Cement and Concrete Composites 134 (2022) 104773

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Cement and Concrete Composites

journal homepage: www.elsevier.com/locate/cemconcomp

Improving the effectiveness of internal curing through engineering the pore

structure of lightweight aggregates
Li Yang a, Xianwei Ma c, Jianhui Liu d, Xiang Hu a, **, Zemei Wu a, Caijun Shi a, b, *
a
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, International Innovation Center for Green &
Advanced Civil Engineering Materials of Hunan Province, College of Civil Engineering, Hunan University, Changsha, 410082, China
b
Department of Civil Engineering, The University of British Columbia, Vancouver, BC, V6T 1Z4, Canada
c
College of Civil and Transport Engineering, Henan University of Urban Construction, Pingdingshan, 467036, China
d
Key Laboratory of Disaster Prevention and Structural Safety of China Ministry of Education, School of Civil Engineering and Architecture, Guangxi University, Nanning,
530004, PR China

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

Keywords: A low absorption rate and a small thermal conductivity coefficient are the main targets in the preparation of
Fine lightweight aggregates traditional coarse lightweight aggregate (LWA). Fine LWA is generally used as internal curing materials and
Paper sludge crushed from coarse LWA. Large pores or low water absorption will reduce the effectiveness of internal curing. In
Bauxite tailings
this study, a waste-based fine LWA with high water absorption (≥20%) has been made of bauxite tailings, silica
Internal curing
fume, and paper sludge. The pore structure formation of fine LWA was analyzed. Time-dependent water ab­
High-strength mortars
sorption, water desorption, and pore structure of fine LWA were tested. Their effects on the early-aged hydration,
autogenous shrinkage, pore structure, and compressive strength of high-strength mortars were studied. The
results showed that different from the isolated and large pore structure of the expanded shale, fine LWA had a
connected and fine pore structure of 200–2000 nm. It could absorb about 30.6% water by mass and quickly
reaches saturation, and more than 95% of water absorbed was released at 97% relative humidity (RH). Fine LWA
had a good water retention capacity and did not result in the delay of the main hydration. The capillary pore size
of 20–50 nm increased and the total porosity reduced due to the increased degree of hydration. Compared to the
high-strength mortars with the same mixing water content, fine LWA reduced the autogenous shrinkage of
mortars by up to 88% and increased the strength of mortars by up to 2.5%.

1. Introduction
Pre-saturated or pre-wetted lightweight aggregates (LWA) are
commonly used as internal curing materials to mitigate the autogenous
shrinkage and sustain the hydration of concrete with low water to binder
(w/b) ratio [1,2]. But the conclusions on the strength of concrete are
quite different. It has been reported that LWA reduces the compressive
strength of concrete [3,4]. While some researchers have found positive
results on the strength of concrete [5,6]. These inconsistent findings are
attributed to the difference in the LWA itself, mixing proportion, curing
conditions, etc. [7–9]. LWA of small particle size decreases the defects
caused to concrete and more evenly distributed particles in the matrix
can improve the effectiveness of internal curing, which can offset the
negative effects of LWA itself on concrete strength to a certain extent
[10]. However, the particle size of LWA should be within a reasonable
range.
Coarse LWA for structural concrete is usually prepared to meet the
requirements of lightness, low thermal conductivity, and a low absorp­
tion rate. This LWA has a very large pore size, mostly between tens to
hundreds of microns. While fine LWA is often used as the internal curing
material of high-performance concrete and ultra-high-performance
concrete, it is usually crushed from coarse LWA. The crushing opens
some closed large pores, but the water absorption has little change.
Water retention capacity is very poor due to the large pore size, some
water absorbed is easily lost during the mixing [10,11]. This will in­
crease the initial w/b ratio and adversely affect the porosity and strength
of concrete. Besides, when this LWA is further crushed into smaller sizes,
too small pore size will make it difficult to absorb water, and the inhaled

* Corresponding author. Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, International Inno­
vation Center for Green & Advanced Civil Engineering Materials of Hunan Province, College of Civil Engineering, Hunan University, Changsha, 410082, China.
** Corresponding author.
E-mail addresses: xianghu@hnu.edu.cn (X. Hu), cshi@hnu.edu.cn (C. Shi).

https://doi.org/10.1016/j.cemconcomp.2022.104773
Received 14 April 2022; Received in revised form 17 August 2022; Accepted 13 September 2022
Available online 17 September 2022
0958-9465/© 2022 Published by Elsevier Ltd.
L. Yang et al.
water is difficult to release [10,12]. As a result, the mitigating effect of
autogenous shrinkage is limited [3]. In summary, large pores or low
water absorption will reduce the internal curing effect of LWA [7]. It is
necessary to produce LWA with the development of open and inter­
connected porosity (increased water absorption) and appropriate pore
size through optimizing the composition of raw materials and control­
ling calcinating conditions, to achieve a better internal curing effect.
Most LWA currently on the market are manufactured by firing nat­
ural raw materials like vermiculite, shale, clay, slate, or waste materials
in rotary kilns (at maximum temperatures from 1000 to 1300 ◦ C) [13,
14]. In the calcinating process, the LWA experiences a bloating/foaming
process. However, this mechanism is unsuitable for the preparation of
LWA for internal curing since the gas expansion results in large and
isolated pores. In general, calcinating slowly at a relatively low tem­
perature (below 1000 ◦ C) and a high content of the organic residue in
the matrix can result in an open porosity, but the bloating of LWA is
absent [15,16]. Paper sludge is a kind of waste material generated from
the paper industry. It is estimated that for every ton of paper produced,
approximately 0.4 tons of waste is generated [17]. Many solutions have
been proposed for the disposal of paper sludge. One of the most common
solutions is the landfill. It not only causes serious environmental prob­
lems but also a high cost for the industry because the high humidity
content of paper sludge results in transportation difficulties [18]. Other
applications have been proposed for paper sludge, for example, as the
raw material of brick [19], ceramics and cement [20], and fine sand
[21]. Considering that paper sludge is rich in carbonate and organic
matter, it can be used as a pore-forming agent to increase the porosity of
the matrix. Bauxite tailings are a by-product after the physical separa­
tion of bauxite. About 0.2 t of tailings is generated for every 1 t bauxite
ore processed by flotation [22]. Large quantities of bauxite tailings not
only occupy large space but also cause damage to the environment.
In this study, bauxite tailings and silica fume were used as bulk
materials, and the effects of paper sludge amount on the formation of
Fig. 1. The schematic diagram for preparing LWA.
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Cement and Concrete Composites 134 (2022) 104773
fine LWA were investigated. The properties and pore structure of fine
LWA were compared to those of commercial expanded shale. A high-
water absorption (≥20%) of fine LWA was used for the internal curing
of high-strength mortars. The autogenous shrinkage, compressive
strength, hydration heat, and pore structure of high-strength mortars
were tested.
2. Preparation of LWA
2.1. Treatment of raw materials
Bauxite tailings and paper sludge were from local plants in Henan
Province, China. Before use, they were both pretreated as shown in
Fig. 1. The dried powder obtained was preserved in polyethylene vessels
to avoid humidification.
It should be noted that such materials may be characterized by
different chemical and mineralogical features from one batch to another.
To ensure the repeatability of the LWA performance, the material
characteristic should be analyzed before LWA production. If the chem­
ical composition of other batches of materials is quite different, other
materials need to be added for adjustment.
2.2. Characteristic analysis of raw materials
The X-ray fluorescence (Rigaku Supermini200 spectrometer) was
used to analyze the oxide contents of the bauxite tailings. As shown in
Table 1, the main chemical compositions of bauxite tailings were Al2O3
(44.68%) and SiO2 (34.54%). It is known that Si and Al are the main
components of the LWA skeleton, which provide strength for the LWA.
The ratio of Al2O3/SiO2 in the materials affected the calcination tem­
perature and range [23]. As the ratio increased, the calcination tem­
perature and range also increased. The high content of Al2O3 in bauxite
tailings increases the Al2O3/SiO2 ratio, which increases the melting
L. Yang et al. Cement and Concrete Composites 134 (2022) 104773

Table 1
Chemical composition of raw materials (wt.%).
Sample code Al2O3 SiO2 Fe2O3 K2O CaO Na2O MgO LOI

Bauxite tailings 44.68 34.54 10.64 4.86 0.55 0.49 0.46 12.7
Silica fume 0.17 96.75 0.05 0.49 0.26 0.24 0.50 3.2
Paper sludge 1.27 1.86 8.99 0.20 80.71 0.34 1.46 48.8

Noted: LOI refers to loss on ignition (at 1050 ◦ C for 2 h).

temperature. Different from the SiO2 in quartz, SiO2 in silica fume is

Table 2
amorphous silicon. During the firing process, the Si4+ is solidified in
Mixture proportions of different LWAs.
tectosilicate with network tetrahedron of SiO4− 4 and decreases the
forming temperature of the liquid phase [24]. Therefore, the addition of Sample code Mixture proportion (wt.%)

silica fume can be considered to increase the content of the flux agent. Bauxite tailing Silica fume Paper sludge
With the increase in the amount of silica fume, a more liquid phase was S0 95 5 0
generated in the green body. According to our preliminary study, further S5 90 5 5
increasing the content of silica fume would result in a reduction in the S10 85 5 10
water absorption of LWA. Therefore, 5% silica fume was kept constant in S20 75 5 20
S30 65 5 30
all mixtures. More CaO (80.71%) in the paper sludge indicated the
presence of calcite. A high LOI of paper sludge suggested a high amount
of gas generated in the firing process, which contributes to the devel­ gas release can enhance the particle voids to form pore channels. The
opment of the porous structure. pellets continued to be fired at 1050–1150 ◦ C for 5 min, with a heating
The mineral compositions of the bauxite tailings were determined by rate of 10 ◦ C/min. After then, the samples were cooled to room tem­
Rigaku X-ray diffractometer with Cu Kα radiation, scanning from 5◦ to perature inside the laboratory electrical furnace.
70◦ with a step size of 0.02◦ at a rate of 2◦ /min. Rietveld analyses were
carried out to provide a semi-quantitative analysis of the crystalline 3. Materials and methods
phases by using rutile (20% by mass of the powder) as a reference. XRD
pattern and quantitative XRD results are plotted in Fig. 2. The main 3.1. Materials and mixtures
mineral components of bauxite tailings were illite (KAl2(Si3Al)
O10(OH)2), diaspore (AlOOH), kaolinite (Al2Si2O5(OH)4) and other less P.I. 42.5 Portland cement and silica fume were used as the binder.
abundant components such as hematite (Fe2O3) and montmorillonite Cement was purchased from China Building Materials Research Institute
(Na0.3Al4Si6O15(OH)6(H2O)4). Co., Ltd, and silica fume was purchased from Hunan Guli engineering
new materials Co., Ltd. A commercial polycarboxylate-based super­
2.3. Mix design and firing procedure plasticizer (SP) was used to guarantee workability, which was obtained
from Sika building materials Co., Ltd. Natural river sand from Xiang­
Dried powders were first mixed thoroughly to ensure homogeneity jiang River, Hunan Province, China, and two types of LWA fired at
according to the designed proportions in Table 2. Then 20–22% of water 1050 ◦ C were used as fine aggregates. The particle size distributions of
was added to the mixture and spherical pellets of approximately 2–5 mm the three types of sand are shown in Fig. 3.
in diameter were obtained. The fresh pellets were first placed in a The internal curing effectiveness of LWA is affected particularly by
ventilated area for 6 h and then dried at 105 ◦ C in an oven for 12 h. The the size of aggregates [8,25]. If the particle size of LWA decreases, the
dried pellets were then fired in a laboratory electrical furnace to form distribution of weak areas tends to homogenize. Therefore, these fired
LWA. Detailed methods for firing the fresh pellets are shown in Fig. 1. balls were crushed and sieved to obtain particles with a size below 1.18
Preheating treatment of 700 ◦ C for 2 min was first employed to maxi­ mm. The 24 h water absorption ratios of crushed LWA are 22.5% for S10
mize the dehydroxylation of phyllosilicates, decomposition of carbon­ and 30.6% for S30.
ates, and the combustion of the organic matter so that a large amount of

Fig. 2. XRD pattern of bauxite tailings. Fig. 3. Sieve analyses of employed aggregates.

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L. Yang et al. Cement and Concrete Composites 134 (2022) 104773

Four different mix designs of mortars were adopted to investigate the Table 4
internal curing performance of LWA. The mixture proportions of mor­ Salts used for control of RH in the measurement of water release.
tars are shown in Table 3. The method developed by Bentz [26] was used Saturated salt solution K2SO4 KNO3 BaCl2–2H2O KCl KBr
to estimate the amount of internal curing water and the corresponding
RH 97% 94% 90% 85% 80%
volume of LWA. The amount of internal curing water was 5.8% of binder
mass in all mixtures. The amount of LWA varied depending on their 24 h
water absorption. deformation starting approximately 1 h after mixing. Nevertheless, all
the results are referenced to the length at the final set to comply with
ASTM 1698 [30]. The final set of the mixtures was confirmed when the
3.2. Experimental methods penetration resistance value reached 28 MPa, according to GB/T
50080-2016 [31]. The samples were then placed on a rigid
3.2.1. Properties and microstructure of LWA length-measuring gauge, after measuring the original length. The
The loose bulk density and water absorption (24 h) of LWA were autogenous shrinkage data were recorded at intervals of 10 min. The
tested following Chinese standards GB/T 17431.2 (2010) [27]. When whole setup was maintained in a constant temperature humidity
used for internal curing, water absorbed by LWA has to be readily chamber at 20 ◦ C, until the test age of 48 h.
released to the surrounding cementitious matrix. To study the water
release of LWA, some saturated salt solutions were used to control 3.2.3. Compressive strength of mortars
different humidity between 97% and 80% (Table 4) in a sealed desic­ For the compressive strength test, the mixed mortar was cast into the
cator. The desorption test device is shown in Fig. 4, and the specific molds with the size of 40 × 40 × 40 mm3. They were demolded after 24
operation steps are as follows: the LWA samples were first soaked in h and then cured in the standard chamber (RH>95%, 20 ± 2 ◦ C) until
water for 24 h and the water of the aggregate surface was removed based the testing ages (3, 7, and 28d). At each age, a compression test was
on the paper towel method Castro et al. [28]; about 20 g saturated LWA carried out on three samples, with a loading rate of 0.6 MPa/s.
samples were placed in a porous pan with a pore size smaller than 1 mm;
the samples were first stored in a desiccator with the highest RH value 3.2.4. Pore structure of mortars
for 5 days at 20 (or 23) ± 1 ◦ C followed by weighing before moving to 1
H nuclear magnetic resonance (NMR) relaxometry was employed to
the next desiccator with a lower RH. After finishing all the desorption assess the pore structure of the mortars. More theoretical details and
processes, the samples were then oven-dried at 60 ◦ C for 2 weeks to explanations of the NMR basics can be found in Ref. [32]. The time
obtain the final equilibrium dry weight. The water content of LWA at constant of the disappearance of transverse magnetization is called the
each RH value can then be calculated based on the measurement. Two transversal relaxation time (T2). For the determination of T2 relaxation
replicates of each group were used to calculate the average value. time, the Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence was
The surface of the raw LWA and their interior structure were employed. The NMR results were transferred into pore size distribution
observed using a Phenom Pharos Desktop environmental scanning according to the following equation [33].
electron microscopy. The backscattered electron (BSE) imaging mode
was performed, with an electron beam energy of 10 kV and magnifica­ 1 S
= ρ( )pore =
F×ρ
(1)
tions of 5000 × . Raw LWA was broken with a hammer. Then, the T2 V r
aggregate particles with flat cross-section were selected to observe the
Where, T2 is the transversal relaxation time of water (m/s); (S/V) is the
interior. A mercury intrusion porosimeter (MIP, Micromeritics AutoPore
specific surface area of the pore, determined by pore surface area (S) to
Iv 9510) was adopted to analyze the pore structure of LWA. Pores with
volume (V) ratio, μm− 1; ρ is surface transverse relaxation strength, μm/s;
sizes from 800 μm down to 5 nm could be measured via the intrusion of
F is a geometrical factor; r is the radius of the pore.
mercury into the connected pores under an intrusion pressure of up to
207 MPa. The mineral composition of LWA was analyzed using a Rigaku
3.2.5. Early-aged hydration
X-ray diffractometer with Cu Kα radiation. The 2θ scans were carried out
The heat of hydration of the binder in different mortars was
between 5◦ and 70◦ with a step size of 0.02◦ at a rate of 2◦ /min. Rietveld
measured by a TAM Air 08 Isothermal Calorimeter for 72 h at 20 ◦ C.
analyses were carried out to provide a semi-quantitative analysis of the
River sand was excluded in the mixtures and LWA was included. All
crystalline phases by using rutile (20% by mass of the powder) as a
mortars were mixed outside and transferred to glass bottles. The glass
reference.
bottles were sealed and placed into the calorimeter. Three replicates
were prepared for each batch.
3.2.2. Autogenous shrinkage of mortars
A non-contact corrugated tube system equipped with a laser sensor
4. Results
was employed to measure the autogenous shrinkage of mortars [29,30],
as illustrated in Fig. 5. A fresh mixture was cast into the corrugated tubes
4.1. Effects of paper sludge amount on properties and microstructure of
with a length of 400 mm and a diameter of 30 mm using a wide-mouth
fine LWA
funnel. The free ends of the specimens were immediately sealed using
stainless steel covers. Automatic measurements allowed recording the
4.1.1. Bulk density and water absorption
Fig. 6 shows the effects of paper sludge amount and calcination
Table 3
temperature on the bulk density and water absorption of fine LWA. The
Mixture proportions of mortar (kg/m3).
bulk density decreased with the increase in paper sludge amount. The
Num. Binder River LWA Extra Basic SP higher the amount of paper sludge amount, the greater the LOI values,
sand w/b w/b
Cement Silica resulting in the reduction of particle mass. The dehydroxylation of
fume phyllosilicates and decomposition of calcite occurs usually in the calci­
REF-0.3 855 212 1067 – – 0.3 2.1 nation area below the sintering temperature of LWA. As the rapid sin­
REF- 855 212 1067 – – 0.358 1.1 tering was not applied in this study, the generated gas is released to the
0.358 outside. Therefore, the open and interconnected porosity of LWA was
M-S10 855 212 658 276 0.058 0.3 2.1
developed. This increased the water absorption of LWA, and the higher
M-S30 855 212 715 203 0.058 0.3 2.1
the amount of paper sludge amount, the greater the absorption value.
Note: M-S10 refers to the mortars with S-10.

4
L. Yang et al. Cement and Concrete Composites 134 (2022) 104773

Fig. 4. The diagrammatic sketch of the setup to measure water desorption of LWA.

Fig. 5. Setup for autogenous shrinkage measurement.

Fig. 6. Effects of paper sludge amount and calcination temperature on the (a) bulk density and (b) water absorption of LWA.

5
L. Yang et al.
Also, it can be seen that the water absorption decreased with the in­
crease of calcination temperature, but this effect decreased when the
paper sludge amount was high. The bulk density also showed similar
results.
While Rong et al. [34] found that the addition of more than 10%
paper sludge increased the bulk density of LWA when clay and fly ash
were used as raw materials. This can be attributed to the bloating phe­
nomenon associated with the formation of closed porosity due to the
trapping of part of the gases generated. In their study, paper sludge was
conducive to the formation of a glassy phase in the sintering process. The
amount of liquid phase increased with the increase of paper sludge
amount, and the viscosity of the liquid phase decreased at high tem­
peratures. This led to gas escaping and affected the bloating of LWA. As a
result, the volume of LWA became smaller and the bulk density
increased.
4.1.2. Microstructure
The surface texture is an important factor affecting the water ab­
sorption of LWA. A well-vitrified surface of LWA makes the outer surface
impervious to water [35]. Fig. 7 shows the effects of paper sludge
amount on the interior and surface of fine LWA at 1050 ◦ C. A large
number of narrow pores are observed both in the interior and on the
surface of LWA. The paper sludge amount had hardly influenced the
pore size of LWA. Paper sludge contains high content of carbonates and
organic matter. With the increase of paper sludge amount, the high
content of pore generating components increases the connectivity of
particle gap, which is conducive to the formation of open pores. With the
increase of calcination temperature to 1150 ◦ C (Fig. 8), the pores of LWA
with low paper sludge amount are significantly reduced, and an external
glassy film can be observed. While 30% paper sludge makes the LWA
still maintain the porous structure. This explains that when the paper
sludge amount was greater than 20%, the water absorption and bulk
density were hardly affected by the calcination temperature.
Fig. 7. SEM images of fine LWA with different amounts of paper sludge at 1050 ◦ C (I: interior and E: surface).
6
Cement and Concrete Composites 134 (2022) 104773
Fig. 9 shows the SEM images of expanded shale from Yichang Baozhu
ceramsite Development Co., Ltd. It can be seen that the pore structure of
expanded shale is different from that of LWA. The pore size varies
greatly, and the large pore size can reach 100 μm. Three types of pores in
the expanded shale can be distinguished: (i) small isolated pores, (ii)
bigger connected pores, which are formed by merging small pores, and
(iii) the walls of larger pores are perforated by smaller pores, i.e., so-
called ink-bottle cavities.
XRD patterns and quantitative XRD results are plotted in Fig. 10 and
Fig. 11. As seen, the addition of paper sludge resulted in the formation of
anorthite and an intermediate phase (gehlenite). This is because free
CaO from the decomposition of carbonates can react with metakaolinite
(formed by the dehydroxylation of kaolinite) to produce anorthite [36,
37], or react with mullite and cristobalite generated after the decom­
position of metakaolinite to form anorthite [38]. XRD quantitative an­
alyses by Rietveld refinement were carried out to allow the detection of
mineralogical changes. A substantial increase in anorthite and gehlenite
and a decrease in the amorphous phase with the increase of paper sludge
content were observed. It is reported that the phase composition mostly
consisting of anorthite-mullite-corundum contributes to the improve­
ment of strength [39,40]. Sglavo et al. [41] also considered that a large
amount of silicate glass and calcium silicate, especially anorthite,
improve the strength of clay-based ceramics.
4.2. Time-dependent water absorption of fine LWA after crushing
Water absorption of LWA has an important effect on the internal
curing of concrete. The change in water absorption rate of fine LWA was
measured for 24 h in our experiments. As shown in Fig. 12, the time-
dependent water absorption of fine LWA showed two stages: rapid
stage and slowly increasing stage. The rapid stage lasted for about 1 h for
two kinds of fine LWA, but 8 h for the expanded shale [8]. After 1 h, the
amount of water absorbed was up to 95.1% and 96.4% of that at 24 h for
L. Yang et al. Cement and Concrete Composites 134 (2022) 104773

Fig. 8. SEM images of fine LWA with different amounts of paper sludge at 1150 ◦ C (I: interior and E: surface).

Fig. 9. SEM images of expanded shale.

S10 and S30, while expanded shale absorbed only 47.7% water of that at
24 h. Similarly, in the absorption results shown in the study of Kim et al.
[42], the absorption of expanded shale continuously increased as the
soaking time increased; the absorption values were 7%, 10%, and 25%
at 1, 3, and 14 d, respectively. This implies that the soaking time of LWA
made in this study could be shortened greatly. 1 h is enough for water
absorption of LWA in our experiment. The water absorption of LWA is
related to its pore structure. This proves once again that the pore
structure of LWA is different from that of expanded shale. Its pore
structure is due to the voids left after the release of gas from the raw
material. Therefore, the pore size is relatively small and the water ab­
sorption speed is faster.
4.3. Desorption isotherm of fine LWA after crushing
The desorption isotherm provides some important information about
the amount of internal curing water provided by LWA at different
relative humidity [28]. Some studies have reported that the internal
curing efficiency of LWA is affected by the water release rate [43,44]. As
shown in Fig. 13, the LWA had already lost almost all absorbed water at
the RH of 97%. S10 and S30 had desorbed about 94.8% and 96.1% of the
total amount of absorbed water, respectively. It seems to show that their
desorption ratios have little difference, but the water amount desorbed
has a great difference which will affect autogenous shrinkage and hy­
dration of mortars. The LWA could be used as an efficient internal curing
material for high-strength mortars due to the high water absorption and
timely water desorption.

7
L. Yang et al.
Fig. 10. XRD patterns of different types of LWA (C = Corundum; M = Mullite;
H = Hematite; Q = Quartz; A = Anorthite; G = Gehlenite; R = Rutile).
Fig. 11. Qualitative XRD results of different types of LWA.
4.4. Early-aged hydration
The influence of LWA on early hydration is especially important in
terms of setting time and strength development. In general, an increase
in the w/b ratio will result in a delay of the main hydration heat peak
[45]. An appropriate LWA for internal curing should have a good water
retention capacity. It means that this LWA can effectively store the in­
ternal curing water without loss in the mixing process so that the initial
w/b ratio does not change.
The rate of hydration heat during 72 h is shown in Fig. 14. S10 and
S30 did not result in the delay of the main hydration heat peak. The end
of the induction period is thought to be the beginning of the initial
setting. This indicates that LWA did not release water before the initial
set and almost had no effect on the porosity of the paste. After the end of
the induction period, LWA increased the heat release rate due to the
release of water absorbed.
The total hydration heat was also increased with the addition of
LWA, but slightly lower than the REF- 0.358 (Fig. 15). Although the heat
of hydration of the mortars with LWA was close to the REF- 0.3 before 6
h, the hydration then went faster and approached that of the REF- 0.358.
This indicates that the absorbed water took part in the hydration. After
8
Cement and Concrete Composites 134 (2022) 104773
Fig. 12. Time-dependent water absorption of fine LWA.
Fig. 13. Water desorption of fine LWA.
24 h, the hydration heat of M-S10 began to be lower than that of REF-
0.358. After 48 h, the hydration heat of M-S30 also was lower than
that of REF-0.358. This indicates that some water was still retained in
the pores of LWA. This water will be released at the lower internal RH of
the mortar. In addition, M-S30 released a higher amount of hydration
heat than M-S10. This indicates that S30 can release more internal
curing water at an early age.
4.5. Autogenous shrinkage of mortars
Autogenous shrinkage of mortars with and without fine LWA has
presented in Fig. 16. Autogenous shrinkage of mortars decreased as the
w/b ratio increased. This decrease, however, will increase the porosity
[46] and the effectiveness is also lower than that of LWA. Compared to
the reference REF-0.3, the two kinds of LWA reduced autogenous
shrinkage of mortars by 80.1% for M-S10, and 88% for M-S30, respec­
tively. S30 showed more positive effects than S10 as more internal
curing water was released. Generally, when the same amount of internal
curing water is carried by a higher volume of LWA (S10), it will be more
evenly distributed through the matrix, and the effectiveness of internal
curing is thus improved [47]. However, this is contrary to the
L. Yang et al.
Fig. 14. Rate of Hydration heat of the binder in mortars.
Fig. 15. Cumulative heat of hydration of the binder in mortars.
experimental results. This might be due to the difference in the pore
structure. S30 has more and larger pores which can release more water
to make up for the water consumed in the capillary pores at the same
change in relative humidity. Therefore, the autogenous shrinkage of
mortars with S30 was lower. Zou et al. [7] also found that LWA with
high water absorption had similar results.
4.6. Pore structure of mortars
Usually, the strength of mortars is closely related to their porosity.
The higher the compressive strength, the lower porosity would be found
[48]. Fig. 17 (a) gives the total porosity of the mortars obtained from 1H
NMR measurement. The mortars with LWA had reduced total porosity
than the reference mortars, and this effect was more evident in the
M-S30. This indicates that the porosity introduced by LWA can be
compensated by a higher degree of hydration. Fig. 17 (b) shows the pore
size distributions of the mortars. Pores larger than 100 nm were found in
the M-S10 and M-S30 due to the porous structure of LWA (Fig. 18). The
pores in LWA tested by NMR also show that there are still some inter­
communicating pores between the paste and LWA. Or else water cannot
enter the pore of LWA in the vacuum saturation and these pores will not
9
Cement and Concrete Composites 134 (2022) 104773
Fig. 16. Autogenous shrinkage of reference mortars and mortars with LWA.
The results were zeroed at the final set of the reference paste.
be found. But pores of this size were less found in the M-S30. Besides, the
volume of mesopores (<50 nm) inside the M-S10 and M-S30 increased.
This was also caused by the increased degree of hydration since these
pores are mainly existing among hydration products [9].
4.7. Compressive strength of mortars
The effect of LWA on the strength of mortars mainly depends on the
strength of LWA itself and the contribution of internal curing to the
hydration. The negative effects of LWA on the strength of concrete are
usually observed at earlier testing ages (<7d), and the same result was
obtained in the mortars (Fig. 18). After 7d, compared with REF-0.3, the
partial replacement of river sand with LWA did not lead to a significant
reduction in strength, while the strength of REF-0.358 was greatly
reduced. The 3-d strength of M-S30 was much lower than that of REF-0.3
but only slightly lower than that of REF-0.358 and M-S10. At 7d, the
strength values of M-S10 and M-S30 were comparable to that of REF-0.3.
At 28d, the strength of M-S10 and M-S30 was slightly higher than that of
REF-0.3. The lower strength of mortars than that of reference samples at
3d can be explained by the fact that the LWA used was not only saturated
surface dry but had a wet surface. This can lead to the formation of a
weak interfacial transition zone between the LWA and the cement paste
[3]. As the internal curing was ongoing in the later time, the promoted
hydration of cement and silica fume overwhelmed the initial disad­
vantages of the water desorption of LWA. Therefore, the compressive
strength of mortars containing LWA was higher than that of reference
samples at 7 d and 28 d. Similar findings can be obtained by other re­
searchers [7,49,50]. Besides, it can be seen that the strength of M-S30
was also slightly higher than that of M-S10. This is because fewer par­
ticles of LWA were used to provide the same content of internal curing
water in the mortars when they are more porous or absorptive. There­
fore, the reduction in the weak component of mortars mitigated the loss
of strength. But there is optimum water absorption. Too high water
absorption of LWA will result in an obvious strength loss of concrete due
to large pores and high porosity [4,7].
5. Discussion
Increasing the w/b ratio of mortars can delay the formation of empty
pores and the occurrence of air-water menisci [51]. This method can
mitigate the autogenous shrinkage of mortars, and also reduce the
strength of mortars. Although the capillary pressure increases rapidly in
the mortars with a lower w/b ratio, a relatively compact solid skeleton
L. Yang et al. Cement and Concrete Composites 134 (2022) 104773

Fig. 17. (a) Porosity and (b) pore size distribution of mortars at 28 d.

low w/b ratio, the pore size is mostly between 10 and 50 nm [53]. Even
at 12 h, the pores of 10–100 nm account for a large proportion [11].
According to the capillary tension theory, the fluid always transfers from
the large pores to the small pores. 100 nm of pore size is thus thought to
be a critical value for internal curing [12,54,55]. Fig. 19 shows the pore
size distributions of LWA tested by MIP. The pore size of S10 and S30 is
greater than 100 nm, and a large number of pores are located at
200–2000 nm. Therefore, when the relative humidity changes slightly,
the S10 and S30 can release a large amount of water, which could reduce
the autogenous shrinkage of mortars remarkably.
Unlike the rapid water loss from LWA at high RH, only 15.71%–
31.50% of the water was removed from the recycled fine aggregates
(RFA) when the RH was >94% RH [56]. The lower desorption of RFA
than that of LWA can be explained by its pore distribution, as shown in
Fig. 20 (b). In addition to some pores larger than 10000 nm, most of the
pores are smaller than 100 nm. As a result, the absorbed water may not
be released completely from those pores even if the RH is close to the
theoretical value. Consequently, RFA may be less useful than LWA for
internal water curing. This is also found in the natural zeolite [12], as
shown in Fig. 21. Lightweight expanded clay aggregate (LECA) had
interconnected pores in the size range of 100–5000 nm, which confirms
Fig. 18. Compressive strength of mortars at different ages.
the excellent desorption characteristics of LECA. However, a visible in­
crease of pore volume for sizes below 100 nm can be obtained in the
network is formed. This will improve the stiffness of the matrix and thus natural zeolite. This characteristic results in the fact that most of the
limit the development of autogenous shrinkage to some extent. At the
same time, the water released by the LWA keeps a high internal RH in
the mortars, which reduces the capillary stresses and shrinkage and also
promotes hydration. The porosity of the paste matrix can be reduced due
to the generation of more hydration products, which explains the
enhanced strength of mortars. Therefore, incorporating LWA with an
appropriate pore structure is more effective in improving the properties
of mortars than directly increasing the dosage of mixing water.
According to Castro et al. [28], LWA as an efficient internal curing
material must be porous to hold water in the pores, and also able to
release the water into paste at a high RH. Only when the pores of LWA
are larger than those of paste, the water absorbed can be released. The
amount of water released by LWA depends on the amount of pore larger
than the critical pore size at a certain internal RH [44] and the saturation
degree of the pore being consumed by the hydration. To make the
capillary porosity of the hydrating cement paste remain saturated, LWA
should have a suitable range of pore sizes. At the same time, the pore size
cannot be too large, otherwise, the water would migrate out too early to
increase the w/b ratio of the paste matrix.
In mature cement pastes, pore size does not exceed 1000 nm, and
most of the pores are below 100 nm [52]. While in cement pastes with a
Fig. 19. Pore size distributions of different types of LWA.

10
L. Yang et al.
Fig. 20. (a) Desorption isotherm and (b) pore size distributions of RFA with different water absorption capacities. The figures are adapted from Ref. [51].
Fig. 21. (a) Desorption isotherm and (b) cumulative pore volume of LECA and zeolite aggregate. The figures are adapted from Ref. [12].
absorbed water is still retained in the zeolite even at 80% RH. Compared
to the reference mixtures, shrinkage in specimens containing zeolite
aggregates not only did not decrease but even increased.
Based on the experimental results in our study, the pore structure and
performance of LWA can be successfully designed to meet the practical
requirements of internal curing through the composition of raw mate­
rials and calcinating conditions. The open and interconnected pores of
200–2000 nm not only make the LWA has high absorption, but a good
water retention capacity and controllable water release capacity. The
internal curing of LWA with high water absorption improved the per­
formance of high-strength mortars and overcame the disadvantages
associated with its high autogenous shrinkage. This means that at a
certain range of pore size, LWA with high water absorption can improve
the effectiveness of internal curing. This is because, LWA with high
water absorption has a coarser pore structure, which reduces the driving
force required for water movement in the same environment. For the
mortars at high RH, a weak driving force can draw out more water from
the larger pores of LWA into the smaller pores of nearby paste. Rodrí­
guez-Álvaro et al. [57] also thought that an effective LWA should have a
high absorption capacity and a high desorption capacity at high internal
RH. Specific types of porous aggregates for use in internal curing should
be selected based on these characteristics.
Although the function of internal curing is to reduce the autogenous
11
Cement and Concrete Composites 134 (2022) 104773
shrinkage of concrete with a low w/b ratio and to prevent its early-age
cracking, the introduction of highly porous LWA into the dense matrix
evidently should alter the durability-related properties of concrete. On
the one hand, the use of LWA in internal curing improved the degree of
hydration and refined the pore structure, which can improve the
permeability and prevent the expected increase due to the use of high-
porosity aggregates. On the other hand, the introduction of LWA
might lead to an increase in the volume of pores in the concrete. In terms
of the pores of LWA, the big pores in LWA, especially larger than 1000
nm pores, are quickly saturated but have very poor water retention
capacity [10]. If most of the internal curing water is released by LWA
before the initial setting, the effectiveness of internal curing will
decrease [11]. However, once the absorbed water has been drawn from
the pores of LWA, these pores then can function as entrained air space to
house water expansion, potentially improving freeze-thaw resistance
[58]. From the discussion above, the durability of concrete with LWA is
positively affected by the internal curing effect whereas negatively
influenced by the high porosity of the LWA itself. In other words, the
effect of LWA on the durability of concrete mainly depends on the
characteristics of LWA itself and the contribution of internal curing to
hydration. Certainly, the amount of collated findings is not enough to
state general, more studies should be carried out to investigate the effect
of the pore structure of LWA on the durability-related properties of
L. Yang et al.
concrete.
6. Conclusions
In this study, paper sludge was used as a pore-forming agent to
produce fine LWA from bauxite tailings. The effects of paper sludge
amount on the properties and microstructure of fine LWA were inves­
tigated, and the formation mechanism of fine LWA was analyzed. The
internal curing effects of two types of LWA in the high-strength mortars
were investigated to select the optimal LWA. The following conclusions
could be made:
(1) Different from the isolated and large pore structure of the
expanded shale, fine LWA has a concentrated and fine pore
structure of 200–2000 nm. Fine LWA can absorb about 30.6%
water by mass and quickly reaches saturation. At 97% relative
humidity, more than 95% of water absorbed can be released.
These characteristics make fine LWA can act as a suitable internal
curing material.
(2) The shrinkage reduction effect of fine LWA on the high-strength
mortars is related to its water absorption. Fine LWA with high
water absorption has a coarser pore structure, making the inter­
nal curing water more easily released. Compared to the mortars
with the same mixing water content, the autogenous shrinkage of
mortars can be reduced by up to 88%.
(3) Fine LWA has a good water retention capacity and thus does not
result in the delay of the main hydration heat peak. The capillary
pore size of 20–50 nm increases and the total porosity reduces
due to the increased degree of hydration. The enhanced hydra­
tion offsets the negative effect of fine LWA itself on the strength of
mortars. Thus, the strength of mortars increases, and this effect is
more obvious when using LWA with high water absorption.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
The data that has been used is confidential.
Acknowledgments
The authors gratefully acknowledge the financial support from the
Graduate Research and Innovation Projects of Hunan Province (grant
number 541109080261); the Science Foundation of Henan Province
(grant number 222300420399); and the National Natural Science
Foundation of China (grant number 52208237).
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