Construction and Building Materials 211 (2019) 73–79

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Construction and Building Materials

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Development of Alkali-activated Cementitious Material using

Copper Slag
Jagmeet Singh, SP Singh 1,⇑
Dr B R Ambedkar National Institute of Technology, Jalandhar, India

h i g h l i g h t s

 CS was use as source of aluminosilicate for development of ACM.

 The mixes were activated using alkali content of 5% and 7% by weight of binder.
 Addition of mineral admixtures in alkali-activated CS improves its performance.
 MK was found to be more effective than FA.

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

Article history: The paper presents results of an investigation conducted to study the feasibility of use of Copper Slag (CS)
Received 18 September 2018 as aluminosilicate material for developing Alkali-activated Cementitious Material (ACM). The effect of
Received in revised form 15 March 2019 addition of mineral admixtures such as Fly Ash (FA) and Metakaolin (MK) on the performance of
Accepted 18 March 2019
alkali-activated CS was also investigated. In addition to a control mix which was prepared using 100%
CS; two other mixes were also prepared by replacing CS with 30% FA and 30% MK respectively. These
mixes were activated using alkali content of 5% and 7% by weight of binder. Sodium hydroxide and
Keywords:
sodium silicate were used as alkali-activators. Compressive strength tests were performed on alkali-
Alkali-activated Cementitious Material
Compressive strength
activated cement mixes at different curing ages. The pore-size distribution, mineralogy and microstruc-
Copper Slag ture of selected alkali-activated cement mixes were determined using Mercury Intrusion Porosimetry
Microstructure (MIP), X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray
Porosity Spectroscopy (EDS). Test results indicate that CS has great potential as aluminosilicate material for devel-
oping ACM. Further, the addition of mineral admixtures in alkali-activated CS cement improves its per-
formance; however, the addition of MK was found to be more effective than FA in terms of compressive
strength and microstructure development.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction ashes and zeolites. The reaction products of alkali-activation

Alkali-activated Cementitious Material (ACM) is a product of a
chemical reaction of aluminosilicate material and an alkali compo-
nent at high temperature. Purdon in 1940 developed the first ACM
using slag as aluminosilicate material and caustic soda as an alkali
component [1]. In 1978, Davidovits introduced a new term for this
reaction, which was known as geopolymerization [2]. The sources
of aluminosilicate materials may be industrial wastes such as
Ground-Granulated Blast Furnace Slag (GGBFS), Fly Ash (FA), Rice
Husk Ash (RHA) and natural pozzolans i.e. calcined clay, volcanic
⇑ Corresponding author.
E-mail address: spsingh@nitj.ac.in (SP Singh).
1
Department of Civil Engineering, Dr B R Ambedkar National Institute of
Technology, Jalandhar 144011, India.
depend upon the chemical composition of aluminosilicate materi-
als. High calcium binders react with alkali activators, produce C-
(A)-S-H–type gel and low calcium binders produce N-A-S-(H) type
gel, where N represents Na+ or K+ cations [3,4]. Alkali-activated
cementitious materials provide comparable mechanical properties
to Portland Cement (PC) and have greater resistance to corrosion,
acid attack and chemical attack [5–7]. Alkali-activation of indus-
trial waste takes many economic and environmental benefits as
the production process of ACM releases less CO2 and requires less
energy as compared to PC [8,9].
In earlier studies, ACMs were mainly derived from precursors
such as GGBFS and FA and its chemical composition, physical prop-
erties and optimum synthesis parameters (i.e. activator type, acti-
vator content, curing type and curing temperature) are briefly
described in the literature [5,6]. However, the growing demands

https://doi.org/10.1016/j.conbuildmat.2019.03.233
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
74 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79

of ACMs and supplementary cementitious materials lead to the
consumption of significant amount of GGBFS and FA. According
to a rough estimate, the use of GGBFS and FA in cement production
was of the order of 43.7 million tons and 39.8 million tons respec-
tively in the year 2015 [10]. As cement consumption increases
rapidly, these materials are expected to fulfill approximately 20%
requirement of total cement production by 2050 [11]. So, there is
a need to identify the new aluminosilicate materials such as Cop-
per Slag (CS), which may be used as a precursor for the develop-
ment of ACM.
Copper Slag is metallurgical waste generated during the
extraction of copper from copper ores. During smelting phase
reducing agent (Silica) separates the sulphides and oxides, which
are present in the Copper ores. The sulphides do not make any
anions and develop matte phase (Copper rich) and reducing
agent combines with oxide to form slag phase (Impurities rich).
The water quenching of slag produces glassy, amorphous and
granulated slag. Copper Slag has a specific gravity in the range
of 3.4–3.7 and consists of Fe (30–40%), SiO2 (35–40%), Al2O3
(<10%), CaO (<10%) and Cu (0.5–2.1%) [12]. It was estimated that
in the smelting process, 2–3 times more CS is generated than
copper and approximately 24.6 million tones of CS is generated
annually worldwide [12]. Copper slag usually dumped at sites,
which creates environmental issues and utilizes the valuable
land. As per National Green Tribunal, around 3.52 lakh tonnes
of CS has dumped at Thoothukudi (Tamil Nadu, India), which
affecting the surrounding agricultural land and water ways
[13]. Copper Slag can be used as an abrasive material, manufac-
turing of floor tiles and glass-ceramic [14–16]. Copper slag has
been used in construction industry as aggregates [17,18] and
also cementitious materials [19,20]. The presence of alumina
and silica in the CS makes it suitable as precursor in the
alkali-activation [21–23]. Ahmari et al. [21] developed the ACM
using CS and mine-tailing (MT) as source of aluminosilicate. It
was found that ACM synthesis using 100% CS and cured at
90 °C for 7 days exhibits the maximum compressive strength
up to 50 MPa. Nazer et al. [22] studied the effect of curing time
and curing temperature on the performance of alkali activated
CS cement matrices. The performance of heat cured specimens
at 65 °C for 3 days was similar to ambient cured specimens at
20 °C for 90 days. Qianmin et al. [23] studied the effect of
elevated temperature on the mechanical properties of alkali-
activated CS. The optimum elevated temperature for alkali-
activated CS was 200 °C, above this mechanical properties of
alkali-activated CS was reduced due to the decompositions of
hydration products.
From above literature, it can be observed that heat curing of
After that the final concrete mix will be evaluated in terms of cost,
energy suitability and environmental sustainability.
2. Experimental programme
2.1. Materials used
Copper Slag obtained from Rajasthan, India was used in the investigation. To
enhance the performance of alkali-activated CS, FA and MK were added as addi-
tional source of alumina and silica. The chemical composition of CS, FA and MK
was determined using X-ray fluorescence and is shown in Table 1. Commercially
available MK was used, which is supplied as MetaCem 85C and has calcining tem-
perature of 600–800 °C. It can be seen from Table 1 that there is significant amount
of Fe2O3 in CS. The role of Fe2O3 in the geopolymerization process is vague. Other
than CS, Fe rich slags have been thoroughly studied as potential precursors,
although it remains yet unclear exactly how it participates at the atomic level in
geopolymerization. The Standard sand conforming to IS 650 [24] was used to pre-
pare alkali-activated cement mortars. Locally available Sodium Hydroxide (SH) and
Sodium Silicate (SS) was used as alkali-activators. The SH was supplied in pellet
form with 98% purity, whereas SS was supplied in solution form with Ms = 3.3
(Si2O = 26.5%, Na2O = 8%, H2O = 65.5% by weight). Only CS was ground in Laboratory
Ball Mill using 20 mm and 25 mm stainless steel balls for 2 h to attain its fineness
equal to FA. As such there in no standard available regarding specification of CS for
use as cement. However, the specification of FA for use with cement is given in
Indian Standard 3812. According to this standard, FA particles retained on 45 mm
IS sieve should be less than 34%. Therefore, to attain equal and more fineness than
FA, CS was sieved through 45-mm sieve.
The ratio of stainless steel balls (kg) to CS (kg) was 2. The parentage passing
through 45-mm sieve for CS, FA and MK was 95%, 82% and 100% respectively. The
specific gravity and BET surface area of used materials is given in Table 1.
The X-ray Diffraction patterns of CS, FA and MK are shown in Fig. 1. The XRD
patterns show that CS is a fully amorphous material with minor peaks of crystalline
mineral i.e. Fayalite (F) and Clinoferrosilite (C) and slags with a high degree of amor-
phous content reflect higher reactivity towards alkali-activation [5]. Strong devia-
tions of crystalline minerals; Quartz (Q) and Mulite (M) were detected on 2h
range of 15° to 40° in MK and FA and some peaks of Magnetite (MT) and Sillimanite
(SM) were also detected. Except these crystalline peaks, MK and FA were observed
to be partially amorphous materials.
2.2. Mix proportions of alkali-activated cement mortars
Alkali-activated cement mortars were prepared using CS, MK and FA as a binder
with standard sand in the ratio of 1:3. In addition to a control mix which was pre-
pared using 100% CS; two other mixes were also prepared by replacing CS with 30%
FA and 30% MK respectively. These mixes were activated using alkali content of 5%
and 7% by weight of the binder. Sodium hydroxide and sodium silicate were mixed
to prepare the alkali activator solution of modulus Ms = 1.25 (Ms = Si2O/
Na2O = 1.25), which was constant for all the mixes. A water-to-solid ratio of 0.3
was fixed for all the mixes. Mix proportions of different mixes for 1000 g of the bin-
der are given in Table 2.
2.3. Mixing, casting and curing
To prepare alkali activator solution, sodium hydroxide flakes were dissolved in
water and then sodium silicate was added in this solution and stirred constantly.

alkali-activated CS gives better results than ambient curing. How-

ever, the effect of addition of mineral admixtures on the perfor- Table 1
mance of alkali-activated CS is scanty in literature. Therefore, the Chemical composition and physical properties of CS, FA and MK.
aim of the present study is to develop the alkali-activated CS with
Compound (%) Composition
addition of mineral admixtures. The addition of mineral admix-
tures in alkali-activated CS could improve its performance and will CS FA MK

make it more suitable as cementitious material. The alkali- Si2O 37.6 56.6 58.1
activation process of CS was evaluated through compressive Al2O3 11.5 31.5 39.1
Fe2O3 42.4 4.72 1.21
strength tests conducted on mortar specimens with different per-
CaO 3.80 1.10 0.23
centages of CS and mineral admixtures. The results of microstruc- Na2O 0.74 0.10 0.08
ture analysis, porosity and reaction products of different mixes K2O 0.76 0.35 0.09
were also evaluated and compared. TiO2 0.37 1.62 0.83
SO3 0.01 0.32 0.13
It is mentioned here that the work reported in this paper is part
MgO 0.57 0.36 –
of a larger investigation on the strength and durability properties MgO 0.62 0.02 –
of alkali-activated copper slag concrete. First, the optimum synthe- P2O5 0.13 – –
sis parameters for alkali-activation of copper slag such as alkali MnO 0.01 – –
content, type of alkali, curing regime and mineral admixtures will Loss on ignition (%) 1.50 3.3 0.23
Specific gravity 3.21 2.34 2.62
be selected. The effects of these synthesis parameters on the
BET surface area (m2/kg) 503 465 1055
mechanical and durability properties of concrete will be evaluated.
 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79 75

Fig. 1. XRD patterns of CS, FA and MK.

Table 2
Mix proportions for 1000 g of binder (By weight).

Mix CS (g) FA (g) MK (g) Sand (g) SH (g) SS (g) Water (g) Alkali content W/S ratio
1 1000 – – 3000 40 236 181 5% 0.3
2 700 300 – 3000 40 236 181 5% 0.3
3 700 – 300 3000 40 236 181 5% 0.3
4 1000 – – 3000 56 330 135 7% 0.3
5 700 300 – 3000 56 330 135 7% 0.3
6 700 – 300 3000 56 330 135 7% 0.3

W/S ratio = Water/Solid ratio, where water is water in activator and extra water; Solid is solid part of activators and binders.

The alkali activator solution was prepared 24 h prior to mixing to cool down the
temperature of the solution. First, dry materials such as CS, FA, MK and standard
sand were weighed in the required quantity and put into the mortar mixture and
mixed for 5 min. Subsequently, alkali activator solution was added in the mixer
and mixed for another 2 min. After the mixing, the mortar was poured into cube
specimens of size 50  50  50 mm and sealed to prevent any moisture loss.
Though expected, the authors did not observe any significant loss in workability
on account of addition of MK. It can be seen from literature that the performance
of heat cured alkali-activated CS specimens was better than ambient cured speci-
mens [21–23]. Keeping this in view, the authors selected heat curing for the
alkali-activation of CS. After the casting, the cube specimens in sealed condition
was placed into oven and heat cured for 24 h at 80 °C along with moulds. The spec-
imens de-moulded and placed in laboratory conditions at a temperature of 25 ± 3 °C
and relative humidity of 50 ± 5% until testing. The specimens were cured in labora-
tory conditions for 3, 7 and 28 days until testing.
2.4. Compressive strength test
The compressive strength tests on alkali-activated CS cement mortars were
conducted as per IS 516 [25]. The compressive strength was determined using com-
pression testing machine of capacity of 2000 kN at a loading rate of 0.6 kN/s.
2.5. Pore-size distribution and porosity
Pore-size distribution and porosity of alkali-activated CS cement mortars were
determined using Mercury Intrusion Porosimeter (MIP) at a pressure range of 0.2–
50,000 psia. For MIP, samples were collected from broken cubes after conducting
compressive strength tests at 28 days of curing of some of the mixes made with
an alkali content of 5%. Prior to testing, the samples were dried in an oven at a tem-
perature of 100 °C until constant weight was achieved.
2.6 Microstructure and mineralogy
The microstructure of alkali-activated samples was observed using high-
resolution field emission Scanning Electron Microscopy (SEM) with Energy Disper-
sive X-ray Spectroscopy (EDS). Samples for SEM were put in ethanol to stop the
reaction and then dried in an oven up to constant weight and for better observa-
tions; all samples were gold-coated. Mineralogical study of alkali-activated samples
was carried out using X-Ray Diffraction (XRD). The XRD patterns were obtained
using a Cu-Ka radiation under conditions of 45 kV and 40 mA. For SEM and XRD
tests, samples were collected from broken cubes after conducting compressive
strength tests at 28 days of curing of some of the mixes made with an alkali content
of 5%. The XRD test was also performed on raw aluminosilicate materials such as CS,
FA and MK.
3. Results and discussion
3.1 Compressive strength
The compressive strength results of different mixes of alkali-
activated CS cement mortars with different alkali contents and cur-
ing ages are shown in Fig. 2. The 28 days compressive strength of
alkali-activated CS mortars for 5% and 7% alkali content was
27.56 MPa and 34.12 MPa respectively, which seems to be suffi-
cient for structural applications in various construction works.
The amorphous nature of CS helps in the dissolution of silicates,
which promotes the alkali-activation process and improves com-
pressive strength [22]. The amorphous materials are structurally
76 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79
Fig. 2. Effect of alkali content on compressive strength of alkali-activated mixes (a)
CS (b) CS + FA and (c) CS + MK.
disordered and these materials can easily breaks down in to its
constituents. Due to amorphous nature of CS, when it meets highly
alkaline environment, dissolution or break down of different con-
stituents such as alumina and silica takes place. The effect of curing
ages, alkali contents and mineral admixtures on compressive
strength of alkali-activated CS mortars is briefly described in the
following sections.
3.1.1. Effect of curing ages on compressive strength
From Fig. 2, it was observed that the compressive strength of all
mixes was increased with increase in curing age. The increment in
compressive strength with curing age was symmetric in the all
mixes; however major portion of compressive strength was gained
in just 3 days of curing. In all mixes, up to 80% of 28 days compres-
sive strength was achieved in 3 days of curing. This can be attrib-
uted to the heat curing of mixes, which accelerate the alkali-
activation process of binders and develop the compressive strength
in short curing periods. It was also observed in the literature that
during the heat curing of alkali-activated CS mortars, maximum
gain in compressive strength was achieved in just 3 days of curing
period [22].
3.1.2. Effect of alkali content on compressive strength
The effect of alkali content on the compressive strength of dif-
ferent mixes is presented in Fig. 2. It was found that the compres-
sive strength of all mixes was increased with an increase in alkali
content. With the increase in alkali content, the compressive
strength of mix CS was increased from 23.75 MPa to 31.46 MPa
at 3 days, 25.63 MPa to 32.41 MPa at 7 days and 27.56 MPa to
34.12 MPa at 28 days of curing as shown in Fig. 2(a). A similar
trend was also observed for mix CS + FA shown in Fig. 2(b),
wherein compressive strength was increased from 25.27 MPa to
33.55 MPa at 3 days, 26.74 MPa to 36.27 MPa at 7 days and
30.72 MPa to 39.01 MPa at 28 days of curing. It can be seen that
with the increase in alkali content from 5% to 7%, the compressive
strength of mix CS + MK as shown in Fig. 2(c) was increased by
12.95%, 11.47% and 11.11% at 3, 7 and 28 days of curing respec-
tively. Higher content of alkali provides extra species of Si and
Na, where Na dissolves the silicate and aluminate from the binders
and extra Si species from activator helps in formation aluminosil-
icate gel [26,27]. The solidification of aluminosilicate gel results
in the formation of the alkali-activated binder, which improves
the compressive strength of mixes.
3.1.3. Effect of mineral admixture on compressive strength
The effect of different mineral admixtures on the compressive
strength of alkali-activated CS mortars is shown in Fig. 2. It was
observed that the addition of mineral admixtures improved the
compressive strength of alkali-activated CS mortars. However,
the addition of MK was more effective in improving the compres-
sive strength than the addition of FA in alkali-activated CS mortars.
For 5% and 7% alkali content, CS + MK mix exhibits maximum com-
pressive strength of 40.78 MPa and 45.31 MPa at a curing age of
28 days as presented in Fig. 2(c). The performance of MK additive
mixes was better than other mixes due to its chemical composition
and fine particles. Metakaolin contains some large amount of sili-
cate and alumina than FA and CS (Table 1), which is released in
the presence of alkali media and combines with alkali cations to
form cross-link gel, which acts as a binder and strengthen the
alkali-activated CS mortars [28]. Also, the fine particles of MK than
FA and CS make it more reactive and provide the large surface area
than FA and CS for alkali-activation.
3.2. Pore-size distribution and porosity
The porosity and pore-size distribution of selected samples
were determined by MIP. Samples were collected from broken
cubes of 28 days compressive strength tests of mixes made with
CS, CS + FA and CS + MK activated with 5% alkali content. The
porosity of different mixes measured is shown in Fig. 3. The poros-
ity of alkali-activated CS mix was highest amongst all the mixes i.e.
15.12%, followed by mix made with CS + FA = 11.97% and mix con-
taining CS + MK = 10.11%. It can be seen that with the addition of
FA and MK, the porosity of alkali-activated CS mixes was
 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79
Fig. 3. Porosity of alkali-activated CS, CS + FA and CS + MK mixes, 5% alkali content.
decreased. However, the addition of MK was found to be more
effective in reducing the porosity than FA. The reduced porosity
of mix containing MK may be attributed to the finer particles of
MK compared to FA, which is responsible for better particle pack-
ing and results in the dense microstructure. The pore-size distribu-
tion of different mixes is shown in Fig. 4, where the pores are
separated into mesopores (<50 nm diameter) and macropores
(>50 nm diameter). It has been found that MK-based mixture con-
sists of macropores, however the macropores compared to FA and
CS mix were negligible. The alkali-activation of MK produces NASH
type gel, which fills most of the macropores and gives more refined
structure than mixes containing FA and CS. The porosities have a
direct relationship with the compressive strength of ACM. Lower
porosity gives the refined structure and a more refined structure
of ACM can acquire uniform stress distribution, which leads to a
higher compressive strength [29–31]. The mix containing MK hav-
ing least porosity shows better compressive strength than mixes
containing FA and CS.
3.3. Mineralogy
X-ray diffraction patterns of mixes activated with 5% alkali con-
tent are shown in Fig. 5. The XRD patterns of various mixes tested
in this investigation indicate crystalline peaks of quartz and mul-
Fig. 4. Pore size distribution of alkali-activated CS, CS + FA and CS + MK mixes
indicating Mesopores and Macropores, 5% alkali content.
77
Fig. 5. XRD patterns of alkali-activated CS, CS + FA and CS + MK mixes, 5% alkali
content.
lite. The crystalline peaks of quartz and mulite were initially pre-
sent in MK and FA (Fig. 1), which were also reflected after alkali-
activation in Fig. 5. The alkali-activated CS mix also shows the crys-
talline peak of quartz and mullite, which may be due to non-
reactive silicate species. It was observed that new hydration prod-
ucts formed during alkali-activation process were not detected in
XRD patterns may be due to their amorphous nature. However,
the MK mix contains very small peaks of zeolite X, which is alumi-
nosilicate mineral and represents the existence of aluminosilicate
gel.
3.4. Microstructure
Micrographs of alkali-activated CS, CS + FA and CS + MK mixes
with 5% alkali content were detected using SEM and are shown
in Fig. 6. It can be observed that alkali-activated CS mix shows
maximum micro-cracks as seen in Fig. 6(a). Some micro-cracks
were also observed in alkali-activated CS + FA mix as can be seen
in Fig. 6(b), but alkali-activated CS + MK mix shows most compact
and dense microstructure in Fig. 6(c). In addition to this, some
geopolymer gel phase was also detected as a brightened portion
in the alkali-activated CS + MK mix. Microstructure analysis
reflects that alkali-activated CS mix has most porous structures,
but the addition of FA and MK makes its structure dense due to
the formation of geopolymer gel and smaller particle size of FA
and MK also helps in solidification of the microstructure of
alkali-activated CS mix. Due to the densest microstructure of
alkali-activated CS + MK mix, it demonstrates the highest compres-
sive strength amongst all mixes.
Test results of EDX analysis of alkali-activated mixes are also
shown in Fig. 6. The Al/Si ratio is most important factor in alkali-
activated materials for determination the behavior of geopolymer
gel. The increase of Al/Si ratio indicates more dissolved aluminum
in alkaline medium and which enhances its contribution in forma-
tion of geopolymer gel [32]. In Fig. 6(f), alkali-activated mix CS
+ MK shows maximum Al/Si ratio, which indicates its well-
formed geopolymeric matrix. Some atoms of Fe are shown in
EDX of alkali-activated mixes of CS and CS + FA in Fig. 6(d) and
(e) respectively. The lower compressive strength of alkali-
activated CS and CS + FA mixes is due to presence of Fe in these
mixes. The existence of Fe in alkali-activated mixes provides resis-
tance to discharge of Si and Al in an alkaline environment, which
78 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79

Fig. 6. SEM micrographs of alkali-activated mixes (a) CS (b) CS + FA (c) CS + MK and EDX analysis results of alkali-activated mixes (d) CS (e) CS + FA (f) CS + MK, 5% alkali
content.

opposes the alkali-activation process and thus results in reduced
compressive strength [21].
4. Conclusions
Following conclusions can be drawn from the present study:
(a) All alkali-activated mixes achieved 80% of 28 days compres-
sive strength within 3 days due to heat curing.
(b) The compressive strength of all alkali-activated mixes was
increased by more than 11%, when alkali content was
increased from 5% to 7%.
(c) Alkali-activated CS mix activated using 7% alkali content
exhibits compressive strength of the order of 34.12 MPa,
which seems to be sufficient for structural applications in
various construction works.
(d) The compressive strength of alkali-activated CS was
increased by more than 11% and 32% with addition of FA
and MK respectively. The microstructure of alkali-activated
CS was also improved with addition of FA and MK.
(e) In general it can concluded that CS can be used as alumi-
nosilicate in the development of ACM. The addition of FA
and MK in alkali-activated CS makes it more suitable as
cementitious material in construction industry.
 J. Singh, SP Singh / Construction and Building Materials 211 (2019) 73–79
Acknowledgments
The authors acknowledge financial assistance in the form of a
fellowship to the first author from the Ministry of Human Resource
Development (MHRD), Government of India. The authors also
acknowledge the help from the staff of Concrete Technology and
Structures Testing Laboratories at Dr B R Ambedkar National Insti-
tute of Technology, Jalandhar during the experimentation work.
Conflict of interest
The authors declare that there is no conflict of interests regard-
ing the publication of this article.
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