials.
87
4.4. Properties in the fresh state of the ternary concretes
Results indicate that the addition of 10% UtSCBA to the concrete
mixture containing 20% FA caused a slump reduction of approxi-
mately 30%, and the addition of 20% UtSCBA a reduction of approx-
imately 40% (Table 4). However, the use of the superplasticizer
admixture (SP) contributed to all the mixtures having a
75 ± 20 mm slump value. This also allowed the water-to-
cementitious materials ratio to be kept constant at 0.50.
In the mixture T0, the slump was reached largely because of the
spherical shape of the FA particles, which causes a ball-bearing
effect [33]. In this manner, its workability improved and as a result
less SP than the control was required. On the other hand, in the
mixtures containing UtSCBA an increase of SP was needed because
significant slump reduction occurred; the reduction was in the first
place caused by the great variety of shapes and the large size and
rough texture of the UtSCBA particles [21]. The high LOI content,
which indicates a high level of unburned carbon particles, can also
be blamed for this detrimental effect, as high levels of unburned
carbon particles increase the requirement for water [34].
The results of the analysis for the air content and volumetric
weight are shown in Fig. 6. The air contents of the four mixtures
range from 1 to 3%, which are valid for non-air-entrained concrete
mixtures [30]. Volumetric weights of mixtures T1 and T2 were lower
than those of mixtures C and T0. This is directly related to the density
of the materials as the density of the CPC is higher than the density of
the FA, and both densities are higher than the density of UtSCBA. Fur-
thermore, the reductions of the air contents for the mixtures with
UtSCBA would lead to the increase of the volumetric weights.
4.5. Analysis of the microstructure of the hydrated cementitious pastes
in ternary concretes
4.5.1. Qualitative analysis using XRD
The major crystalline phases identified in the mixtures at 7, 28,
90 and 120 days are shown in Figs. 7–10.
Fig. 7 shows the XRD patterns of mixture C for the four studied
ages. The main hydration products such as tobermorite (C-S-H),
(b) (c)
(e) (f)
88 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95

Fig. 5. Particle size distribution of used materials.

Table 3
Specific surface areas of the used materials. Fig. 7. Identification of the hydration products in the C mixture (control).

Material Specific Surface Area, m2/g Total volume of pores, cc/g

2
UtSCBA 36.0 4.464  10
2
FA 6.9 1.212  10
2
CPC 3.9 1.273  10

Table 4
Workability reduction of the ternary concrete mixtures containing UtSCBA.

Mixture Initial Slump Final Slump, Temperature,

Slump, reduction, % mm °C
mm
C 75 – 78 25
T0 80 +7 79 25
T1 58 23 88 24
T2 50 33 90 24

Fig. 8. Identification of the hydration products in the T0 mixture.

and definitively the mechanical resistance of the conglomerate

Fig. 6. Air contents and volumetric weights of the fresh concrete mixtures.
portlandite (CH) and ettringite (AFt) are identified. From 7 to
28 days there is an important decrease in intensity of the peaks
of these products; this mostly indicates the hydration of C2S, which
contributes to the increase of the compressive strength beyond
7 days. At 90 and 120 days the intensity of the peaks of portlandite
and ettringite are similar to that of 28 days. However, the intensity
of the tobermorite peak increases with age. This product is respon-
sible for the internal structure of the cement paste, the bonding
between this paste and the aggregates in mortars and concretes,
[35]; therefore, it is an indispensable and always positive con-
stituent [36]. This can be corroborated with the compressive
strength results.
The XRD patterns for mixture T0 are shown in Fig. 8. Similar to
the C mixture, C-S-H, CH and Aft products were identified; how-
ever, the dynamics of the intensity of the peaks is different. From
7 to 28 days, a light increase in intensity of the C-S-H peaks is
observed, while the intensities of the other products remain basi-
cally the same.
After 28 days a progressive increase in the intensity of the C-S-H
peaks and a progressive decrease in CH are observed. This indicates
the beginning of the occurrence of the pozzolanic reaction caused
by the crystallization of the C-S-H and the consumption of CH. This
corroborates that the CH produced from the hydration of cement
reacted with the FA in order to form additional C-S-H with a lower
calcium-to-silicon ratio [37].
The comparison between the results in XRD patterns for T0 and
C shows important differences (see peak located at 2h = 20.9). At
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
Fig. 9. Identification of the hydration products in the T1 mixture.
Fig. 10. Identification of the hydration products in the T2 mixture.
7 days the CH peaks are less intense for the T0 mixture as a result
of the replacement of 20% CPC by FA, which decreases the quantity
of CH produced during the CPC hydration. The reactivity of FA is
slowly developed as a result of the vitreous particles. It is known
that at early ages, before 28 days, the CH crystals form on the sur-
face of the FA particles as a result of the nucleation spots, which
leads to the dispersion of the CH, according to the FA particle dis-
tribution. In this manner, the likelihood that the CH forms on the
aggregates surface is low; therefore, the concrete matrix is modi-
fied and its structure is improved [38]. At 28 days, the intensity
of the peaks are similar, but at later ages the peaks of the T0 mix-
ture are more intense than the peaks of the C mixture.
The XRD patterns for the mixture T1 are shown in Fig. 9. From 7
to 28 days, a slight increase in the intensity of the C-S-H peak is
observed, while CH and Aft are quite similar; however, at 90 days
there is a noticeable increment in the intensity of C-S-H while
the CH cannot be identified. This can be attributed to the fact that
the cement replacement in this mixture was higher than for the
mixture T0 and that the quantity of CH produced during the
cement hydration allows the pozzolanic reaction of both ashes to
89
occur (FA and UtSCBA). Comparing the XRD results of T1 and T0,
the following can be observed: at 7 days the intensity of the C-S-
H (located at 2h = 20.9) are similar, at 28 and 90 days T1 is more
intense than T0, and at 120 days it is slightly less intense than
T0. This suggests that the compressive strength of the T1 mixture
could be higher than for the T0 mixture at that age.
The XRD patterns for the mixture T2 are shown in Fig. 10. At
7 days there is enough availability of CH for the posterior develop-
ment of the pozzolanic reaction. For this mixture it was not possible
to identify CH, even at 28 days of age. This suggests that the UtSCBA
reacts faster than the FA. The same behaviour was observed at 90
and 120 days; however, in these cases the C-S-H peak is more crys-
talline. Because of the vast availability of CH, both the FA and the
UtSCBA compete for its consumption, and this competition actually
balances when the percentage of both ashes is similar.
Comparing the results of the T2 mixture with the T0 mixture
shows that at 7 days, the intensity of the C-S-H peaks for the T2
is higher than for T0; however, at 28, 90 and 120 days the intensity
of the T0 peak is higher; once again, this suggests a higher com-
pressive strength of T0 for these ages.
4.5.2. Analysis of the SEM/EDS results
The results of the SEM test carried out for the C concrete mix-
ture at different ages are shown in Fig. 11. At 7 days [Fig. 11(a)],
a hydrate cement paste (HCP) with large capillary pores (having
an average diameter of 20 mm) is observed. These pores represent
zones previously occupied by water between unhydrated cement
grains that are now pores between the hydration products [39].
Fig. 11(b) shows the growth of Ettringite needles between the
pores, which indicates a gain in strength at an early age. Further-
more, large quantities of CH crystals can be observed. In Fig. 11
(c), the Interfacial Transition Zone (ITZ) is observed, where porous
CH laminar crystals were deposited, building up an apparently
weak bonding between the cement paste and the aggregate. At
28 days [Fig. 11(d)], important progress on the hydration process
is observed. The C-S-H filled the empty pores, decreasing the diam-
eter to approximately 5 mm. Furthermore, at this age the formation
of isolated hexagonal CH crystals prevails, as well as the continua-
tion of the formation of Ettringite needles, indicating the continu-
ous increment of the structure’s strength [Fig. 11(e)]. At 90 and
120 days no significant changes in the microstructure of the HCP
were observed.
Fig. 12 shows results of the SEM tests carried out for the T0 con-
crete mixture. At 7 days [Fig. 12(a)], unhydrated FA particles are
observed. Some particles are covered by a C-S-H gel, which indi-
cates that the degree of hydration is still low. This accords with that
observed at the corresponding diffractograms; however, the sizes of
the pores represent approximately one fourth of that observed in
Fig. 11(a) (Mixture C at 7 days). The reason for this is the existence
of fine particles of FA which are similar or smaller (17 mm) than the
average CPC particles, causing at an early age a purely physical
effect of packing and acting as nucleation points for the hydration
of the Portland cement particles [40]. At 28 days the reduction of
the pore size at the ITZ is evident when compared to the cementing
paste in general, even though at this age the presence of unreacted
FA in this area could weaken the zone [41]. The diameter of the
pores decreased by approximately 50% compared with the previous
age. It is also worth noticing that the diffractograms at this age for
this mixture and the C mixture showed no observable differences.
At 90 days [Fig. 12(c)], a densified cementing paste is observed
showing that the majority of the particles have reacted. This occurs
because most of the CH is consumed by the pozzolanic reaction of
the FA, and even the remaining CH can be covered by the C-S-H
gel [42]. At 120 days [Fig. 12(d)], the degradation of the FA particles
can be observed, as well as how the reaction products become part
of the microstructure.
90 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95

(a) 7days (b) 7 days (c) 7 days

(d) 28 days (e) 28 days

a) General morphology, b) Ettringite growth, c) porous ITZ and laminar CH crystals, d) Reduction of
porosity and CH crystals, e) continuous formation of Ettringite
Fig. 11. SEM micrographs for the C mixture at different ages.

(a) 7 days (b) 28 days

(c) 90 days (d) 120 days

a) Unreacted FA particles at 7 days, b) ITZ at 28 days, c) densification of HCP at 90 days, d) degradation of
FA particle and products of the pozzolanic reaction at 120 days.
Fig. 12. SEM micrographs for the T0 concrete mixture at different ages.

The results of the SEM tests carried out for the T1 concrete mix-
ture are shown in Fig. 13. At 7 days unhydrated particles of CPC
and FA are observed [Fig. 13(a)], while UtSCBA particles are at first
sight practically not observed, a result of the low proportion of
UtSCBA compared with CPC and FA. A more detailed analysis
indicates that UtSCBA particles can be identified because of their
characteristic shape and high carbon content.
It is probable that the cellular porous UtSCBA particles react
with the CH of the cement hydration products promoting the
beginning of a pozzolanic reaction at 7 days. The UtSCBA also acts
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95 91

as a filler, improving the packing of the particles and might serve as
nucleation sites for the FA particles. This synergistic effect might
prevent a drop in the compressive strength of this concrete matrix.
Fig. 13(b) shows a magnification of a detail in square of Fig. 13(a). A
capillary pore of about 5 mm radius is surrounded by C-S-H gel,
which is the most important and complex structure in the con-
crete. The addition of supplementary materials makes this struc-
ture even more complex by the formation of C-S-H with different
Ca/Si ratios [43]. According to Kar et al. [44], the Ca/Si ratio of
the primary C-S-H (P), a product of the hydration of cement, is
between 1.57 and 2.1; whereas, it is 1.5–1.6 for the secondary C-
S-H(S), the product of the pozzolanic reaction of FA. Spectra 1
and 2 [Fig. 13(c) and (d)] show an example of C-S-H(P) and C-S-
H(S) as the Ca/Si ratios are respectively 1.9 and 1.2. The Si peak
in spectrum 2 has the highest intensity when compared to the peak
in spectrum 1; therefore, the results from spectrum 2 probably
belong to the products generated by the FA and UtSCBA which
reacted at early ages. The results for 28 days are shown in Fig. 13
(e). Some FA and UtSCBA particles and some unhydrated CPC par-
ticles are observed. This figure also seems to prove the increase in
likelihood of the occurrence of the pozzolanic reaction at this age.
The EDS shows a Ca/Si ratio of 1.3 [Fig. 13(f)] and several zones
with morphology and texture similar to the region analyzed by
the EDS. The results for 90 days are shown in Fig. 13(g). A relatively
homogeneous and a dense microstructure are observed. At
120 days [Fig. 13(h)], there are no apparent changes in the
microstructure since 90 days. Nevertheless, the EDS results can
identify carbon particles [Fig. 13(i)], which may inhibit the contin-
uous improvement of the concrete matrix.
The results of the SEM tests carried out for the T2 concrete mix-
ture are shown in Fig. 14. At 7 days unhydrated CPC and ash parti-
cles are observed [Fig. 14(a)]. At 28 days [Fig. 14(b)], a
microstructure with more complex hydration products is observed.
The microstructure shows the formation of floccules, which are the
results of the hydration products covered and connected by fibrous
hydrates, indicating the start of the hydration of the cementitious
matrix. At 90 days [Fig. 14(c)], a more compact and homogeneous
cementitious paste then for T1 mixture is observed. The ITZ [Fig. 14
(d)] is less porous and has a larger amount of CH. CH tends to form
on the surface of the particles of the aggregate; therefore, the

(a) 7 days (b) 7 days (c) Spectrum 1 (d) Spectrum 2

(e) 28 days (f) Spectrum 3

(g) 90 days (h)120 days (i) Spectrum 4

(a) Anhydrated particles of CPC, FA and UtSCBA at 7 days, (b) Capillary pore surrounded by primary C-S-H,
(i) Carbon particles between de C-S-H products
Fig. 13. SEM micrographs for the T1 concrete mixture at different ages.
92 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95

transformation to the secondary C-S-H densifies the ITZ. This con-
tributes to the efficient load transfer between the mortar and the
coarse aggregate, which in turn contributes to the increase of the
compressive strength of the concrete [45]. At 120 days [Fig. 14
(e)], the hydration degree of the cementitious matrix continues
increasing and the formation of the hydration products with cer-
tain carbon content increases as well. At this point, an increment
in the compressive strength is expected, because the large FA par-
ticles and the porous UtSCBA particles slowly consume all the CH
produced by the hydration process.
4.6. Mechanical properties of the ternary concretes
4.6.1. Compressive strength
The results of the compressive strength tests are shown in
Fig. 15. In all the tested concrete mixtures the compressive
strengths increased with age. The compressive strengths for the
C mixture at different ages are similar to those reported in the lit-
erature for a conventional concrete with a 0.5 water-to-cement
ratio [46]. At 7 days, its strength was the highest. This was
expected because the mixture had only CPC particles, which
hydrated and generated a large quantity of C-S-H, allowing an early
densification of the matrix, as observed in the mineral phases’
identification and morphology analysis sections. In terms of
strength development, the concrete prepared with the mixture
T0 was consistently stronger than both the control and the ternary
concretes. At 7 days, its strength was lower than the control and at
28 days was similar to it; however, at later ages it showed higher
strength values. Results are consistent with those reported by
Huang et al. and Guzmán [47,48]. The compressive strength of
mixture T1 was lower than the control mixture at early ages. At
7 days, its compressive strength was approximately 80% of C,
which was similar to that obtained for T0. At 28 and 56 days, its
strength was lower than the control but at 90 days levelled up.
At 120 days, the strength for the concrete mixture was higher than
the control, but lower than the strength of T0. The compressive
strength of the T2 was the lowest of the concrete mixtures at 7,
28 and 56 days; however, it progressively increased at all ages,
and at 120 days was similar to the control.
The reduction in strength of the mixtures containing UtSCBA is
the result of the combination of a few factors. One, there is a lower
amount of SiO2 in the UtSCBA available for reaction than in the FA.
Consequently, the formation of a significant lower amount of C-S-H
for these concretes was identified by XRD. Nevertheless, for later

(a) 7 days (b) 28 days

(c) 90 days (d) 90 days

(e) 120 days (f) 120 days

(a) Anhydrated particles of CPC, FA and UtSCBA at 7 days, (b) significant microstructural changes at 28 days
(c) homogeneous and compact concrete matrix, (d) improvement of the ITZ
Fig. 14. SEM micrographs for the T2 concrete mixture at different ages.
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95 93

Relative Compressive Strength, (%)

Mixture 7 days 28 days 56 days 90 days 120 days
C 1.00 1.00 1.00 1.00 1.00
T0 0.81 1.01 1.06 1.12 1.12
T1 0.81 0.91 0.92 0.98 1.04
T2 0.69 0.74 0.83 0.93 1.00

Fig. 15. Results of compressive strength for the concretes under study.

Relative Modulus of Elasticity, (%)

Mixture 28 days 56 days 90 days
C 1.00 1.00 1.00
T0 0.97 1.02 1.02
T1 0.90 0.96 0.95
T2 0.79 0.92 0.92

Fig. 16. Summary of the moduli of elasticity for the concretes under study.

ages the performance of the T1 and T2 concrete mixtures improved
as the result of the pozzolanic reaction of the UtSCBA. A second fac-
tor is that the UtSCBA contains larger particles than FA, which act
as a filler because unreacted FA particles were observed in that
mixture. Furthermore, UtSCBA has significantly more carbon con-
tent than FA, and carbon particles inhibit or slow-down the chem-
ical reactions between the pozzolans and the hydration products
[49]. Another study has reported that the use of SCBA in concrete
mixtures improves their compressive strengths at ages later than
28 days; however, this improvement can be attributed to the fact
in that study that the ultrafine SCBA was obtained from grinding,
which is a highly demanding energy process [50].
The UtSCBA used in this research was only sieved through the
No. 200 ASTM (75 mm) sieve for four minutes, and based on the
above, it can be said that the addition of 10% and 20% of this ash
in concretes containing FA affects their compressive strength only
at early ages.
Recent studies on the addition of UtSCBA in mortars suggest
that there is no detrimental effect on strength when 10% and 20%
are incorporated into the mixture, as only a slight increase in
strength was registered when 20% UtSCBA was added [51]. In that
study, at 450 and 600 days, the compressive strength of the mortar
containing 20% UtSCBA was significantly higher than that of the
control.
94 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
Relative Poisson’s ratio, (%)
Mixture 28 days
C 1.00
T0 0.88
T1 0.97
T2 0.86
Fig. 17. Summary of the Poisson’s Ratios for the concretes under study.
In this research, the compressive strengths of concretes con-
taining UtSCBA do not significantly differ from the strength of
the control mixture, especially at later ages. The compressive
strength of mixture T2 improved after 90 days, probably as a result
of a purely chemical effect (pozzolanic reaction) between the
amorphous silica in the ashes and the CH produced during the
hydration of the CPC to form secondary C-S-H, as corroborated
by the XRD analysis.
4.6.2. Moduli of elasticity and Poisson’s ratios
Results for the static moduli of elasticity of the different con-
crete mixtures at 28, 56 and 90 days are shown in Fig. 16. It can
be observed that the values obtained are within the values
reported in the literature for concrete; it can also be observed that
an increase in value is observed as time passes and a clear reduc-
tion when UtSCBA is incorporated into the mixtures T1 and T0
[52]. Mixture T0 again had the best performance in terms of elastic
behaviour after 90 days. The moduli of elasticity for mixtures T1
and T2 were lower than that of mixture C; nevertheless, an
increase of the modulus of elasticity for mixture T2 is expected
at latter ages as the compressive strength of that concrete was
slightly higher than for mixture C at 120 days.
Further analysis of the results indicates that the modulus of
elasticity of concrete is directly related to its compressive strength.
Therefore, a reduction in the modulus of elasticity caused by the
addition of FA or a larger reduction by the addition of the combina-
tion of FA plus UtSCBA corresponds to reductions in the respective
compressive strengths of the concretes. Nevertheless, this ten-
dency is clearly reversed after 28 days for concrete containing fly
ash and is not significant after 90 days for the ternary concretes.
The moduli of elasticity of the concrete mixtures correlate well
with the compressive strength values of the same concretes with
determination coefficients of 0.914, 0.988, 0.929 and 0.922 for
the C, T0, T1 and T2 mixtures, respectively.
The average Poisson’s ratios for all the mixtures are shown in
Fig. 17. Estimated values are in the range of 0.15 and 0.23, which
correspond to those reported in the literature [52].
56 days 90 days
1.00 1.00
1.12 1.11
1.10 1.06
1.08 1.08
5. Conclusions
Based on the analysis of results, the following can be concluded:
1. The sugarcane bagasse ash used in this research (UtSCBA) is a
SCM which does not require a high-energy-demanding post-
treatment in order to be used in combination with for the
preparation of ternary concretes.
2. The shape and size of the average UtSCBA particles negatively
affected the workability of the mixture containing FA. The loss
of workability was caused by the high carbon content, the
shape, and the larger size of the UtSCBA particles compared
with those from FA; nevertheless, the detrimental effect did
not prevent the concrete mixtures T1 and T2 to achieve the tar-
get slump value when a superplasticizer was added.
3. The addition of 10% UtSCBA to the mixture affected the com-
pressive strength at early ages with respect to the control con-
crete prepared using only cement; however, this effect occurs
only at early ages because after 90 days the strength is compa-
rable to the control.
4. The addition of 10% UtSCBA did not significantly affect the
development of the compressive strength of the concrete; how-
ever, the addition of 20% UtSCBA decreased the compressive
strength at early ages, but an increase in strength occurred after
90 days.
5. The improvement of the mixture T0 was caused by a physical
effect such as packing and the formation of nucleation zones
for the hydration of the CPC. The results also show that the
reduction in compressive strength at early ages in the ternary
mixtures can be attributed to the physical effect of the dilution
of the CPC and to the high carbon content in the UtSCBA. The
improvement at later ages is caused by the occurrence of the
pozzolanic reaction.
6. The results indicate that the UtSCBA can be considered to be a
pozzolan; however, the LOI is higher than the maximum allowed
in the Standard. UtSCBA particles are heterogeneous (in shape
and size) and its specific surface area similar to that of the
 V. Ríos-Parada et al. / Construction and Building Materials 157 (2017) 83–95
CPC, but with a larger volume of total pores. The use of UtSCBA
leads to a reduction of workability and volumetric weight. The
air content and temperature are not affected. The results of
XRD and SEM/EDS suggest that at early ages, the physical effect
of the dilution of CPC and the high carbon content in the SCBA
negatively affects the compressive strength of the concretes,
while the pozzolanic reaction of the SCBA is beneficial at later
ages. Regarding the compressive strength results, the combina-
tion of 10% UtSCBA plus 20% FA did not affect either the develop-
ment of strength or the modulus of elasticity of the concrete. The
addition of 20% UtSCBA decreased the strength at early ages, but
was similar to the control after 90 days.
Acknowledgements
The authors thank the Instituto Politécnico Nacional of Mexico
(IPN) for the financial support for this research, and to the Investi-
gación de Materiales de Construcción, y Ecomateriales y Energía
laboratories of the Universidad Autónoma de Nuevo León of
México, as most of the testing was carried out in these laboratories.
The authors are also grateful with the Consejo Nacional de Ciencia
y Tecnología of Mexico (CONACyT) for the Master Scholarship
given to V. Ríos-Parada.
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