Construction and Building Materials 312 (2021) 125459

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Construction and Building Materials

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Properties of dredged sludge solidified with alkali-activated slag-based

materials and blended with copper slag as fine aggregates of mortars
Zhenzhong Chen 1, Nanqiao You 1, Chun Chen , Yamei Zhang *
School of Materials Science and Engineering, Jiangsu Key Laboratory of Construction Materials, Southeast University, Nanjing 211189, China

A R T I C L E I N F O A B S T R A C T

Keywords: Dredged sludge (DS), a waste with high annual output, is widely distributed in rivers and lakes worldwide.
Dredged sludge Although the application of DS as construction materials has been studied, it only focuses on cement-based
Solidification solidification, accompanied by low strength and high energy consumption. In this paper, to maximize waste
Alkali-activated slag-based materials
reuse and reduce carbon emissions, various industrial by-products (fly ash (FA), steel slag (SS) and ground
Copper slag
Mortars
granulated blast-furnace slag (GGBS)) were utilized to solidify DS to develop a novel construction material with
Construction materials relatively higher strength. Copper slag (CS), an industrial waste, was reused to replace natural sand (NS) as fine
aggregates of mortars. The properties of setting time, workability, rheological performance, hydration heat,
mechanical properties and water absorption were explored. The results show that the obtained 28d-compressive
strength is above 3.9 MPa, which reveals excellent cementitious effect of the binder. Compared with low strength
(LS, 50 wt% FA + 50 wt% GGBS) and middle strength (MS, 50 wt% SS + 50 wt% GGBS) group, high strength
(HS, 100 wt% GGBS) group presents faster setting time, lower spread, higher cumulative hydration heat, higher
strength and lower water absorption. The increase of replacement ratio of NS by CS improves workability, de­
creases yield stress and lowers water absorption. When 50% CS was used to replace NS, the strength increases
because more hydration products formed. But when the replacement ratio increases from 50% to 100%, the 28d-
strength variation is not obvious. Hence, CS can be recommended as a complete substitution for NS to maximize
solid waste utilization.

1. Introduction stabilization/solidification application, severed as a sustainable solution

for the disposal of several waste types, which will provide manufactures
Sludge, naturally deposited in flowing or still water environment, is and scientific research with a promising technique. Therefore, solidifi­
widely distributed in rivers and lakes worldwide. According to statistics, cation is a practical and available way to deal with DS. Currently, binder
over 20 billion cubic meters of sludge has been deposited in various like Portland cement (PC) is a common cementitious material applied to
rivers and lakes in China, and about 160 million cubic meters of sludge is solidify DS to achieve desired engineering properties. Cation exchange,
additionally generated every year, so the annual production of dredged flocculation/agglomeration, hydration, and pozzolanic reaction are
sludge (DS) is quite huge [1]. DS is a kind of fine-grained soil funda­ considered traditional soil stabilization mechanisms. Ca2+, Fe2+ and
mentally, with high clay content, high initial water content and some Al3+ released from cement could replace low valence metal cations
organic matter. The particle arrangement of DS is characterized by around clay particles, compressing absorbed water layer around clay
honeycomb and flocculated fabric caused by molecular attraction and minerals. As clay particles gather together, hydration products of
electrostatic force between soil particles, determining the characteristics cement could continuously fill the gap between soil particles and a
of high porosity, high compressibility and low bearing capacity [2]. Due strong soil-cement skeleton could be formed [4,5]. But relevant studies
to its poor natural engineering properties and high annual output, the found that cement-based binder still had some drawbacks. For example,
disposal of DS has become an urgent issue. organic matter in DS, including humic acid, would lower the pH and
The reuse of waste to minimize risks has received extensive atten­ combine with calcium and aluminum, greatly weakening the solidifi­
tion. Ferraro et al. [3] highlighted the cold-bonding process, a kind of cation effect of cement [6]. It was reported that humic acid severely

* Corresponding author.
E-mail address: ymzhang@seu.edu.cn (Y. Zhang).
1
Both authors have contributed equally.

https://doi.org/10.1016/j.conbuildmat.2021.125459
Received 30 June 2021; Received in revised form 10 October 2021; Accepted 26 October 2021
Available online 4 November 2021
0950-0618/© 2021 Elsevier Ltd. All rights reserved.
Z. Chen et al. Construction and Building Materials 312 (2021) 125459

decreased the unconfined compressive strength of soil samples, espe­ of solid waste, CS was used to replace NS to reduce the cost and increase
cially early strength. When the content of humic acid increased to 4.5%, economic benefits. A series of experiments were carried out to study the
the 7-day strength decreased by 89%. The addition of oxidants could setting time and hydration heat of AAM solidified DS (ASD) pastes, as
decompose organic matter and mitigate the negative effects caused by well as the workability, rheological performance, mechanical properties
organic matter [7]. Lang et al. [8] confirmed that the higher pH of and water absorption of ASD mortars.
alkaline environment could promote the dissolution of Si and Al, which
was conducive to the strength development of cement solidified DS. In 2. Experimental
addition, due to the high water content, high specific surface area and
single gradation of soil particles in DS, a large amount of cement has to 2.1. Raw materials
be added to achieve expected strength, so the solidification efficiency of
cement is not satisfactory. Moreover, cement is an industrial product The DS was taken from the Qinhuai River in Nanjing, Jiangsu
with high prices, high natural resources and energy consumption, which Province, China, and its basic properties are listed in Table 1. According
undoubtedly greatly increases the treatment cost of DS and environ­ to Chinese Standard JTG 3430-2020, the natural water content, organic
mental burden. It is estimated that per ton of cement produced will emit matter, specific gravity, plastic limit and liquid limit were tested and the
800 kg of CO2, and CO2 emitted by cement industry accounts for 5.5–7% studied DS was classified as high plasticity clay. The particle size dis­
of global anthropogenic CO2 emissions, seriously exacerbating the tribution curve of dry DS is shown in Fig. 1. The chemical composition of
greenhouse effect [9–11]. In consequence, the cement-based binder is dry DS determined by X-ray fluorescence (XRF) is listed in Table 2. It
not a good choice to stabilize DS and there is an urgent need for a green, could be seen that DS was mainly composed of SiO2 and Al2O3, both of
high-efficiency and low-cost binder to truly remedy the current situation which took up 81.13% of the total amount, and a small amount of Fe2O3
where a large amount of DS needs to be processed effectively. was also detected. XRD analysis shows that the main minerals in DS were
Alkali activated materials (AAM), known as low-carbon and envi­ quartz, illite, and kormelite, as seen in Fig. 2.
ronmentally friendly green cementitious material, a substitute for In this study, FA, SS and GGBS were used as precursors of AAM. Their
cement, could effectively achieve waste utilization and reduce green­ chemical compositions are shown in Table 2. The specific gravity of FA,
house gas emissions [12]. Because alkali solution is used as activator, SS and GGBS are 2.31 g/cm3, 3.15 g/cm3, and 2.95 g/cm3, and their
additional alkali source could form a more stable alkali environment and surface area is 454 m2/kg, 370 m2/kg, and 416 m2/kg, respectively.
compensate for pH loss caused by organic matter. Also, the character­ Precursors are activated by alkali activator, consisting of water,
istics of rapid hardening and early strength of AAM could meet the needs NaOH and water glass (WG) (9.52 wt% Na2O + 30.48 wt% SiO2 + 60 wt
of certain projects. % H2O). NaOH is analytically pure, with purity higher than 96% and the
Therefore, AAM as the binder has recently been explored to substi­ initial modulus Ms of WG is 3.31.
tute PC to solidify DS. Corrêa-Silva et al. [13] evaluated the behavior of CS and NS were used as fine aggregates, as shown in Fig. 3.
soft soil stabilized by 7.5% ground granulated blast-furnace slag (GGBS)- Compared with NS, the surface of CS is dense, glassy and angular. The
NaOH (total dry soil weight). Through X-ray diffraction (XRD) analysis, apparent density of NS and CS is 2612 kg/m3 and 3239 kg/m3, respec­
they discovered the dissolution of mineral phases (muscovite and albite) tively. Their particle size distribution was determined according to
and the formation of new cementitious gels. The leachate results Chinese National Standard GB/T 14684-2011, as shown in Fig. 4.
demonstrated that stabilized soil was classified as “inert waste” and
showed no risk for soil contamination. Lang et al. [14] investigated the
2.2. Preparation of ASD mortars
effect of different GGBS-based binders on stabilizing DS compared with
PC. They concluded that composite activator was superior to single
The details of mix proportions designed for ASD mortars are given in
activator in activating GGBS. The mass ratio of NaOH and Na2SiO3 in the
Table 3. The addition dosage of precursors was 30% of the mass of the
composite activator affected the development of unconfined compres­
untreated wet DS. According to the difference of targeted strength and
sive strength, and it was feasible to replace 20% PC with equivalent
volume replacement of NS by CS, ASD mortars in this investigation
GGBS binder (NaOH/Na2SiO3 = 2/3, 2/3, 1/4) to stabilize DS with
could be classified into 9 groups. LS represents low strength (50% FA
water content of 60%, 70% and 80% respectively. But current research
and 50% GGBS by mass in the precursor), MS represents middle strength
on DS is mainly limited to the application of ground improvement and
(50% SS and 50% GGBS by mass in the precursor) and HS represents
soil reinforcement, and the desired strength is generally low. Numerous
high strength (100% GGBS by mass in the precursor). The binder/fine
studies revealed that when different binders (PC, GGBS, fly ash (FA),
aggregates ratio was 0.5 and NS was replaced by CS with 0%, 50%, and
steel slag (SS), lime, carbide slag, etc.) with a dosage of 15–40% were
100% volume, respectively.
used, the unconfined compressive strength of solidified DS at 28 d with
The mole ratio of SiO2/Na2O in the alkali activator was designed to
water content of 60–90% was usually lower than 1–2 MPa [8,14–18].
be 1.2 and Na2O was 6% of the mass of precursors. The water/binder
This trend restricts the use of DS as a kind of construction material with
ratio was set to 0.4, which correspondingly referred to the liquid/binder
relatively higher strength.
ratio of 0.53.
Past research focused on the solidification effect of cement-based
The alkali activator solution was prepared by the following steps.
mortars on sludge [19–21], but the resources of natural sands (NS) are
limited. Copper slag (CS) is solid waste arising from copper production.
Table 1
When 1 ton of copper is manufactured, 2.2–3 tons of CS is produced
Basic properties of DS.
accordingly, and about 40 million tons of CS is generated annually in the
world copper industry [22–24]. Recently, CS as an alternative to NS has Property Value
gained widespread acceptance. You et al. [25] found that 20% and 40% Natural water content ω0 (%) 61.2
volume replacement of NS by CS in alkali-activated GGBS-FA mortars Organic matter (%) 3.1
could slightly increase fluidity and mechanical strength, inhibit drying Specific gravity Gs 2.57
shrinkage and refine pore structure of mortars. Plastic limit PL (%) 28.3
Liquid limit LL (%) 53.4
In this study, to make full use of DS, AAM is used as a low-carbon and Plastic index PI (%) 25.1
efficient binder to solidify DS to develop environmentally friendly Sand fraction (>0.075 mm, %) 12.4
construction materials. FA, SS and GGBS were used as precursors for Silt fraction (0.002–0.075 mm, %) 77.3
different active calcium content, and FA instead of metakaolin was Clay fraction (<0.002 mm, %) 10.3
Classification CH (high plasticity clay)
chosen for less expensive raw material [26]. To further increase the use

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(TAM AIR) at 20 ◦ C. The fresh ASD pastes were evenly stirred, poured
into a 20 ml high-density polyethylene ampoule, and then immediately
placed inside the calorimeter. The heat released was recorded by the
instrument over 7 d.
The ASD mortars were cast in molds of size 40 mm × 40 mm × 160
mm, vibrated to remove the air entrapped, then sealed with plastic film
to isolate humid air, and placed in a standard room (RH = 90 ± 5%, T =
20 ± 2 ◦ C) for curing. Due to the low early strength of ASD mortars,
according to the experience of previous experiments, the specimens
could not be demolded until 3 d to avoid the damage caused by
demolding. The flexural strength and compressive strength of cured
specimens at specific days were tested according to Chinese National
Standard GB/T 17671-1999.
Water absorption was measured according to Chinese National
Standard GB/T 2542-2012. The samples cured for 28 d were dried at 105
◦
C to constant weight and the dry weight was recorded. After that, they
were soaked in water for 24 h and the water on the surface was wiped
off, then the wet weight was recorded.
Fig. 1. Particle size distribution curve of dry DS. The microstructure of specimens was analyzed by Field Emission
Scanning Electron Microscope (FE-SEM, FEI-Sirion, Holland), and En­
The weighed NaOH and water were evenly mixed and then sealed to ergy Dispersive Spectrometer (EDS) was employed to determine the
prevent the water from evaporation. After the solution was cooled to composition of different phases.
room temperature, WG was poured and mixed uniformly and left for 24
h before use. 3. Results and discussion
Due to the sticky nature of DS, it was difficult to form uniform
mortars through traditional stirring methods. Therefore, a new stirring 3.1. Setting time
method was proposed to ensure the uniform dispersion of all ingredients
in the system. It is noted that to ensure that precusors were quickly The initial setting corresponds to the formation of gels and solidifi­
dissolved in alkali activator to reduce dilution and dispersion effect of cation of ASD pastes. At this moment, the generation of gels brings to the
DS, the mixing and stirring of precursors and alkali activator should be overlap of soil particles in DS, resulting in the plasticity loss of ASD
separated from DS instead of together. The procedure of ASD mortar pastes and the appearance of initial setting. As hydration reaction con­
preparation is illustrated in Fig. 5. Firstly, alkali activator was homo­ tinues, hydration products gradually increase, pastes completely lose
geneously mixed with precursors to form AAM pastes, while naturally their plasticity, and the final setting is reached while strength begins to
uneven DS was stirred to form DS paste. Secondly, the weighed fine develop.
aggregates according to the mass ratio of (AAM paste)/(DS paste) were It could be seen from Table 4 that the initial setting and final setting
separately incorporated and then mixed to achieve two kinds of even time of ASD pastes are significantly longer than those of normal AAM
mortars. Thirdly, AAM mortars were poured into DS mortars and stirred pastes. It could be attributed to the low mass of precursors which is only
at a high speed for 30 s, and then ASD mortars were obtained. Finally,
the mortars were cast in molds, sealed to insulate humid air and cured at
RH = 90 ± 5% and T = 20 ± 2 ◦ C.

2.3. Test methods

The initial and final setting time of ASD pastes was tested based on
Chinese National Standard GB/T 1346-2011. A fluidity tester for mor­
tars was used to measure the spread of ASD mortars based on Chinese
National Standard GB/T 2419-2005.
The rheological test of ASD mortars was carried out by RST-SST
Rheometer at 20 ◦ C with a VT20-10 rotor. The shearing system was
divided into acceleration stage and deceleration stage. The fresh ASD
mortars prepared by the procedure mentioned above were sheared, and
the rotation speed of the rotor was linearly accelerated from 0 r/min to
150 r/min within 75 s, and then linearly decelerated from 150 r/min to
0 r/min within 75 s. 150 data points were collected in either stage. The
test method was widely used in AAM according to relevant literature
[25].
Fig. 2. The mineralogy of DS from XRD test.
The hydration heat test was performed by isothermal calorimeter

Table 2
Chemical composition of DS, FA, SS and GGBS (%).
CaO SiO2 Al2O3 Fe2O3 MgO TiO2 SO3 K2 O P2O5 Na2O MnO LOI

DS 2.08 61.97 19.16 6.04 1.91 0.92 0.73 2.59 0.33 1.05 0.09 3.13
FA 3.89 46.73 36.94 4.31 0.58 1.56 1.25 0.95 0.55 0.39 0.04 2.81
SS 34.18 25.73 10.44 15.86 5.09 0.66 2.99 0.15 1.52 0.34 2.28 0.76
GGBS 41.65 29.33 14.91 0.27 7.03 0.68 3.67 0.25 0.02 0.48 0.15 1.56

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Z. Chen et al. Construction and Building Materials 312 (2021) 125459

Fig. 3. Comparison of the surface of (a) NS and (b) CS.

the perspective of formed hydration product amount. During the early

stage of hydration, the formation of hydration products (C-S-H and C-A-
S-H) mainly depends on the combination of SiO42− and Ca2+ [27,28].
There is a large quantity of available SiO42− provided by alkali activator
in the system, while the content of Ca2+ is dependent on precursors
dissolved in alkaline solution, so the early reaction is mainly controlled
by Ca2+. GGBS with more amorphous phases means higher reactivity
and more Ca2+ could be dissolved compared with FA and SS, hence the
setting of HS is the fastest.
The reasons that the setting of MS pastes is slower than that of LS
pastes could be explained from two aspects. Firstly, calcium in SS is not
easy to dissolve during early hydration. The amount of CaO in SS
(34.18%) is significantly higher than that in FA (3.89%), as shown in
Table 2, but in fact, calcium resolved is limited because the γ-C2S in SS is
relatively inert under alkaline conditions diluted by DS [29]. Secondly,
the negative effect of DS also leads to the slowest hydration speed. The
density of SS (3.15 g/cm3) is higher than that of FA (2.31 g/cm3), and
the actual volume occupied by SS is 75.39% of FA in a unit volume.
Fig. 4. The particle size distribution of CS and NS. Table 5 illustrates the volume fraction of each component in the unit
volume of ASD pastes. In MS pastes, the volume fraction of SS is 2.54%
30% of DS. Hence, the distance between precursors particles is far and lower than that of FA in LS pastes. This leads to 1.75% higher volume of
they are mainly surrounded by DS. Meanwhile, soil particles are also DS in MS pastes, which means more DS needs to be solidified by limited
dispersed due to the water in DS, so that the formed gels are hard to fill hydration products and would inevitably retard hydration. As for LS
big gaps between soil particles, which is called the dispersion effect of pastes, due to less volume of DS, when exposed to an environment where
DS. Furthermore, a large amount of water in DS dilutes the alkali acti­ humidity is lower than that of internal pastes, the water around soil
vator and reduces pH, which could make the dissolution rate of active particles migrates out more easily, then the soil particles draw closer due
particles much slower. This is called the dilution effect of DS. Conse­ to the soil suction, which contributes to the development of strength
quently, DS serves as inert material and its negative effect (dispersion [30]. When the setting time was tested, the sinking of the needle was
effect and dilution effect) on alkali-activated reaction is dominant, so the subject to resistance. Therefore, the beneficial effect of soil suction effect
hydration is greatly slowed down and the setting time of ASD pastes is on setting time is more obvious in LS pastes.
prolonged.
In Table 4, the initial and final setting time of HS pastes are the
fastest, while MS pastes are the slowest. This could be explained from

Table 3
Mix proportions for ASD mortars (kg/m3).
Precursors Alkali activator Fine aggregates DS

GGBS FA SS NaOH Water WG NS CS

LS-0 134.0 134.0 – 13.2 67.5 61.2 536.0 – 893.2

LS-50 134.0 134.0 – 13.2 67.5 61.2 268.0 332.3 893.2
LS-100 134.0 134.0 – 13.2 67.5 61.2 – 664.6 893.2
MS-0 134.0 – 134.0 13.2 67.5 61.2 536.0 – 893.2
MS-50 134.0 – 134.0 13.2 67.5 61.2 268.0 332.3 893.2
MS-100 134.0 – 134.0 13.2 67.5 61.2 – 664.6 893.2
HS-0 268.0 – – 13.2 67.5 61.2 536.0 – 893.2
HS-50 268.0 – – 13.2 67.5 61.2 268.0 332.3 893.2
HS-100 268.0 – – 13.2 67.5 61.2 – 664.6 893.2

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Fig. 5. The stirring and curing method of ASD mortar.

NS was around 1.2%, whereas CS had low water absorption of only 0.2%
Table 4
because of its dense and glassy surface [35,36]. The lower water ab­
Setting time of different ASD pastes (h:min).
sorption of CS means more free water works like lubricant in the system,
Group Initial setting Final setting so the friction between particles is reduced, leading to the increase of
LS 16:46 21:12 spread. Relevant literature also confirmed the improvement effect of CS
MS 26:06 28:14 on flowability [37,38]. Therefore, CS could work well in ASD mortars.
HS 14:53 18:54
On the one hand, the introduction of CS could help improve the work­
ability of ASD mortars. On the other hand, good cohesion of ASD mortars
could prevent segregation of CS from the matrix.
Table 5 The spread of fresh ASD mortars is largely related to the specific
The volume fraction of each component in the unit volume of ASD pastes (%). surface area of particles and aggregates. Compared with MS mortars, LS
Group Precursors Alkali activator DS and HS mortars exhibit lower spread, owing to the higher specific sur­
GGBS FA SS
face area of FA and GGBS than SS. Additionally, for HS mortars, angular
morphology of GGBS and more formation of primary C-A-S-H gels make
LS 8.08 10.32 19.75 61.85
particles easily agglomerate together [39–41].
–
MS 8.31 – 7.78 20.30 63.60
HS 16.54 – – 20.20 63.27

3.3. Rheological performance

3.2. Workability
The results of rheological tests measured by rheometer on different
The water content of as-received DS is high, and the fine soil particles mortars are shown in Fig. 7 and Table 6. It could be seen that with the
are highly hydrophilic, hence a considerable part of water is adsorbed on increase of shear rate, the shear stress increases linearly, which suggests
the surface of soil particles. When AAM and fine aggregates are intro­ that ASD mortars and DS paste are non-Newtonian flow. Hence, Bing­
duced into the system, the amount of free water decreases, making the ham model (Eq. (1)) was employed to fit the experimental data [42]:
system change from flow to plastic state. The spread of different fresh
τ = τ0 + μp γ̇ (1)
mortars is shown in Fig. 6.
The spread of ASD mortars, varing from 146 mm to 157 mm, shows
where τ represents shear stress (Pa), τ0 represents the yield stress (Pa), μp
favorable cohesion. Cohesion originates from suction stress between fine
soil particles caused by the surface tension of water. Generally, the represents plastic viscosity (Pa⋅s), and γ̇ represents shear rate (s− 1).
smaller soil particles mean higher suction stress and good cohesion Plastic viscosity is an index to evaluate the size and quantity of flocs,
[31,32]. It was reported that when CS used as fine aggregates exceeded a and yield stress characterizes the strength and quantity of inter-floc
certain range, it would cause segregation and bleeding, not only in AAM interrelations that are invalid when shear is applied [43]. Previous
system (e.g. alkali-activated GGBS-FA mortars [25]), but also in PC studies confirmed that solid content was an important parameter that
system (e.g. PC concrete [33]). However, due to the excellent matrix affected rheological behavior [44]. For DS paste, high water content of
cohesion from the suction of soil particles [34], a stable environment the paste determines its low plastic viscosity and yield stress. Obviously,
could be offered to hold heavy aggregates like CS uniformly without the introduction of AAM pastes and fine aggregates increases the overall
segregation. yield stress and plastic viscosity. The 9 groups of mortars are 2.05–3.22
It could be seen that the spread increases with the increment of CS times the yield stress of DS paste. When more free water is adsorbed
replacement ratio. Relevant studies show that the water absorption of around fine aggregates, the distance between soil particles decreases,
leading to the increase of friction between particles and the enhanced

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Fig. 6. Spread of (a) LS-0 mortar, (b) LS-50 mortar, (c) LS-100 mortar, (d) MS-0 mortar, (e) MS-50 mortar, (f) MS-100 mortar, (g) HS-0 mortar, (h) HS-50 mortar and
(i) HS-100 mortar.

resistance of the system to flow when subjected to shear [45,46]. the presence of SS in MS pastes has an obvious promotion effect on the
In Fig. 7, LS-0, MS-0 and HS-0 mortars exhibit higher yield stress hydration of GGBS. Due to its low specific surface area of SS, relatively
compared with mortars in respective groups, but with the increment of less alkali activator could be absorbed on the surface of low activity SS,
volume replacement of NS by CS, the yield stress decreases accordingly. while more absorbed on GGBS. More alkali activator could penetrate the
It is the angular morphology of CS (Fig. 3) that influences rheological hydration product layer and contact with GGBS, contributing to the
properties. As described in the literature [47], yield stress would further reaction. For HS pastes, the rapid reaction of GGBS could cause
decrease as particle morphology gets further from the spherical shape. the precipitation of a layer of hydration products on the surface,
delaying the further reaction of GGBS. Therefore, the exothermic peak of
MS pastes appears at the earliest time (58 h).
3.4. Hydration heat The exothermic peaks of MS, HS and LS pastes reach 0.16 mW/g,
0.28 mW/g and 0.11 mW/g, respectively. This is because hydration is
Hydration heat mainly reflects the reaction between precursors and mainly controlled by Ca2+ concentration during this period [49]. More
alkali activator in the ASD pastes. Fig. 8 describes the hydration heat GGBS in HS pastes could release a large amount of Ca2+ to generate
flow and cumulative hydration heat of ASD pastes within 168 h. The hydration products, which contributes to the highest exothermic peak.
exothermic peaks of MS, HS, and LS pastes appear at 58 h, 80 h, and 108 Relevant literature revealed that calcium in SS was mainly in the form of
h, respectively. Unlike AAM pastes, the exothermic peaks of ASD pastes C2S, followed by merwinite and bredigite, of which only C2S was hy­
are greatly delayed and their duration is longer. It confirms that the draulic and the others non-hydraulic [50,51]. Therefore, apart from
addition of DS reduces the pH of the solution, leading to the slowing- GGBS, SS in MS pastes could also additionally provide active calcium
down of the dissolution of precursors. sources in the system and has a higher exothermic peak compared with
At 0–2 h, the cumulative hydration heat increases rapidly (Fig. 8(b)), LS pastes.
due to the full contact of the precursors and alkali activator in the After that, the hydration rate decreases with time and the reaction
preparation of AAM pastes (Fig. 5), making most of the precursors reaches the deceleration period. At 168 h, cumulative hydration heat of
dissolve quickly. At 2–36 h, the reaction of ASD pastes reaches the in­ ASD pastes is dependent on the active calcium content that precursors
duction period, which corresponds to the precipitation of primary C-A-S- could provide in respective pastes, of which HS pastes are the highest
H [48]. Then MS pastes firstly reach acceleration period at 36 h, fol­ (58.38 J/g), while LS pastes are the lowest (33.39 J/g) for the limited
lowed by HS pastes at 55 h and LS pastes at 64 h. The exothermic peak of Ca2+ dissolved from precursors.
MS pastes appears 22 h earlier than that of HS pastes (Fig. 8(a)). In fact,

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Table 6
Plastic viscosity and yield stress of different mortars.
Group Plastic viscosity (Pa⋅s) Yield stress (Pa)

LS-0 1.47 499.86

LS-50 1.67 343.20
LS-100 1.42 341.43
MS-0 1.72 449.52
MS-50 1.48 448.86
MS-100 1.31 387.29
HS-0 1.48 535.68
HS-50 1.98 402.08
HS-100 1.71 370.33
DS paste 0.64 166.37

Fig. 8. (a) Hydration heat flow and (b) cumulative hydration heat of
ASD pastes.
Fig. 7. Rheological behavior of different mortars (a) LS mortar, (b) MS mortar,
(c) HS mortar. be attributed to the excellent cementitious effect of binder and a new
stirring method proposed (Fig. 5).
3.5. Mechanical properties From Fig. 9, HS mortars exhibit relatively higher strength and the
strength of MS mortars is higher than LS mortars, which is consistent
The flexural and compressive strength of ASD mortars with different with the active calcium content provided by precursors. As for MS
CS content from 3 d to 28 d are shown in Fig. 9. The number in the mortars, the strength is a little higher than that of LS at 3 d, 7 d, and 14 d,
legend (0, 50, 100) stands for the replacement ratio (%) of NS by CS. while at 28 d, the flexural and compressive strength is 20.9% and 55.0%
With the increase of curing ages, almost all groups exhibit a growing higher than that of LS mortars, respectively. This indicates that the
trend. Among all mortars, the flexural strength is higher than 1.0 MPa strength growth of MS mortars is mainly concentrated at 14–28 d, owing
and the compressive strength lies in the range of 3–14 MPa at 28 d. to the hydration of SS.
Generally, the flexural strength and compressive strength of ASD mor­ In all groups, when 50% CS is used to replace NS, the 28d-flexural
tars are higher than those of previous research [8,14–18], which could strength and 28d-compressive strength of LS mortars increase by

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CS. Water absorption measures the volume of water-accessible pores.

Corresponding to the cumulative hydration heat above, the water ab­
sorption of HS mortars is the lowest, standing for the most hydration
heat and hydration products, while LS mortars is the highest for the least
hydration products.
It could be seen that with the increase of CS substitution amount, the
water absorption decreases accordingly, which is consistent with pre­
vious research [53]. For LS mortars, when CS replacement ratio grad­
ually increases, the water absorption decreases by 0.8% and 1.1%,
respectively, and MS mortars also show a similar tendency. But for HS
mortars, the reduction of water absorption is relatively larger, with a
decrease of 1.4% and 1.4%, respectively. Obviously, the incorporation
of CS indeed helps improve the workability of ASD mortars, decrease the
air bubbles introduced and form a more compact structure. Further­
more, the low water absorption of CS helps promote the hydration de­
gree of precursors and generate more hydration products. The result is
consistent with the mechanical properties mentioned above.

3.7. SEM analysis

Fig. 10 (a) shows the surroundings around the soil particle. Ac­
cording to EDS result, the soil particle is mainly composed of Si and Al
phase, which is consistent with the XRF test results above. The uniform
and smooth soil particle is tightly enwrapped by hydration products, and
the boundary is dense and continuous. This confirms the effective so­
lidification effect of AAM on soil particles in DS.
The comparison of the typical boundary of NS and CS with matrix is
shown in Fig. 10 (b) and Fig. 10 (c). It could be observed that the
morphology of CS is angular and sharp-edged, while NS is relatively
rough. It is evident that there is an interfacial zone where more pores are
observed near the NS particle in Fig. 10 (b), while the matrix and CS
particle are very closely packed with no obvious interfacial zone in
Fig. 10 (c). Through higher magnification observation shown in Fig. 10
(d), it could be seen clearly that the hydration products adhere tightly to
the surface of CS. Fig. 10 (e) shows the leaching trace of CS, indicating
that CS has been dissolved to a certain extent and participates in the
Fig. 9. (a) Flexural strength, and (b) compressive strength of ASD mortars with hydration reaction, which makes the adhesion between CS and hydra­
different CS content from 3 d to 28 d. tion products tighter. This might also explain the promoted strength and
the low water adsorption of the mortars with the replacement of NS by
17.1% and 37.3%, respectively, and MS mortars increase by 42.5% and CS.
29.4%, respectively. This demonstrates that the replacement of 50% NS
by CS indeed enhances the strength development of mortars. Due to the 4. Conclusions
low spread of ASD mortars, the increase of CS could release more free
water to improve workability as mentioned above, so more uniform and In this investigation, AAM was utilized to solidify DS and CS was
compact mortars could be obtained. Furthermore, due to low water used to replace NS to prepare ASD mortars, The effect of different ASD
absorption of CS, less alkali activator is absorbed around CS, then pre­ pastes (50 wt% FA + 50 wt% GGBS, 50 wt% SS + 50 wt% GGBS and 100
cursors could have a more fully contact with more alkali activator, wt% GGBS) and different volume replacement ratio (0%, 50% and
which brings more hydration products and contributes to strength 100%) of NS by CS was explored. A new stirring method was proposed to
development. But this beneficial effect is limited when CS content ex­ ensure quick dissolution of precursors and uniform dispersion of all in­
ceeds a certain range. In most groups, when 100% CS was used to gredients. The obtained 28d-compressive strength is above 3.9 MPa and
replace NS, the flexural and compressive strength of 100% CS groups is water absorption is below 24.9%. According to the results of this study,
close to 50% CS groups, but still significantly higher than 0% CS groups. the main conclusions are summarized as follows:
Rajasekar et al. [52] found that in the ultra high strength concrete sys­
tem, the optimum replacement ratio of untreated CS was 40%, and the (1) The setting time of ASD pastes is greatly prolonged due to the
strength decreased when CS beyond 40% because the existence of more dispersion and dilution effect of DS. The longest setting time of
free water caused more porous matrix. Wu et al. [38] and Al-Jabri et al. MS pastes is owing to the limited calcium resolved from SS and
[33] also reached similar conclusions in different systems. But in ASD the significant negative effect of DS. Good cohesion of ASD
mortars, the strength reduction of complete CS group is not significant mortars could effectively prevent segregation of CS from matrix.
for excellent cohesion. Therefore, it is recommended to use CS as a
complete substitution for NS to maximize the utilization of solid waste. Table 7
Water absorption of ASD mortars at 28 d (%).
Group 0 50 100
3.6. Water absorption
LS 24.9 24.1 23.0
Water absorption of ASD mortars is listed in Table 7, and the number MS 24.4 23.7 23.1
HS 23.9 22.5 21.1
in the header (0, 50, 100) stands for the replacement ratio (%) of NS by

8
Z. Chen et al. Construction and Building Materials 312 (2021) 125459

Fig. 10. SEM images of different mortars (a) HS-50, (b) (c) LS-0 and (d) (e) LS-50.

In ASD mortars, the increase of the replacement ratio of CS by NS (4) From SEM images, the soil particle is tightly enwrapped by hy­
contributes to better workability and lower yield stress; dration products, showing the effective solidification effect of
(2) The exothermic peak of MS pastes is 22 h earlier than that of HS AAM. An interfacial zone with more pores could be observed near
pastes, because the presence of SS in MS pastes has an obvious NS particle, while the matrix and CS particle are very tightly
promotion effect on the hydration of GGBS. Cumulative hydra­ packed with no obvious interfacial zone. The leaching trace of CS
tion heat of HS pastes is the highest, followed by MS and LS could also be observed, confirming that CS participates in the
pastes; hydration reaction, which makes the adhesion between CS and
(3) The water absorption of ASD mortars decreases with the increase hydration products tighter.
replacement ratio of CS by NS, of which HS mortars decline most
significantly. The proper replacement ratio of NS by CS increases
the strength due to the low water absorption of CS. More free CRediT authorship contribution statement
water is released to help form a more compact structure and more
alkali activator promotes the hydration degree of precursors; Zhenzhong Chen: Conceptualization, Investigation, Writing –
original draft, Formal analysis, Data curation. Nanqiao You:

9
Z. Chen et al. Construction and Building Materials 312 (2021) 125459

Conceptualization, Formal analysis, Writing – review & editing, Super­ [20] B. Mansour, D. Rocheddine, M. Karim, B. Youcef, Stabilization/solidification of
industrial waste sludge of hydroxides in mortars and concretes, Rev. Rom. Mater.
vision. Chun Chen: Writing – review & editing, Supervision. Yamei
47 (3) (2017) 406–414.
Zhang: Conceptualization, Methodology, Writing – review & editing, [21] L. Chaabane, K. Moussaceb, A. Aït-Mokhtar, Factors affecting the leaching of heavy
Supervision, Funding acquisition. metals (Ni+2, Pb+2, Cr+3) contained in sludge waste stabilization/solidification
by hydraulic benders, Part I: water/cement and waste/cement ratio in S/S mortars,
Environ. Progress Sustainable Energy 36 (1) (2017) 93–103, https://doi.org/
10.1002/ep.v36.110.1002/ep.12450.
Declaration of Competing Interest
[22] C. Shi, C. Meyer, A. Behnood, Utilization of copper slag in cement and concrete,
Resour. Conserv. Recycl. 52 (10) (2008) 1115–1120, https://doi.org/10.1016/j.
The authors declare that they have no known competing financial resconrec.2008.06.008.
interests or personal relationships that could have appeared to influence [23] K.D.O.B.E. Ravindra, B. Jorge de, M. Raman, L. Chao Qun, Sustainable
Construction Materials: Copper Slag, first ed., Woodhead Publishing, Duxford, U.
the work reported in this paper. K., 2017.
[24] D. Wang, Q. Wang, Z. Huang, Reuse of copper slag as a supplementary
cementitious material: Reactivity and safety, Resour. Conserv. Recycl. 162 (2020)
Acknowledgment
105037, https://doi.org/10.1016/j.resconrec.2020.105037.
[25] N. You, Y. Liu, D. Gu, T. Ozbakkaloglu, J. Pan, Y. Zhang, Rheology, shrinkage and
The authors greatly acknowledge the support provided by the Na­ pore structure of alkali-activated slag-fly ash mortar incorporating copper slag as
fine aggregate, Constr. Build. Mater. 242 (2020) 118029, https://doi.org/10.1016/
tional Natural Science Foundation of China (No. 51972057).
j.conbuildmat.2020.118029.
[26] G. Roviello, L. Ricciotti, O. Tarallo, C. Ferone, F. Colangelo, V. Roviello, R. Cioffi,
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