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High Volume Slag Mortar With Nano Limestone PDF
High Volume Slag Mortar With Nano Limestone PDF
A R T I C L E I N F O A B S T R A C T
Keywords: This paper presents the effects of various nano-CaCO3 (NC) contents on 28 days compressive strength and
High volume blast furnace slag microstructure of high volume slag (HVS) pastes and high volume slag-fly ash (HVSFA) blended pastes. The
Slag-fly ash blend results show that addition of 1–4% NC improved the compressive strengths of HVS pastes containing 70%, 80%
Nano calcium carbonate
and 90% slag, respectively by 8–24%, 1–16% and 2–20% compared to their reference pastes. The compressive
Compressive strength
Microstructure and carbon footprint
strength of HVSFA paste containing combined slag and fly ash content of 70% is also increased significantly by
16–24% than the reference control paste due to the addition of 1–4% NC and maintained higher compressive
strength than OPC paste after 28 days of curing. The addition of NC reduced the large capillary pores and cu
mulative pore volume of HVS pastes and HVSFA paste. Significant reduction of calcium hydroxide (CH) in
HVSFA paste containing combined slag and fly ash content of 70% is found due to the addition of NC by
thermogravimetric analysis (TGA) and a slight increase of CH is noticed in all HVS paste. A denser microstructure
with fewer internal micro-cracks and more hydrated products are revealed in scanning electron microscopic
(SEM) images and EDS trace analysis in all HVS and HVSFA pastes due to the addition of NC. HVS and HVSFA
paste with significantly lower carbon footprint and higher compressive strength than control cement paste can be
achieved with the inclusion of 1% NC.
1. Introduction (SCM), slag and fly ash have been widely used as a partial replacement of
cement to investigate the mechanical and durability properties of con
The demand for concrete as a construction material was always in a crete as well as reducing the CO2 emission into the atmosphere [6,7].
rising trend in the past and will be very high in future due to the rapid However, the partial replacement of cement by SCM is still lying under
urbanisation across the world which requires a significant amount of 50% in many studies [8–16] due to the several challenges like very low
binding materials. Recent study expected that global demand for cement early-age compressive strengths, significant autogenous and drying
will rise by approximately 115–180% by 2020 compared to 1990s and shrinkage, briskly progress of carbonation though high volume (>50%)
may climb to 400% by 2050 [1]. Ordinary Portland Cement (OPC) is replacement of slag and fly ash. Few researches have also been examined
used as the binder for concrete which is extremely energy intensive and the use of ternary and quaternary blend of high volume slags and fly ash
every single tonne of OPC manufacture releases roughly one tonne of with cement, silica fume, and limestone filler but did not notice any
carbon dioxide (CO2) during the calcination process and contributes 7% significant improvement in mechanical and durability of properties of
of global CO2 into the atmosphere per year [2–5]. Global warming concretes due to slow pozzolanic reaction of slag and fly ash at early ages
associated with CO2 emission due to cement manufacturing plays a vital [17–21].
role to find alternative option of cement or huge reduction of cement While in numerous studies the use of fly ash and slag in concrete
content in concrete, which resulted in the use of several industrial shows improvement of mechanical and durability properties and eco
by-products such as ground granulated blast furnace slag (GGBFS), fly nomic benefit, these industrial by-products are also identified as the
ash (FA), silica fume, metakaolin etc. as partial replacement of OPC in potential source of toxic substances which might cause leaching of heavy
the concrete. Among various supplementary cementitious materials and trace metals in to soil and surface/ground water if they are used to
* Corresponding author.
E-mail address: s.ahmed@curtin.edu.au (F.U.A. Shaikh).
https://doi.org/10.1016/j.jobe.2019.100929
Received 22 February 2019; Received in revised form 22 July 2019; Accepted 19 August 2019
Available online 26 August 2019
2352-7102/© 2019 Elsevier Ltd. All rights reserved.
A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
stabilise soil [22]. However, no such leaching of heavy metals is re 1.2. Materials
ported in concrete [23].
Recently, many researchers studied the use of small amount of nano Ordinary Portland cement (OPC) was used in all pastes this study.
materials such as nano calcium carbonate, nano silica, nano titanium, The ground granulated blast furnace slag (BFS) was supplied by BGC
nano alumina, nano carbon tubes etc. as partial replacement of cement cement, Australia and class F fly ash (FA) was supplied by Eraring power
in concretes to influence the mechanical and durability properties and station of New South Wales in Australia. Dry nano-CaCO3 (NC) powder
found an impressive improvement in mechanical and durability prop used in this study was purchased from Nanostructured and Amorphous
erties due to their enormous specific surface area and extremely tiny Materials, Inc. of the USA with an average particle size of 15–40 nm,
particle sizes [24–43]. Nano-CaCO3 is used as a filler material initially as 40 m2/g of specific surface areas and 97.8% calcite content. Physical and
partial replacement of cement and gypsum in concrete, and some studies chemical properties of these materials are given in Table 1 and Figs. 1
have found it can be used as an economically beneficial material to and 2 shows the X-ray diffraction (XRD) analysis of cement, BFS, FA and
improve early strengths, accelerating hydration of concrete [27–33]. NC. It is clear that NC was less amorphous than BFS and FA by
Sato and Beaudoin [44] concluded that the addition of nano-CaCO3 as comparing the results. However, among both SCM, the BFS is more
partial replacement of cement accelerated the hydration of OPC and amorphous with amorphous content of 97.5% compared to 67.8%
acceleration was greater with a higher amount of nano-CaCO3. In their amorphous content of FA based on the quantitative XRD results. A
study, 10% and 20% of micro- and nano-CaCO3 were added to binder naphthalene sulphonate based superplasticiser was used to maintain the
along with 50% fly ash as partial replacement of cement. It is also found workability of pastes containing NC.
that micro-hardness and modulus of elasticity of hydration products at
an early age are significantly improved and increased with an increase in
1.3. Mix proportions
nano-CaCO3 contents. High volume replacement of cement with fly ash
increased workability and which causes the bleeding while the addition
A total sixteen mixes of high volume BFS pastes and high volume
of nano-CaCO3 minimises that workability especially for the concrete
BFSFA pastes mixes were prepared by partially replacing cement at 60%,
containing 40% fly ash [45].
70%, 80% and 90% in the first part of the study as shown in Table 2. Five
On the other hand, 5% addition of nano-CaCO3 significantly reduced
mixes among those were selected based on their 28 days compressive
the initial and final setting times of pastes samples with a 50%
strengths for further mixes to evaluate the effect of NC on compressive
replacement of cement with fly ash compared to ordinary cement paste
strength and microstructure of those HVS, and HVSFA pastes in the
and exhibited the same setting times when sonication process applied
second part of this study as shown in Table 3. The dosages of NC were
for the mixing of nano-CaCO3 [46]. It is reported that the use of 1%
varied from 1%, 2%, 3% and 4% by total mass of cementitious materials.
nano-CaCO3 in concrete containing 40% fly ash as partial replacement of
All the mixes had a constant water-to-cementitious materials ratio (w/b)
cement improved the compressive strengths by 46% and 54% at 3 days
of 0.4. Superplasticizer was used to maintain the adequate workability
and 28 days, respectively compared to control concrete containing 40%
of pastes containing NC by ranging from 0.5% to 1% by total mass of
fly ash as partial replacement of cement. However, no such great
cementitious materials.
improvement is noticed in the compressive strengths of concrete con
taining 59% fly ash and 1% nano-CaCO3 [47]. In this study, compressive
strengths of mortars showed improvement of about 25%, 15% and 1.4. Specimen preparation and curing
8.33% at 3, 28 and 90 days, respectively.
Moreover, it is found that 1% addition of nano-CaCO3 in high volume All mixes were prepared using a Hobart mixer at room temperature
fly ash concrete containing 59% fly ash reduced the water sorptivity by where dry cement, BFS and FA were mixed first for approximately for
19% and 60% than ordinary concrete at 28 days and 90 days, respec 3 min. In the first phase, water was added and mixed for a further 1 min
tively due to the formation of additional CSH gels. This study also re at low speed followed by adding superplasticisers when required and
ported significant improvement of durability properties due to the then again mixed for 1 min at high speed. In the second phase, NC and
inclusion of 1% nano-CaCO3 in high volume fly ash concretes. It is clear
from the above literature review that nano-CaCO3 improved the me Table 1
chanical and durability properties and enhanced the hydration process Physical properties and chemical compositions of Ordinary Portland Cement
of cement matrix as well as high volume fly ash matrix but there is no (OPC), Blast Furnace Slag (BFS), Class F Fly Ash (FA) and Nano-Calcium car
study reported its effects on the high volume slag and high volume slag- bonate (NC).
fly ash blended pastes containing more than 60% partial replacement of OPC Slag Fly-ash Nano
cement. This study is designed to investigate the effects of various nano- calcium
CaCO3 content varies from 1% to 4% on the 28 days compressive carbonate
strengths of high volume slag (HVS) and high volume slag-fly ash Chemical CaO 64.39 41.20 4.30 97.8a
blended (HVSFA) pastes ranges from 60% to 90% as partial replacement composition SiO₂ 21.10 32.5 51.11 –
(%) Al₂O₃ 5.24 13.56 25.56
of cement. Effects of nano-CaCO3 content in the microstructure of these
–
Fe₂ O₃ 3.10 0.85 12.48 0.02a
pastes after 28 days of curing are also presented in this study. MgO 1.10 5.10 1.45 0.5a
MnO – 0.25 0.15 –
1.1. Experimental details K2 O 0.57 0.35 0.7 –
Na2O 0.23 0.27 0.77 –
P2O5 – 0.03 0.88 –
The experimental program is divided into two parts. In the first part, TiO2 – 0.49 1.32 –
high volume slag (HVS) pastes containing 60%–90% slag as partial SO3 2.52 3.20 0.24 –
replacement of cement are considered. High volume slag-fly ash blended LOI 1.22 1.11 0.57 –
(HVSFA) pastes containing combined fly ash, and slag contents of 60%– Physical Particle 25–40% 40% of 50% of 15–40 nm
properties size �7 μm 10 μm 10 μm
90% are also included in this part. In the second part, the effects of Surface – – – 40
various nano-CaCO3 (NC) contents of 1%–4% on compressive strength area (m2/
and microstructures of HVS and HVFA pastes exhibited higher g)
compressive strength in the first part are evaluated. Thus, thirty-seven Specific 2.7 to 3.2 2.6 – –
gravity
mixes were prepared to evaluate the effect of nano-CaCO3 on those
HVS, and HVSFA pastes mixes. a
Information from supplier.
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 1. XRD analysis of Cement, Blast furnace slag and fly ash.
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Table 2
Mix proportions of cement paste containing high volume blast furnace slag (BFS) and slag-fly ash blend.
Mix Series Mix ID Mix proportion (wt. ratio) Water/Binder Superplasticizera
Table 3
Mix proportions of high volume slag and slag-fly ash blended cement pastes incorporation of nano-calcium carbonate (NC).
Mix Series NC (wt. %) Mix ID Mix Proportion (wt. ratio) Super-plasticizera
2. Results and discussion can be seen in Fig. 4b that the compressive strengths of HVSFA pastes
containing combined slag and fly ash content of 60% is higher than the
2.1. Compressive strength development control OPC and the HVS paste containing 60% slag in which the highest
compressive strength is shown by 30% replacement of slag by fly ash. On
2.1.1. Effect of high volume slag and high volume slag-fly ash blend the other hand, the compressive strengths of HVSFA pastes containing
Compressive strengths of different high volume slag and high volume combined slag and fly ash contents of 70%, 80% and 90% are lower than
slag-fly ash blend pastes at 28 days are shown in Fig. 4. It is evident from the control OPC paste and HVS pastes. Due to lower CaO content of
Fig. 4a that the compressive strength of HVS pastes is decreased when HVSFA pastes than the HVS pastes, the higher reduction of compressive
partial replacement of cement by blast furnace slag is increased more strength is observed in the HVSFA pastes.
than 60%. The compressive strength of HVS paste containing 60% slag
paste is 4% higher than the control OPC cement paste and very similar to 2.1.2. Effect of nano-CaCO3
the HVS cement paste containing 70% slag. However, about 9% The results in the first part show that the HVS paste containing 60%
reduction in compressive strength is observed in HVS paste containing slag shows higher compressive strengths than control OPC paste and
80% slag compared to control while huge reduction is noticed when the HVSFA paste containing combined slag and fly ash content of 90%
replacement increased to 90% as expected which is due to the extremely shows significantly lower compressive strengths than control OPC as
lower OPC content and slow hydration reaction of slag particles. Similar well as HVS paste 90% slag. Therefore, those two mixes were not
trends of compressive strengths of high volume slag composites at 28 considered in the second part of this study. Average compressive
days also reported in other studies [10,15]. The effects of different fly strengths at 28 days of different high volume slag and high volume slag-
ash contents of 30%, 40% and 50% as partial replacement of slag on 28 fly ash blend pastes incorporating various NC contents of 1%–4% are
days compressive strengths of HVSFA pastes are shown in Fig. 4b–e. It shown in Fig. 5 in comparison to that of control OPC and their respective
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2.2. Microstructure
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Fig. 4. Effect of high volume slag and slag-fly ash blend mixes on the compressive strengths of cement paste at 28 days of age.
slag and fly ash due to the addition of NC and formed additional CSH and 2.2.2. Thermogravimetric analysis (TGA)
CAH gels in mixes. Reduced larger and medium capillary pores of HVS The results of thermogravimetric analysis (TGA) of HVS and HVSFA
and HVSFA pastes with NC compared to control OPC paste will pastes with and without NC compared to control OPC paste are shown in
contribute to the resistance of penetration of detrimental ingredients Fig. 7a. The curves show the normalised mass loss of a substance in per
into the composites. cent (current mass divided by initial mass) under the control environ
ment as a function of temperature. It has been reported that mass loss
between 420 � C and 540 � C corresponds to the dehydration of calcium
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Fig. 5. Effect of Nano calcium carbonate on the compressive strengths of high volume slag and slag-fly ash blended paste at 28 days of age.
hydroxide [50]. It can be seen from the TGA curves that mass loss be However, in case of HVS paste containing 80% slag and HVSFA paste
tween those temperature ranges of HVS paste containing 70% slag due containing combined slag and fly ash content of 70% the weight loss is
to the addition of NC is lower than their reference paste as well as higher due to the addition of NC than their respective reference pastes
control OPC paste. This is clearly the evidence of lower amount calcium and control OPC paste, and it is more pronounced in the case of HVSFA
hydroxide in paste containing NC than the control paste indicating the paste. The amount of calcium hydroxide (CH) can also be quantified
formation of more CSH gel which was also shown in the MIP analysis. according to Taylor’s formula [51] shown as follows in equation (2):
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 6. Effect of nano-CaCO3 on the a) cumulative pore volume and b) pore size distribution of HVS and HVSFA pastes.
MWCH greater in HVS paste containing 80% slag after inclusion of NC. This
CHð%Þ ¼ WLCH ð%Þ (2)
MWH20 shows that NC did not produce much CSH in those paste rather formed
calcium aluminium hydroxide (CAH) hydrate and calcium carbonate
where WLCH is the weight loss during the dehydration of CH as a per hydrate due to the reaction with calcium oxide of slag which is also
centage of the ignited weight (%); MWCH is the molecular weight of CH; found in X-ray diffraction analysis of this study.
MWH2O is the molecular weight of H2O.
Fig. 7b shows the calculated CH contents of pastes with and without 2.2.3. X-ray diffraction (XRD) analysis
NC. It is clear that the CH content in all HVS and HVFSA pastes with and The reactions during cement hydration of HVS and HVSFA pastes
without NC is lower than the control OPC paste which indicates that with and without NC at 28 days are studied through XRD analysis. The
through pozzolanic reaction of SiO2 in slag and fly ash with CH the CSH horizontal scale is the diffraction angels measured in degrees, and the
is formed in those pastes. It can be also be seen that addition of NC vertical scale is the height of the peak of the intensity of the diffraction
reduced the CH content significantly by 37% in HVSFA paste which can measured in pulses/s. XRD patterns of control OPC paste and different
be interpreted due to the reaction of SiO2 of fly ash with CH in that paste HVS and HVSFA pastes are shown in Fig. 8a. The Diffraction spectra
sample. However, a slightly higher amount of CH is found in HVS paste analysis showed that an enormous amount of calcium hydroxide was
containing 70% slag due to the addition of 1% NC and this increment is formed in OPC paste as expected. By comparing diffraction spectrum of
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 7. TGA analysis a) High volume slag and High volume slag-fly ash blended pastes with and without nano-CaCO3 and b) Ca(OH)2 contents.
HVS containing 70% and 80% slag and HVSFA containing combined noticeable changes due to the addition of NC except a slight reduction of
slag and fly ash content of 70%, it is clear that the intensity of CH peaks intensity at 2θ angle of 47� . Also, a slight increase of CAH peak at 2θ
in those high volume mixes are significantly lower than the OPC paste, angle of 10.8� is observed in paste samples with NC.
and higher peak of calcium silicate hydrate (CSH) at 2θ angle of 31.4� Moreover, the intensity of CSH peaks at 2θ angle of 31.4� is also
and calcium aluminate hydrate (CAH) at 2θ angle of 10.8� is also found. increased due to the addition of NC and increase in the intensity of
This could be the reason for the high volume of slag and fly ash and less Ettringite is also noticeable at 2θ angle of 36� in the paste mixes with NC.
OPC which reduced the CH peaks and formed higher CAH and CSH due Moreover, the addition of NC increased calcium carbonate (CC) signif
to the pozzolanic reaction. Increased gehlenite (Ca2Al2SiO₇) at 2θ angle icantly at 2θ angle of 39.5� in all HVS and HVSFA pastes expectedly. In
of 20.8� and 39.5� and quartz at 2θ angle of 27� of paste mix containing the case of HVSFA paste new mineral peaks of Mullite (M), and Geh
combined BFS þ FA than HVS paste containing BFS only could be due to lenite (G) can be seen at 2θ angles of 16.5� and 20.8� , respectively with
the presence of fly ash in that mix. Fig. 8b shows a comparison of the an increase of Gehlenite peak due to the addition of NA.
XRD pattern of HVS and HVSFA pastes with and without the inclusion of
NC. It can be seen that the intensity of CH peak did not show any
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 8. XRD patterns of a) HVS and HVSFA paste b) HVS and HVSFA paste containing nano-CaCO₃.
2.2.4. Scanning electron microscopy (SEM) and energy dispersive X-ray microstructure. However, there are few unhydrated cements in OPC
spectroscopy (EDS) analysis paste (shown by the arrow) which are lower than the unhydrated/
Backscattered electron images of control OPC, high volume slag and partially hydrated slag particle in HVS paste and unhydrated or partially
high volume slag-fly ash blended pastes at lower magnification are hydrated fly ash particle in HVSFA paste. On the other hand, by
shown in Fig. 9 after 28 days of curing. It can be seen from the images comparing SEM images of HVS and HVSFA pastes, it is clear that HVS
that OPC paste indicates a comparatively dense microstructure with less paste containing 70% slag has denser microstructure than the other HVS
internal cracks and lower black spots than the other HVS and HVSFA and HVSFA pastes. Addition of NC improves the microstructure by
pastes without NC. The fewer number of representing more hydrated reducing the width of internal cracks in all HVS and HVSFA pastes can
products and black spots are an indication of pores/voids in the also be seen in the images in Fig. 10. Also, among all HVS and HVSFA
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Fig. 9. Backscattered electron images of a) OPC b) 70BFS c) 69BFS1NC d) 80BFS e) 76BFS4NC f) 49BFS21FA g) 49BFS20FA1NC pastes at lower magnification.
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 10. Backscattered electron images and EDS spectra of different HVS and HVSFA pastes with and without NC.
pastes, the high volume slag paste containing 69% BFS and 1% NC products (indicated by the arrow in SEM images) than the HVS paste
showed much denser microstructure than others, which is also clearly containing 70% slag. Also, Ca/Si ratio of the CSH gel from EDS spectra
revealed in the discussion of compressive strength. around a slag particle of paste containing NC is lower than the paste
SEM images with higher magnification and EDS spectra of HVS and without NC which indicates that the presence of NC in the paste accel
HVSFA pastes with and without NC are shown in Fig. 10. It can be seen erated the pozzolanic action of slag and increased the Si content of CSH
by comparing Fig. 10a and b that a thin rim had formed around the slag gel. Similar denser microstructural formation such as thin rim around
particle of HVS paste containing 1% NC and evidence of more hydration slag and fly ash particles also can be seen in the HVS paste containing
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
80% slag and HVSFA paste containing combined slag and fly ash of 70% 2.3. CO2 emission analysis
due to the addition of NC by comparing the higher magnification images
and EDS spectra of those mixes. On the other hand, by comparing all the CO2 emission analysis of different HVS and HVSFA pastes with and
HVS and HVSFA paste with NC, it is easily come to the conclusion that without NC are shown in Fig. 11a. The CO2 emission value of 971 kg/
the paste containing 70% slag had a much denser microstructure with tonne for OPC, 214 kg/tonne for slag, 18.9 kg/tonne for fly ash and
much higher hydrated particles and lower pores than the other mixes. In 1610 kg/tonne for nano-CaCO3 are taken from SimaPro software data
addition, a higher peak of silica in EDS spectra is also evident in HVS and base [52]. It can be seen in Fig. 11a a significant reduction of CO2
HVSFA pastes containing NC than their reference pastes, which also emission with increasing content of OPC replacement in all HVS pastes.
indicates the formation of more CSH/CAH in the matrix. However, a slight gradual increase in CO2 emission is observed in all
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
Fig. 11. CO2 emission and CO2 intensity indicator analysis of HVS and HVSFA pastes with and without nano-CaCO3.
HVS and HVSFA pastes with the increasing content of additional NC considerably low CO2 emission. It can also be seen that 1% NC inclusion
compared to their control paste without NC shown in Fig. 11a, though in both HVSFA pastes containing combined fly ash and slag contents of
the amount of CO2 emissions are way lower than the control OPC paste. 70% and 80% exhibited lower ci values among all the HVSFA pastes.
On the other hand, Fig. 11b shows the CO2 intensity indicator (ci ¼ c/ Nevertheless, the compressive strength of both mixes at 28 days age
p) [53] for all the mixes with NC which are considered according to their clearly favours the HVSFA paste containing combined fly ash and slag
28 days compressive strengths along with their control mixes without content of 70% with significantly lesser CO2 emission.
NC, where c is the total CO2 emission, and p is the average compressive
strength in MPa. It can be seen that three mixes of HVS pastes having a 3. Conclusions
similar value of ci ¼ 9.0. However, considering the 28 days compressive
strength values of those three mixes of HVS paste, it is clear that 1% NC Based on above discussion of the effects of various nano calcium
inclusion in HVS paste containing 70% slag and 4% NC inclusion in HVS carbonate contents on the 28 days compressive strengths and micro
paste containing 80% slag could produce a sustainable mixes with structure of high volume blast furnace slag and high volume blast
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A. Hosan and F.U.A. Shaikh Journal of Building Engineering 27 (2020) 100929
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