Case Studies in Construction Materials 17 (2022) e01374

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Case Studies in Construction Materials

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Durability of solidified sludge with composite rapid soil stabilizer

under wetting–drying cycles
Xichen Zhang a, Xiangwei Fang a, *, Jinlong Liu a, Mingming Wang a, Chunni Shen b,
Kaiquan Long a
a
School of Civil Engineering, Chongqing University, Chongqing 400045, China
b
School of Civil Engineering and Architecture, Chongqing University of Science and Technology, Chongqing 401331, China

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

Keywords: Composite rapid soil stabilizer (CRSS) comprising calcium sulfoaluminate cement, gypsum,
Sludge lithium carbonate, and ionic soil stabilizer is characterized by rapid hardening and high strength.
Composite rapid soil stabilizer In this study, it was used to solidify sludge rapidly, and how the number of wetting–drying (WD)
Wetting–drying cycles
cycles and the CRSS dosage influenced the durability of the solidified sludge was studied. The
Unconfined compressive strength
results show that for a given CRSS dosage but an increasing number of WD cycles, the dry mass
Evolution mechanism
and density of the solidified sludge decreased, the water content and pH of the soaking solution
increased, the unconfined compressive strength increased slightly, then decreased slowly, finally
stabilized. The ettringite in the solidified sludge was transformed from columnar to needle-like.
the diffraction peak intensity decreased, and the microscopic pores increased in both size and
quantity. With increasing CRSS dosage, the apparent structure was more intact, the strength
attenuation was smaller. After 12 WD cycles, with a 20% content of solidified sludge, the dry mass
loss was only 2%, the strength loss was only 12%, and the cumulative pore volume did not in­
crease obviously, which was maintained at about 0.20 ml/g, showing the high resistance to WD
erosion. Based on the chemical reaction and combined with the macroscopic and microscopic test
results, the microscopic evolution mechanism of the durability of solidified sludge under WD
cycles—especially the strength evolution mechanism—is revealed clearly. The solidified sludge
with CRSS had good durability against WD cycles, thereby laying a theoretical foundation for
applications of CRSS.

1. Introduction

With the rapid development of projects such as port, river, and lake dredging and land reclamation, large amounts of sludge have
been generated that must be cleaned up urgently [1–3]. According to statistics, the total amount of sludge produced at all commercial
ports in Tunisia reaches 8 M m3 per year [4], the sludge produced by dredging operations in France reaches 45 M m3 per year [5],
China produces more than 7 M m3 of sludge in the Taihu Lake basin per year [6], and there are also considerable amounts of sludge in
other regions [7]. However, because sludge has high water content, high void ratio, high compressibility, low bearing capacity, and
low permeability, it is difficult to use it directly in practical engineering, and therefore the resource utilization of sludge has long been a
topic of much concern.

* Corresponding author.
E-mail address: fangxiangwei1975@163.com (X. Fang).

https://doi.org/10.1016/j.cscm.2022.e01374
Received 2 June 2022; Received in revised form 17 July 2022; Accepted 2 August 2022
Available online 3 August 2022
2214-5095/© 2022 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
X. Zhang et al. Case Studies in Construction Materials 17 (2022) e01374

There are many ways of using sludge as a resource. In civil construction, after modification or solidification, it can be used for
reclamation, backfill soil, and building materials. In particular, the chemical reinforcement method of adding solidifying materials is
used widely and has led to many achievements. The main solidified materials are inorganic cementitious materials such as cement,
lime, and fly ash. Tang et al. [8–12] proposed using the chemical reaction among cement, lime, and soil particles to improve the
properties of soft soil and help to reinforce it. Wareham et al. [13] developed a composite soil stabilizer comprising Portland cement,
lime, cement kiln dust, amorphous silica, and diatomite that is effective for solidifying contaminated port sludge. Asavapisit et al. [14]
considered the alkali activator effect of sodium silicate and sodium carbonate, and they found that in solidifying electroplating sludge,
the early-strength effect of lime–fly-ash stabilizer under alkali activator was significantly better than that of ordinary lime–fly-ash
stabilizer. Ma et al. [15] found that mixing MgO and MgCl2 at a ratio of 3:1 into cemented soil improved the strength of the latter in a
short time. In recent years, in order to reduce the impact of soil additives on the environment, copper slag-based geopolymers,
non-woven geotextiles, lignosulfonates, coal wastes, kenaf fibers, copper sludge, etc. have been gradually applied to soil improvement
[16–22]. Regarding the mechanical properties of solidified sludge in engineering, the main research focus is the relationship between
cement content and the mechanical properties of the solidified soil. Through isotropic compression tests, Chiu et al. [23,24] showed
that the yield stress of solidified sludge was positively correlated with the cement content and curing age. Xu et al. [25] studied the
effect of cement on the mechanical properties of sludge via consolidated–drained triaxial tests, and they found that with increasing
cement content, both the cohesion and internal friction angle of the solidified sludge increased. Ding et al. [26] studied the micro­
structure of solidified sludge via mercury intrusion porosimetry (MIP), and they showed that with increasing content of solidified
material and age, both the pore volume and D50 pore size of the solidified sludge decreased significantly. Regarding the durability of
solidified sludge, the main research focus is the influence of complex environments such as wetting–drying (WD) cycles on the so­
lidified soil. Kamei et al. [27] proposed the joint reinforcement of soft clay with waste gypsum and fly ash; they found that (i) the
durability of the solidified soil was correlated positively with the content of waste gypsum and fly ash but (ii) using fly ash alone had a
negative effect on soil strength. Horpibulsuk et al. [28] discussed the durability of alkaline-activator–fly-ash solidified sludge, and they
established a logarithmic relationship between the strength of the solidified sludge and the number of WD cycles. Helson et al. [29]
studied the laws governing how the mass, wave velocity, permeability, and mechanical properties of solidified soil change under WD
cycles, and they reasoned that the evolution of ettringite crystals during the WD cycles was the main reason affecting the strength of the
solidified soil.
Mostly based on lime, fly ash, Portland cement, etc., the aforementioned sludge solidification materials meet the needs of general
engineering in terms of solidification effect; however, their solidification cycle is long and their early strength is not high, and so it is
difficult to use them in emergency situations that require rapid solidification of sludge, such as rescues, disaster relief, and emergency
road repairs. Instead, the authors’ research group has developed a composite rapid soil stabilizer (CRSS) [30] that is characterized by
rapid hardening and high strength; however, its durability in complex environments such as WD cycles is yet to be studied. Previous
research has shown that WD cycles have an important impact on the durability of solidified sludge [28]. Therefore, it is of great
significance to study the durability of solidified sludge with CRSS under WD cycles.
In the study reported herein, the aforementioned CRSS was used to solidify sludge rapidly, and durability tests of the solidified
sludge with differing CRSS content were performed under WD cycles. X-ray diffraction (XRD), scanning electron microscopy (SEM),
and mercury intrusion porosimetry (MIP) tests were performed on representative samples with different numbers of WD cycles and
different CRSS dosages to (i) study how those variables influenced the durability of the solidified sludge and (ii) explore the strength
evolution mechanism, thereby offering theoretical support for engineering applications of CRSS.

2. Materials and methods

2.1. Materials

The sludge used in the tests was taken from the construction site of Changle Station of Fuping Railway in Shouzhan Town, Changle
District, Fuzhou City, Fujian Province, China. Its main physical properties are given in Table 1, its grain size distribution curve is shown
in Fig. 1, and its main chemical components are given in Table 2.
The soil stabilizer used in the tests was the aforementioned CRSS, whose main components are 42.5 calcium sulfoaluminate cement
(CSA), an early-strength component (lithium carbonate, Li2CO3), an expansion component (gypsum, CaSO4.2 H2O), and thinning
electric-double-layer components [ionic soil stabilizer (ISS)]. CRSS has remarkable early-strength properties, and the strength of
sludge solidified with CRSS can be as much as six times that of sludge solidified with composite early-strength Portland cement after
curing for 1 d [30].

Table 1
Main physical properties of sludge.
Liquid limit (%) Plastic limit (%) Plasticity index Maximum dry density (g/cm3) Specific gravity

42.8 23.6 19.2 1.55 2.625

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Fig. 1. Grain size distribution curve of sludge.

Table 2
Main chemical components of sludge.
compound Mass fraction (%) error element Mass fraction (%) error

SiO2 59.72 0.25 Si 27.92 0.11

Al2O3 24.9 0.22 Al 13.18 0.11
Fe2O3 5.75 0.12 Fe 4.02 0.08
K2 O 3.83 0.1 K 3.18 0.08
MgO 1.59 0.06 Mg 0.959 0.04
S 1.59 0.06 S 1.59 0.06
TiO2 0.902 0.045 Ti 0.541 0.027
CaO 0.658 0.033 Ca 0.47 0.023

2.2. Sample preparation and process of WD cycles

Before the tests, the sludge retrieved from the site was dried in an oven at 65 ◦ C to a constant weight, crushed, and then passed
through a 200-mesh sieve for use. The initial moisture content of the sludge was 50%, and the dry density was controlled to be 1.5 g/
cm3. The required CRSS, sludge, and water were weighed and mixed well, and cylindrical samples with dimensions of
⌀50 mm × 50 mm were made by means of static pressing in two layers. To prevent the sample layers from separating, after the first
layer was compacted, its surface was polished in a timely manner. Because of the rapid hydration reaction of CRSS, sample preparation
had to be completed within ten minutes of adding the water and mixing. Each sample was then placed in a standard curing room at
20 ◦ C and a relative humidity of 90% for 3 d before being taken out for 1 WD-cycle test. The main reason for setting the curing age to 3d
was that the strength of the solidified sludge with CRSS after curing for 3d had reached 87% of the strength of curing for 28d.
The WD-cycles process was improved and optimized based on previous research [31–34]. Each sample was placed in a
constant-temperature blast-drying oven at 60 ◦ C (it was ensured that the temperature did not affect hydration products such as
ettringite [35]) for 48 h, taken out and cooled at room temperature for 1 h, placed in deionized water at 20 ◦ C for 23 h (it was ensured
that (i) the water level did not exceed the sample height by more than 20 mm and (ii) the volume of the soaking solution for each
sample exceeded 200 ml), and then taken out to complete 1 WD cycle.

2.3. Test schemes

To study the durability characteristics and evolution mechanism of the solidified sludge with differing CRSS content under WD

Table3
Test scheme.
Sample number CRSS dosage (%) Curing age (d) Number of w-d cycles Test content

GS-0 0 3 1、2、3 appearance、mass

GS-5 5 5、7、9、12 moisture content
GS-10 10 dry density
GS-15 15 pH of soaking solution
GS-20 20 UCS
XRD、SEM、MIP

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cycles, the CRSS dosage was taken as 0%, 5%, 10%, 15%, and 20%, and the maximum number of WD cycles was set to 12 (if a sample
with a given dosage was damaged prematurely after a certain number of WD cycles, then the test of that sample was terminated). The
samples were tested after 1, 2, 3, 5, 7, 9, and 12 WD cycles for appearance, mass, moisture content, dry density, pH of soaking solution,
unconfined compressive strength (UCS)and by XRD, SEM, and MIP. The test scheme is given in Table 3.

2.4. Test methods

2.4.1. Appearance, mass, size, and moisture content

The appearance was described using high-definition camera observation. The mass was measured using an electronic balance with
an accuracy of 0.01 g. The size was measured using a Deli high-precision electronic digital vernier caliper with an accuracy of
0.01 mm. The moisture content was measured using the drying method (i.e., each sample was dried to a constant weight in an oven at
65 ◦ C, and the moisture content was calculated from the mass before and after drying).

2.4.2. pH of soaking solution

The pH of soaking solution was measured using a SevenCompact S220 desktop multi-parameter tester with a resolution of 0.01 and
an instrument level of 0.001, and the waterproof and dustproof capability could reach IP54 level.

2.4.3. UCS
The UCS was measured using a YZM-IIC multifunctional pavement-material strength testing machine under a loading speed of
1 mm/min. Fig. 2 shows the machine equipped with pressure sensor (a resolution of 0.01 kN), displacement sensor (a resolution of
0.01 mm), control and data acquisition terminals.

2.4.4. XRD, SEM, and MIP

The XRD tests were performed using a multifunctional high-resolution X-ray diffractometer equipped with high temperature stage,
micro sample stage, five-axis sample stage, rotating transmission sample stage, high resolution module and 65536 sub-detectors, for
which the scanning angle was 10◦ − 60◦ and the sample particle size was less than 0.075 mm. The SEM tests were performed using a
Thermo Fisher Quattro S environmental scanning electron microscope with an accelerating voltage of 200 V-30 kV, a variable vacuum
of 10–4000 Pa, for which the sample area was less than 1 cm2. The MIP tests were carried out using a PoreMaster-33 automatic
mercury intrusion porosimeter with one high pressure sample analysis station, two low pressure sample analysis stations and a pore
distribution measuring range of 950–0.0064 µm, for which the sample volume was less than 1 cm3.

3. Results and discussion

3.1. Appearance, mass, moisture content, and dry density

Drying shrinkage and water swelling caused uneven deformation inside the soil, which had a great impact on the appearance of a
sample. Fig. 3 shows the appearance changes of the samples during the WD cycles, where here and elsewhere 0 cycles represents the
state before the WD cycles. As can be seen in Fig. 3, GS-0 samples (unsolidified sludge) failed when they encountered water, and the
samples were damaged as a whole, showing a muddy shape and poor water stability. Because the internal force between the non-
stabilized soil particles is the van der Waals force, which is weaker than the expansion pressure exerted in the pores of the soil par­
ticles, resulting in complete failure of the sample [19]. GS-5 samples had a certain ability to resist WD cycles: after 5 WD cycles, they
appeared to have pores and were accompanied by skin peeling, and their structures were damaged. When the CRSS content exceeded

Fig. 2. YZM-IIC multifunctional pavement-material strength testing machine.

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Fig. 3. The appearance changes of the samples during the WD cycles.

5%, the resistance of the samples to WD cycles was significantly improved: after 12 WD cycles, the structure remained intact, and the
soundness (i.e., the apparent integrity of a sample after WD cycles) was significantly higher than that for 5%. In particular, GS-15 and
GS-20 samples were smooth in appearance with only microcracks and no skin peeling, while GS-10 samples changed from smooth to
rough with a few wide cracks, which is consistent with the conclusion of Helson et al. [29] that the crack width increases with
decreasing cement content. In summary, with increasing CRSS content, the effect of the WD cycles on the appearance of the samples
diminished; when the CRSS content exceeded 10%, after 12 WD cycles the appearance of the samples remained smooth and their
soundness was good.
During the WD cycles, the dry and wet mass of the samples changed continuously because of the influence of soaking and drying on
the solidified sludge. To reflect the law governing how the sample mass changed, we define the mass change rate Wn as
mn − mo
Wn = × 100% (1)
mo

where mn is the dry (wet) mass of a sample during each WD cycle, and mo is the dry (wet) mass of the sample before the WD cycles.
Fig. 4 shows the mass change rate of the samples during the WD cycles; because GS-0 samples were destroyed after 1 WD cycle, they
are not represented. As can be seen, the mass of GS-5 samples decreased sharply after 5 WD cycles, the cumulative dry mass loss
exceeded 4.5%, the cumulative wet mass loss exceeded 2%, and the samples disintegrated and failed. The dry mass of the samples with
CRSS dosages exceeding 5% also decreased to varying degrees: the lower the dosage, the more obvious the decreasing trend. After 12
WD cycles, the dry mass loss exceeded 2%, the main reason being that the “slag drop” phenomenon appeared during the drying
process, which caused the dry mass to decrease. However, the wet mass did not decrease significantly, and the mass change rate
remained close to 0% after 12 WD cycles. This indicated that after a sample was immersed in water, the pores in the sample expanded
slightly, inducing the increment of the water absorption and the water content, which offset the loss of dry mass. Also, previous studies
have also confirmed this finding [34]. On the whole, with increasing CRSS content, the mass loss of the solidified sludge after the WD
cycles decreased gradually, and the samples with higher CRSS content showed better mass stability.
Fig. 5 shows the moisture content of the samples during the WD cycles. As can be seen, with increasing number of WD cycles, the
moisture content of a sample with a given dosage increased gradually. the main reason was that the drying shrinkage and water
swelling caused many microcracks inside the samples [36] and the WD cycles aggravated the development of these microcracks, and
their width and number continued to increase, resulting in an increase in the moisture content of the samples, which also explains why
the wet mass was not reduced significantly during the WD cycles. Also, Fig. 5 shows that with decreasing CRSS content, the moisture

Fig. 4. The mass change rate of the samples during the WD cycles: (a) dry mass (b) wet mass.

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Fig. 5. The moisture content of the samples during the WD cycles.

content of the samples increased gradually, the main reasons being that (i) the low-dosage samples contained few hydration products,
(ii) the bonding area between soil particles and the hydration products was small, (iii) the bonding force was weak, (iii) the number
and width of cracks produced were larger, and (iv) the pore filling was seriously insufficient, and so the water content of the samples
was enhanced.
The dry density of a sample was closely related to its mass, volume, and moisture content. Fig. 6 shows the dry density of the
samples during the WD cycles. As can be seen, with increasing number of WD cycles, the dry density of the samples with various
dosages showed a downward trend, the main reasons being that the volume of a sample expanded rapidly after immersion in water, the
internal pores increased in both size and quantity, the density decreased, the moisture content increased (Fig. 5), and the dry mass
decreased continuously [Fig. 4(a)], resulting in a decrease in dry density. Because the accumulated dry mass loss of GS-5 samples was
relatively large in the early stage, its decreasing trend is obvious. However, the dry density of GS-15 and GS-20 samples changed slowly
in the later stage, with a gentle trend and better stability.

3.2. pH of soaking solution

During the WD cycles, a sample underwent moisture migration and skin peeling. And the solidified sludge with CRSS was alkaline,
so the above phenomenon would promote the increase of the pH of the soaking solution. By studying the pH of the soaking solution,
how it was influenced by the WD cycles was analyzed. Fig. 7 shows the pH of the soaking solution during the WD cycles. The pH of
laboratory deionized water was 7.1, i.e., weakly alkaline; the pH of the sludge was 6.86, i.e., weakly acidic. Fig. 7 shows that the
soaking solution of the samples was alkaline as a whole, and the alkalinity increased with increasing content CRSS, the main reason
being that the early-strength component lithium carbonate (Li2CO3) in CRSS was hydrolyzed to generate lithium hydroxide (Li(OH)),
which provided an alkaline environment conducive to the hydration reaction. Sample soaking was a slow process from surface to

Fig. 6. The dry density of the samples during the WD cycles.

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Fig. 7. The pH of the soaking solution during the WD cycles.

interior. With increasing number of WD cycles, the cracks in a sample continued to develop, and the soaking liquid gradually pene­
trated into the core of the sample. Also, the alkalinity at the core was higher, resulting in a difference in OH− concentration, and OH−
flowed out along the concentration gradient, resulting in an increase in the pH of the soaking solution. In the later stage of the WD
cycles, a fixed moisture migration path formed inside a sample, the difference between the inner and outer OH− concentrations was
small, and the pH of the soaking solution increased slowly and tended to stabilize.

3.3. UCS

The WD cycles increased the moisture content of the samples and decreased their dry density, which may have attenuated their
strength. Fig. 8 shows the UCS of the samples during the WD cycles. As can be seen, as the number of WD cycles increased, the overall
UCS of the samples first increased slightly, then decreased slowly, and finally tended to stabilize, which is consistent with the research
results of Xu et al. [6]. In particular, GS-5 samples disintegrated after 5 WD cycles, while GS-20 samples maintained an average wet
strength of more than 8 MPa after 12 WD cycles, and the strength loss was only 12%, showing high resistance to WD erosion. Although
the structure of samples with CRSS dosages exceeding 5% remained intact, different degrees of strength reduction were observed in
UCS tests after 12 WD cycles, which may also be related to microstructural damage that will be discussed in the following sections [16].
To characterize the stability of the strength of the solidified sludge after WD cycles, the WD stability coefficient Rs is introduced as
qb,n
Rs = (2)
qe

where qb,n is the average wet strength of the samples after the WD cycles, and qe is their average strength before the WD cycles.

Fig. 8. The UCS of the samples during the WD cycles: (a) dry strength (b) wet strength.

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Fig. 9 shows the WD stability coefficient Rs of the samples after 12 WD cycles. As can be seen, the regression line was presented, and
the goodness of fit R2 reached 0.996, indicating that there was an obvious linear relationship between the WD stability coefficient Rs
and the dosage. This is because the closer the R2 to 1, the lesser the dispersion [20]. The WD stability coefficient Rs increased with
increasing CRSS content. It was only 0.224 for a CRSS content of 5%, while increasing to 0.877 for a CRSS content of 20% (a growth
rate of 291.5%), indicating that CRSS was effective for improving the strength and stability of the solidified sludge.

3.4. XRD, SEM, and MIP

To study the effect of the WD cycles on the microstructure of the solidified sludge, GS-10 and GS-20 samples were taken as ex­
amples, and representative samples with different WD cycles were taken for microscopic testing. Fig. 10 shows the XRD patterns of the
samples during the WD cycles, and Fig. 11 shows the corresponding microstructure. As can be seen, before and after the WD cycles,
there were obvious diffraction peaks of calcium silicate hydrate (C-S-H) and ettringite (Aft) in the interior of the samples in addition to
quartz. Also, the higher the CRSS content, the greater the intensity of the diffraction peaks and the better the compactness of the
samples, indicating that the main hydration products of CRSS are ettringite and calcium silicate hydrate [37]; they were wrapped
around the soil particles and were effective at filling the pores in the sludge. The intensity of the ettringite diffraction peak in the
samples reached its peak after 3 WD cycles, when the porosity of the samples was small and their integrity was high; however, after 12
WD cycles, the ettringite diffraction peak intensity decreased significantly, the pores increased in both size and quantity (as shown by
the circle in Fig. 11), and the compactness worsened, which is similar to the UCS change law (Fig. 8), indicating that ettringite was one
of the main products affecting the strength of the solidified sludge. The microscopic changes of ettringite (as shown by the box in
Fig. 11) show that before 3 WD cycles, the ettringite in the samples was columnar, with small bifurcations, neatly arranged, densely
distributed, and wrapped on the surfaces of the particles, which increased the contact area between the soil aggregates and was
effective to improve the strength of the solidified sludge [38]. After 12 WD cycles, the ettringite exhibited needle-like bifurcations, its
arrangement was disordered, its distribution density decreased, its structure was destroyed, and the intensity of its diffraction peaks
decreased, which is consistent with the XRD results.
Fig. 12 shows the cumulative pore volume (CPV) distribution of the samples during the WD cycles. As can be seen, before the WD
cycles, the CPV of the samples decreased with increasing CRSS content, and the CPV of GS-10 samples was 1.2 times that of GS-20
samples. After 12 WD cycles, the CPV of GS-10 samples increased significantly, whereas that of GS-20 samples did not change
significantly and remained at about 0.20 ml/g. At this time, the CPV of GS-10 samples was 1.4 times that of GS-20 samples, which was
greatly improved compared with that before the WD cycles.
To better observe the change of pore size, the pores were classified with reference to relevant research results [39,40] as large pores
(pore size greater than 1 µm), medium pores (pore size between 0.1 µm and 1 µm), or small pores (pore size less than or equal to
0.1 µm). Fig. 13 shows the pore type distribution of the samples during the WD cycles. As can be seen, before the WD cycles, the pore
distribution of GS-10 and GS-20 samples was dominated by medium and small pores, accounting for more than 80%. With increasing
CRSS content, the proportion of small pores increased, that of medium pores decreased, and that of large pores did not change
significantly. After 12 WD cycles, the pore distribution of both samples showed a trend of increasing the proportion of medium pores
and decreasing that of small pores, indicating that the WD cycles promoted the development of pores in the samples, especially the
transformation from small pores to medium pores, which is consistent with the microscopic change law of the samples (Fig. 11). In
general, GS-20 samples exhibited less porosity change, high structural integrity, and good durability against WD cycles after 12 of
them.

3.5. Evolution mechanism of durability under WD cycles

Solidified sludge is a complex multiphase dispersion system. After CRSS was added to the sludge, the calcium sulfoaluminate
cement (CSA) was hydrated rapidly to produce calcium silicate hydrate (CaO⋅2SiO2.3 H2O), calcium hydroxide (Ca(OH)2), and
ettringite (CaO⋅3Al2O3⋅CaSO4.32 H2O); gypsum (CaSO4.2 H2O) provided a large amount of calcium ions (Ca2+) to promote the for­
mation of hydration products such as ettringite; the lithium ions (Li+) in lithium carbonate (Li2CO3) were hydrolyzed to generate
lithium hydroxide (Li(OH)), which maintained an alkaline environment suitable for the hydration reaction so that it could proceed
rapidly and continuously; the ionic soil stabilizer (ISS) reduced the thickness of the bound water film on the surface of the sludge soil
particles, improved the overall compactness, reduced the gaps between soil particles, and was effective in increasing the strength of the
solidified sludge. The main reaction equations are shown below [41]:
3Ca(OH)2 · 3Al2 O3 · CaSO4 + 2(CaSO4 · 2H2 O) + 34H2 O
(3)
→ 3CaO · Al2 O3 · 3CaSO4 · 32H2 O + 2(Al2 O3 · 3H2 O)

(2CaO · SiO2 ) + 4H2 O → CaO · 2SiO2 · 3H2 O + Ca(OH)2

(4)

3Ca(OH)2 + 3CaSO4 · 2H2 O + Al2 O3 · 3H2 O + 20H2 O → 3CaO · Al2 O3 · 3CaSO4 · 32H2 O (5)

Fig. 14 shows the microscopic evolution mechanism of the durability of solidified sludge under WD cycles. As can be seen, several
hydration products played different roles. In particular, calcium silicate hydrate (C-S-H) was mainly responsible for the cementation
between soil particles, ettringite (Aft) was responsible for the skeleton links and filling between soil aggregates, and calcium hydroxide

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Fig. 9. The WD stability coefficient Rs of the samples after 12 WD cycles.

Fig. 10. The XRD patterns of the samples during the WD cycles: (a) GS-10 (b) GS-20.

(Ca(OH)2) was sufficient for promoting the hydration of calcium sulfoaluminate cement (CSA). The three worked together to form a
stable chain or network structure between the soil aggregates, which significantly enhanced the strength and integrity of the sludge
[37].
In the early stage of the WD cycles, a small amount of calcium sulfoaluminate cement in the samples did not react completely during
the curing process. After immersion in water, the hydration reaction continued, and some new hydration products were generated,
which enhanced the skeleton links between adjacent soil aggregates. The intensity of the ettringite diffraction peaks and UCS of the
samples both increased (Figs. 8 and 10), while the UCS of the samples increased slightly (Fig. 8). However, because the solidified
sludge was characterized by water swelling and drying shrinkage, its volume changed during the WD cycles, causing irregular
deformation inside the soil. When it exceeded the limiting deformation range of the internal structure, stress became concentrated in
the weak structure between soil aggregates, which developed into microcracks [42]. As the WD cycles continued, the ettringite evolved
gradually from columnar to needle-like, and the distribution density decreased (Fig. 11). The linking effect of the skeleton was
weakened, and the microcracks developed rapidly. As a result, their opening degree expanded, and the water absorption increased
(Fig. 5) until they developed into large cracks, which damaged the original stable structure and caused the strength of the solidified
sludge to decrease (Fig. 8). However, when a crack developed to a certain extent, it was transformed into a type of “expansion joint”
(Fig. 14), which gave new deformation space to the internal structure of the soil to resist the impact of uneven deformation of drying
shrinkage and water swelling [36], forming a special negative feedback adjustment mechanism to ensure that the strength of the
solidified sludge tended to be stable in the later period of the WD cycles (Fig. 8).

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Fig. 11. The microstructure of the samples during the WD cycles: (a) GS-10 (b) GS-20.

Fig. 12. The CPV distribution of the samples during the WD cycles: (a) GS-10 (b) GS-20.

4. Conclusions

In this study, CRSS was used to solidify sludge rapidly, the laws governing how the physical and mechanical properties of the
solidified sludge changed under the action of WD cycles were studied, and the evolution mechanism of durability under WD cycles was
analyzed. The following main conclusions are drawn.
With increasing number of WD cycles, the dry mass and density of the solidified sludge decreased, while the moisture content and
pH of the soaking solution increased. In particular, the solidified sludge with a CRSS dosage of more than 10% had a dense appearance,
complete structure, and strong resistance to WD erosion after 12 WD cycles.
With increasing number of WD cycles, the UCS of the solidified sludge first increased slightly, then decreased slowly and tended to
stabilize. The larger the CRSS dosage, the smaller the final strength attenuation, indicating that CRSS is effective for improving the
strength and stability of solidified sludge.
The microscopic analysis showed that the WD cycles had a great influence on the ettringite and microscopic pores in the solidified
sludge. After 12 WD cycles, the ettringite was transformed from columnar to needle-like, the distribution density decreased, the
diffraction peak intensity decreased, and the microscopic pores increased in both size and quantity. With increasing CRSS dosage, the
CPV of the solidified sludge increased less obviously after the WD cycles, and the sample integrity was better.

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X. Zhang et al. Case Studies in Construction Materials 17 (2022) e01374

Fig. 13. The pore type distribution of the samples during the WD cycles.

Fig. 14. The microscopic evolution mechanism of the durability of solidified sludge under WD cycles.

The chemical reaction and the macroscopic and microscopic test results show clearly the microscopic evolution mechanism of the
durability of solidified sludge under WD cycles, especially the strength evolution mechanism.
The research results show that solidified sludge with CRSS had good durability against WD cycles. However, it may suffer from
other harsh environments such as freeze-thaw cycles [18], sulfate attack [43], etc. Therefore, considering more environmental factors
will provide a more favorable theoretical foundation for the application of CRSS.

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 authors do not have permission to share data.

Acknowledgements

This work was financially supported by Science and Technology Innovation Project [grant numbers 20-163-13-ZT-007-060-01].

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