Construction and Building Materials 250 (2020) 118933

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Construction and Building Materials

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

Strength properties and associated mechanisms of magnesium

oxychloride cement-solidified urban river sludge
Dongxing Wang a,⇑, Shengjie Di b,c, Xiangyun Gao a, Ruihong Wang d, Zhengguang Chen a
a
Key Laboratory of Geotechnical and Structural Engineering Safety of Hubei Province, School of Civil Engineering, Wuhan University, 8 Dong Hu South Road, Wuhan 430072, China
b
China Hydropower Consulting Group, Northwest Institute of Survey and Design, Shanxi Xi’an 710065, China
c
Dacheng Kechuang Foundation Construction Co. Ltd., Unit 2, SOHO Global NO.297, Huaihai Road, Jianghan District, Wuhan 430090, China
d
Key Laboratory of Geological Hazards on Three Gorges Reservoir Area, Ministry of Education, China Three Gorges University, Yichang, Hubei 443002, China

h i g h l i g h t s

 Eco-friendly magnesium oxychloride cement is innovatively used to stabilize sludge.

 Magnesium oxychloride cement is proved effective in improving strength of sludge.
 Strength is affected by molar ratio of MgO/MgCl2, MOC content and curing period.
 MOC hydration process controls microstructure and strength of solidified sludge.
 Phase 5 and brucite are identified as micromechanisms for MOC solidified sludge.

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

Article history: Eco-friendly magnesium oxychloride cement (MOC) is incorporated to reduce the disposal obstacles and
Received 26 January 2020 mitigate the environmental impacts related to the urban river sludge. Three major factors including MOC
Received in revised form 22 March 2020 content, molar ratio of MgO/MgCl2 and curing time are examined by unconfined compressive strength
Accepted 27 March 2020
(UCS) tests. The microscopic effect caused by the MOC-hydration process is identified using X-ray diffrac-
Available online 3 April 2020
tion (XRD), mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM) technique to
reveal the intrinsic mechanisms. The results show that MOC content, molar ratio of MgO/MgCl2 and cur-
Keywords:
ing time strongly affects the UCS of MOC-solidified sludge. The suitable parameter values for sludge treat-
Urban river sludge
Magnesium oxychloride cement
ment by MOC turn out to be molar ratio of MgO/MgCl2 of 8–10, MOC content of 10% and curing time of 60
Compressive strength d. The UCS and strength retention coefficient of MOC-solidified sludge present an important decreasing
Pore structure trend with water immersion time due to the gradual decomposition of phase 5 – 5 Mg(OH)2
MgCl2
8H2O
Micromechanism into Mg(OH)2 phase, some soluble ions and H2O molecules. The UCS development is directly related to
the formation of phase 5 and brucite, which induces a transformation of pore structure and boosts to
develop a much stronger interlocking microstructure in solidified matrix. The identification of brucite
with a significant volumetric expansion and phase 5 provides an insightful interpretation for the strength
evolution of MOC-solidified sludge. Overall, the innovative incorporation of MOC treatment is supposed
to be an efficient and sustainable approach on sludge solidification.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction ated with high initial water content and toxic substances, the ille-
gal dumping and discharge of urban river sludge is a very great
With the rapid development of industrialization and urbaniza- trouble and should be strictly prohibited. Therefore, it is essential
tion, large amounts of urban river sludge have been annually gen- to establish a suitable and proper approach for waste sludge treat-
erated, and their safe disposal poses a great challenge to lots of ment and resource reuse in practical engineering works. Over
cities in China. Due to the serious environmental concerns associ- recent years, solidification/stabilization is known as an efficient
and cost-competitive technique to solve sludge disposal problems
⇑ Corresponding author. by incorporating cementitious additives. Various binders, such as
E-mail addresses: dongxing-wang@whu.edu.cn (D. Wang), dishj@nwh.cn (S. Di),
Portland cement, lime, silica fume, fly ash, blast furnace slag, steel
xiangyun-gao@whu.edu.cn (X. Gao), wrh@ctgu.edu.cn (R. Wang), zhengguang- slag, cement kiln dust, reactive MgO and Ca/Mg carbonates, have
chen@whu.edu.cn (Z. Chen).

https://doi.org/10.1016/j.conbuildmat.2020.118933
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 D. Wang et al. / Construction and Building Materials 250 (2020) 118933

been commonly implemented in solidification/stabilization [1–25]. China and listed as a key renovation project to improve water qual-
It can be seen that much more attentions have been paid to the ity. This project produced approximately 11,700 m3 of sludge,
application of Ca-bearing additives in soil improvement. Therefore, which should initially be conditioned and subjected to mechanical
the situation of Mg-bearing alternatives is urgently needed to gain dewatering process for safe and economic disposal. The sampling
further insight for developing novel eco-friendly binders. location and processing of sludge is shown in Fig. 1. It was black
Currently, reactive MgO-based alternatives to Portland cement in colour for raw sludge due to the presence of organic matter
have been attracted enormous attentions in solidification/stabi- and became brown for dewatered sludge. The characterization of
lization owning to the low carbon and sustainable advantages dewatered sludge is reported in Table 1. The initial water content
[24,26–33]. Especially, magnesium oxychloride cement (MOC), is 22.1%, measured by oven drying method at 40 °C. The specific
which has many superior properties including weak alkalinity, gravity is 2.66, determined by the density bottle method. The pH
excellent early strength, good abrasion and fire resistance, remark- is around 6.8, which indicates a weak acidity owning to the pres-
able bonding ability and good thermal insulation, is gradually ence of organic matter. The digital soil liquid-plastic limit pen-
becoming a new research hotspot in the construction materials etrometer permits to identify liquid limit, plastic limit and
field [34–47]. The above advantages permit MOC to be applied in plasticity index as 59.2%, 32.0% and 27.2%. Based on the modified
several construction sectors encompassing constructional beam, Proctor compaction tests, the optimum water content and maxi-
compound floor tile, MOC concrete and biomaterials [36,47–49]. mum dry density are respectively 23.5% and 1.5 g/cm3. The relative
In fact, the two major hydration products, including 5 Mg(OH)2- fractions of sand, silt and clay particle size are respectively 17.9%,

MgCl2
8H2O (phase 5) and 3 Mg(OH)2
MgCl2
8H2O (phase 3), are 59.6% and 22.5% through the graded sieving method. According
the main sources of strength and influenced by some factors such to the Unified Soil Classification System, the experimental data
as molar ratio of MgO/MgCl2, H2O/MgCl2 and curing temperature obtained permit to categorize the tested sludge into the group of
[35,38,44,46]. Different additives, including fly ash [37], granite silty sand. It should be noted that the detailed chemical composi-
waste [39], FeSO4 and KH2PO4 [40], silica glass [41], incinerated tions of dredged sludge comprise mainly quartz, illite and kaolin-
sewage sludge ash [42] and glass powder and pulverized fuel ash ite. Some heavy metals cumulated in river sludge contain Cr, Ni,
[45] were frequently chosen to improve the resistance of MOC Cu, Hg, As, Pb, Zn, Cd and so on, and the concentrations of three
pastes to water invasion. However, so far, very few studies have heavy metals (i.e. Ni, Cd and Pb) exceeds the requirement of rele-
focused on the application of MOC in solidification/stabilization, vant specifications.
except for Li et al. [48], Ma et al. [50] and Wang et al. [51], and a For magnesium oxychloride cement, the two starting materials
clear view on the application of MOC on sludge treatment is still responsible for hydration and hardening process are magnesium
lacking. chloride hexahydrate (MgCl2
6H2O) and magnesium oxide (MgO).
To address the shortcoming of current research, the main objec- Their chemical components are shown in Tables 2 and 3. The mag-
tive of this study is to evaluate comprehensively the feasibility of nesium oxide used in this investigation is purchased from a mag-
magnesium oxychloride cement in stabilizing urban river sludge. nesium company in Shandong Province, China. It is actually
A thorough parametric study of MOC is performed to investigate calcined magnesite with purity higher than 97% and has an iodine
the effect of molar ratio of MgO/MgCl2, MOC content and curing time absorption value of 110 (an index reflecting the activity of reactive
on the strength properties of sludge. The examinations by X-ray MgO). For the magnesium oxide, the specific surface area is
diffraction (XRD), scanning electron microscopy (SEM) and mercury 253 m2/kg and the average particle size is 1.14 lm. The MgCl2
6H2-
intrusion porosimetry (MIP) tests are conducted to identify hydra- O with purity greater than 98% taken from a chemical company in
tion products, pore structure and micrograph morphology and Tianjin city, China appears as colourless needle-like or columnar
reveal the associated micromechanisms of MOC-solidified sludge. crystals and is highly soluble in water.
The obtained findings provide a basic framework for developing an
appropriate and eco-friendly solidification/stabilization technology
2.2. Testing methods
for the disposal of urban river sludge with MOC.
The experimental process to probe into MOC solidified sludge is
2. Experimental programs illustrated in Fig. 2, which includes specimen preparation, strength
definition and microstructure characterization. The dewatered
2.1. Materials sludge was oven-dried at a low temperature of 40 °C and ground
into powder by an automatic grinding machine. After that, MgCl2-
The urban river sludge used was dredged from Shuwuzhigou
6H2O was dissolved in certain amount of distilled water and stir-
open channel, which is located at the northwest of Wuhan city, red for 5 min to prepare a ready-to-use solution, which was poured

Fig. 1. Location of sampling site and processing of sludge.

 D. Wang et al. / Construction and Building Materials 250 (2020) 118933 3

Table 1
Main physical indexes of urban river sludge.

Initial water Specific Liquid limit Plastic limit Plasticity Maximum dry density Optimum water Sand Silt Clay pH
content (%) gravity (%) (%) Index (%) (g/cm3) content (%) (%) (%) (%)
22.1 2.66 59.2 32.0 27.2 1.5 23.5 17.9 59.6 22.5 6.8

Table 2 The durability of MOC-solidified sludge was evaluated by water

Chemical components of magnesium oxide.
soaking tests based on 28-day samples cured in standard condi-
Components MgO CaO Fe3+ Others tion, and the compressive strength was recorded after 28 days of
Values in % 97 0.25 0.01 2.73 standard curing and after different days (2, 4, 6, 8, 12 and 16 d)
of water immersion. The mineralogical compositions were identi-
fied by X-ray diffraction (XRD) technique on the oven-dried sludge
ground by mortar pastel and passed through 200-mesh sieve. The
into MgO-sludge blend and mixed by a mechanical mixer at the XRD tests were conducted by the PANalytical X’ Pert Pro X-ray
speed of 800 r/min for 5 min in order to obtain a homogeneous diffractometer with Cu Kɑ radiation source, step length of 0.02°
mixture. The components of MOC were reactive MgO and MgCl2 and scanning range of 2h = 10–80°. The scanning electron micro-
in different molar ratios ranging from 6 to 10, with mass ratios scopy (SEM) tests were performed on a FEI Quanta 200 machine
of MOC to dry sludge of 5%, 10%, 15% and 20%. The MOC-sludge to capture the cross-section morphology of block specimens, which
materials were filled into patches of cylindrical steel molds with were sputter-coated by a thin layer of gold on their fresh surface to
a size of 50 mm in both diameter and height, and compacted by avoid the potential charge effect. The mercury intrusion porosime-
the static compaction method defined by the Chinese standard try (MIP) tests were carried out to characterize quantitatively the
SL237-1999. Afterwards, the demolded samples were hermetically pore structure of solidified sludge on a PoreMaster 33 porosimeter,
sealed by plastic films and cured in standard condition of with pore size measurement range of 0.005–1080 mm and maximal
20 °C ± 2 °C and relative humidity > 95% for 3, 7, 14, 28, 60, 90 intrusion pressure of 228 MPa.
and 180 d. It should be noted that the abbreviation of ‘‘xPyMzd”
represents the sludge sample solidified with x% of MOC at molar
3. Results and discussion
ratio of MgO/MgCl2 of y:1 and curing time of z days.
The unconfined compressive strength (UCS) was tested by using
3.1. Strength characteristics
a WDW-20 universal testing machine with a maximal loading of
5 kN at a vertical displacement rate of 1 mm/min. Three samples
The variation of compressive strength of MOC-solidified sludge
were prepared for each mix series to calculate the average value.
with MOC content, molar ratio of MgO/MgCl2 and curing time is

Table 3
Chemical components of magnesium chloride hexahydrate.

MgCl2
6H2O (%) Insoluble matters (%) Sulfate (%) Total nitrogen (%) Ca2+ (%) Heavy metals (%)
98.0 0.005 0.005 0.005 0.05 0.0005

MgO + H2O

Sludge powder
MgCl2 UCS tests

MIP SEM XRD

Fig. 2. Illustration of testing process.
4 D. Wang et al. / Construction and Building Materials 250 (2020) 118933

4.0 4.0 4.0

0% 5% 10% 15% 20% 0% 5% 10% 15% 20% 0% 5% 10% 15% 20%
3.5 3.5 3.5

3.0 3.0 3.0

UCS (MPa)

UCS (MPa)
UCS (MPa)
2.5 2.5 2.5

2.0 2.0 2.0

1.5 1.5 1.5

1.0 1.0 1.0

0.5 0.5 0.5

3 7 14 28 60 90 180 360 3 7 14 28 60 90 180 360 3 7 14 28 60 90 180 360
Curing time (d) Curing time (d) Curing time (d)

(a) MgO/MgCl2 = 6 (b) MgO/MgCl2 = 7 (c) MgO/MgCl2 = 8

4.0 4.0
0% 5% 10% 15% 20% 0% 5% 10% 15% 20%
3.5 3.5

3.0 3.0
UCS (MPa)

UCS (MPa)
2.5 2.5

2.0 2.0

1.5 1.5

1.0 1.0

0.5 0.5
3 7 14 28 60 90 180 360 3 7 14 28 60 90 180 360
Curing time (d) Curing time (d)

(d) MgO/MgCl2 = 9 (e) MgO/MgCl2 = 10

Fig. 3. UCS of MOC-solidified sludge with curing time at different molar ratios of MgO/MgCl2.

presented in Figs. 3 and 4, which contain the UCS of raw sludge. As ples, hindering to a certain extent the ascending trend of UCS with
the curing time increases, the UCS of raw sludge changes slightly curing time. This is actually the main reason why the phenomenon
within a limited interval of 0.8–0.9 MPa, which is obviously lower of strength retraction emerges for MOC-solidified sludge at 90 d
than that of MOC-solidified sludge (>1.35 MPa). It means that MOC and 180 d.
is proved effective to significantly enhance the strength perfor- Fig. 4 represents the variation of UCS of MOC-solidified sludge
mance of sludge. with MOC content and molar ratio of MgO/MgCl2 at certain fixed
Fig. 3 shows the change in UCS of MOC-solidified sludge at dif- curing age varying from 3 d to 360 d. The obtained result shows
ferent MOC contents and molar ratios of MgO/MgCl2. At each molar that UCS tends to increase with rising MOC content from 5% to
ratio of MgO/MgCl2 from 6 to 10, the UCS at all MOC contents var- 20% and molar ratio of MgO/MgCl2 from 6 to 10, although several
ies consistently, i.e. it increases with curing time and reaches the singularity data unexpectedly appear. The MOC content around
peak at 60 d, followed by an important decrease at 90 d and 180 10%, which has high efficacy to enhance UCS, can be considered
d. Especially, the UCS at 360 d tends to remain constant or slightly as the appropriate value to improve the performance of MOC-
increased, which indicates that the compressive strength would solidified sludge. The improvement in UCS with MOC content is
not continue to decrease at the long-term curing time and the slow tightly correlated with incremental concentrations of Mg2+, Cl
hydration reaction might occur in the presence of unreacted com- and OH– in pore fluids, which are beneficial to the production of
ponents. The early-age UCS at 3 d can even reach more than 50% of brucite and phase 5. For 14-day samples with molar ratio of
peak strength at 60 d owning to the high early strength property of MgO/MgCl2 of 10, UCS has an upward trend from 1.85 MPa to
MOC. In contrast, the late-age curing (i.e. 90 d, 180 d) has a nega- 2.68 MPa, when the MOC content grows from 5% to 20%. For
tive impact on the strength development of MOC-solidified sludge, 360-day samples with MgO/MgCl2 molar ratio of 6, UCS tends to
which is independent of MOC content and molar ratio of MgO/ grow from 1.61 MPa to 2.42 MPa owing to the increasing MOC con-
MgCl2. Take sample 20P7M for example, the UCS values are tent from 5% to 20%. However, a different trend can be observed in
1.84 MPa, 2.01 MPa, 2.21 MPa, 2.43 MPa, 3.01 MPa, 2.97 MPa certain cases such as 180-day samples with molar ratio of MgO/
and 2.47 MPa respectively at 3 d, 7 d, 14 d, 28 d, 60 d, 90 d and MgCl2 of 10. It means that curing time might largely affect the evo-
180 d, and the maximal UCS occurs at 60 d. lution of UCS with MOC content, for a given molar ratio of MgO/
As the curing time is extended from 3 d to 60 d, more cementi- MgCl2.
tious products including phase 5 and brucite are generated, which Compared to MOC content, the molar ratio of MgO/MgCl2 exerts
leads to significant strength improvement. However, the concen- a similar influence on UCS of MOC-solidified sludge, i.e. UCS has an
tration of MgCl2 tends to become insufficient for the formation of overall increasing tendency with molar ratio of MgO/MgCl2, even
phase 5 due to the gradual depletion of MgCl2, especially at higher though some irregular data emerge. For molar ratios of MgO/MgCl2
molar ratio of MgO/MgCl2, increasing the probability of continua- of 6, 7, 8, 9 and 10, the UCS values of 180-day samples with 10%
tion of brucite formation. Nevertheless, the formation of excessive MOC are respectively 1.90 MPa, 2.29 MPa, 2.51 MPa, 2.72 MPa
quantity of brucite would result in the volume expansion and and 2.90 MPa, while the strengths of 360-day samples with 20%
cause potentially the appearance of more microcracks within sam- MOC are correspondingly 2.41 MPa, 2.51 MPa, 2.69 MPa,
 D. Wang et al. / Construction and Building Materials 250 (2020) 118933 5

4.0 4.0 4.0

n=6 n=7 n=8 n=9 n=10 n=6 n=7 n=8 n=9 n=10 n=6 n=7 n=8 n=9 n=10
3.5 3.5 3.5

3.0 3.0 3.0

2.5 2.5 2.5

UCS (MPa)

UCS (MPa)
UCS (MPa)

2.0 2.0 2.0

1.5 1.5 1.5

1.0 1.0 1.0

0.5 0.5 0.5

0.0 0.0 0.0

5 10 15 20 5 10 15 20 5 10 15 20
MOC content (%) MOC content (%) MOC content (%)

(a) 3 d (b) 7 d (c) 14 d

4.0 4.0 4.0
n=6 n=7 n=8 n=9 n=10 n=6 n=7 n=8 n=9 n=10 n=6 n=7 n=8 n=9 n=10
3.5 3.5 3.5

3.0 3.0 3.0

2.5 2.5 2.5

UCS (MPa)
UCS (MPa)
UCS (MPa)

2.0 2.0 2.0

1.5 1.5 1.5

1.0 1.0 1.0

0.5 0.5 0.5

0.0 0.0 0.0

5 10 15 20 5 10 15 20 5 10 15 20
MOC content (%) MOC content (%) MOC content (%)

(d) 28 d (e) 60 d (f) 90 d

4.0 4.0
n=6 n=7 n=8 n=9 n=10 n=6 n=7 n=8 n=9 n=10
3.5 3.5

3.0 3.0

2.5 2.5
UCS (MPa)

UCS (MPa)

2.0 2.0

1.5 1.5

1.0 1.0

0.5 0.5

0.0 0.0
5 10 15 20 5 10 15 20
MOC content (%) MOC content (%)

(g) 180 d (h) 360 d

Fig. 4. UCS of MOC-solidified sludge with MOC content and molar ratio of MgO/MgCl2.

2.93 MPa and 3.06 MPa. These data indicate that the strength evi- formed in this study: (i) to evaluate how the water resistance
dently increases with molar ratio of MgO/MgCl2. In contrast, some of MOC-solidified sludge behaves, and (ii) to prove that further
abnormal data occur such as 180-day samples with 5% MOC. Par- measures should be necessarily taken in the future research if
ticularly, UCS of MOC-solidified sludge reveals that the optimal the solidification method by MOC is employed. The results in
molar ratio of MgO/MgCl2 is proved to be 8–10, and excessively terms of compressive strength evolution with water immersion
low molar ratio of MgO/MgCl2 would be detrimental to the period are presented in Fig. 5, where the strength retention coef-
strength development due to the limited quantity of hydration ficient was identified by comparing UCS of MOC-solidified sam-
products. From the UCS results, the performance of MOC in solidi- ples (10P7M, 10P10M and 20P7M) before and after water
fying sludge strongly depends on the synergistic influence of MOC immersion for different ages. When immersed in water, UCS of
content, curing time and molar ratio of MgO/MgCl2. It is believed MOC-solidified sludge shows a decreasing trend with immersion
that MOC-solidified sludge has the optimal combination of MOC time up to 16 d, and similar phenomenon can be seen for the
content, curing time and molar ratio of MgO/MgCl2 from the view- strength retention coefficient RS. As a matter of fact, both UCS
point of strength gain and economical costs. and RS curves drop rapidly with immersion time from 0 to 6 d,
followed by a relatively gradual reduction once the immersion
3.2. Water resistance time exceeds 6 d. The strength of samples 10P7M, 10P10M and
20P7M decreases accordingly from 2.59 MPa to 1.48 MPa, from
The durability of MOC pastes in water, which limits potentially 2.75 MPa to 1.2 MPa and from 2.8 MPa to 1.95 MPa, respectively
their application in practical engineering, should be evaluated in corresponding to RS at 16 d of soaking time equal to 57.2%, 43.6%
sludge solidification. The water soaking tests deserve to be per- and 69.6%.
6 D. Wang et al. / Construction and Building Materials 250 (2020) 118933

the XRD and SEM results) into Mg(OH)2 phase and some soluble
1.0
ions and H2O molecules, which can be dissolved out of MOC-
3.0 solidified samples by water. The main phases are unstable, leading

Strength retention coefficient RS

0.8
Compressive strength (MPa)

to the poor water resistance of MOC-solidified samples, and this

0.6 has been reported in previous studies such as He et al. [42,45],
2.5
Tan et al. [49] and Wang et al. [51]. It is interesting to mention that
0.4 the formation of phase 5 depends on the concentration of Mg2+
2.0 ions in the pore solution of MOC pastes [42,52], revealing that
0.2 the hydration process is influenced by many factors related to
10P7M the concentration of Mg2+ ions such as MOC content, MgO/MgCl2
1.5 10P10M 0.0
20P7M
ratio and water quantity. Especially, the relationship of water
10P7M immersion until 16 d to the practical environment exposure does
10P10M -0.2
merit further research, which will be highlighted and performed
1.0 20P7M
in the future research.
-0.4
0 2 4 6 8 12 16
Water immersion time (d)
3.3. Phase identification
Fig. 5. Durability of MOC-solidified sludge in water.
The x-ray diffractograms of MOC-solidified sludge at various
MOC contents, molar ratios of MgO/MgCl2 and curing times are
The strength deterioration of MOC-solidified sludge in water is stacked in Fig. 6(a)–(c) to identify the mineral species. The XRD
tightly associated with the progressive decomposition of the main patterns represent different crystalline peaks for kaolinite, brucite,
hydration product 5 Mg(OH)2
MgCl2
8H2O (phase 5, according to quartz and illite and diffused reflections for amorphous phase 5,

1 1 1 - Quartz
1 - Quartz
2 - Brucite 2 - Brucite
3 - Illite 3 - Illite
4 - Kaolinite 4 - Kaolinite
5 - Phase 5 5 - Phase 5
1
4 1 1 1 1
5 53 3 1 4 2 3 1 1 1
4 1 5 4 5 2 21 5 5 2 51
Intensity
Intensity

20P7M90d 1
3 1 34 1 1 1 1
54 5 1 5 4 2 3 14 1 5 2 21 5 5 2 51 1
15P7M90d
10P10M90d

10P7M90d

10P7M90d
5P7M90d

10P6M90d
Sludge

10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
2Theta/° 2Theta/°
(a) MOC amount (b) Molar ratio of MgO/MgCl2

1
1 - Quartz
2 - Brucite
3 - Illite
4 - Kaolinite
5 - Phase 5
Intensity

1
4 1 1 1 1
5 53 3 5 4 2 3 14 1 1
4
1 1 5 2 2 5 5 2 51
1

10P7M90d

10P7M60d

10P7M28d

10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
2Theta/°
(c) Curing time
Fig. 6. X-ray diffraction patterns of MOC-solidified sludge.
 D. Wang et al. / Construction and Building Materials 250 (2020) 118933 7

while brucite and phase 5 are identified as the dominant reinforced 5. At a fixed curing time of 90 d and MOC content of 10%, the peak
compounds. No MgO peak can be detected, meaning that reactive intensity of phase 5 at 2h = 11.8° and 33.1° tends to rise with molar
MgO seems to be almost completely consumed in the formation ratio of MgO/MgCl2 from 6 to 10, indicating a higher amount of
of phase 5 and brucite. For the reason of high molar ratio of phase 5. However, the peak intensity of brucite shocks slightly
MgO/MgCl2 and dilution effect of MgCl2 in sludge, the gelling reac- within a narrow range, because the brucite exists in the form of
tion for phase 5 is incomplete and unreacted product of brucite is flake-like structure that remains relatively undeveloped in a high
still existed. This speculation can be further validated by the SEM alkaline environment (pH  9.7) (see SEM images). As shown in
analysis presented as follows. Fig. 6(c), the peak intensity of phase 5 at 2h = 11.8° and 18.6°
The XRD patterns of solidified sludge at various MOC contents and brucite at 2h = 38.1° and 60.8° is observed to increase with cur-
in Fig. 6(a) illustrate the peaks of brucite at 2h = 38.1°, 51.2°, ing time from 28 d to 90 d revealing that more cementitious prod-
54.1° and 60.8° and phase 5 at 2h = 11.8°, 18.6°, 33.1°, 49.2°, ucts are formed, although the peak intensity of brucite at 2h = 51.2°
57.5°, 58.8° and 63.6°. The intensity of peaks at 2h = 11.8°, 18.6° descends from 60 d to 90 d. The presence of more brucite and
and 58.8° enhances with the increase of MOC content, leading to phase 5 is the intrinsic mechanism for strength improvement,
the formation of more phase 5, which can fill in the interparticle but an excessive quantity of brucite could damage the overall
pores and cement fine particles together. The peaks of phase 5 structure of MOC-solidified sludge as a result of the volumetric
are relatively weak, showing a low degree of crystallinity, and this swelling. This is one of the main reasons why the strength retrac-
can be directly verified by SEM images. In contrary, the brucite tion occurs at the curing time greater than 60 d, besides the disso-
peak with high intensity at 2h = 38.1° demonstrates MgO hydration ciation of polymerized phase 5.
is the more favorable reaction at high molar ratio of MgO/MgCl2,
which is accordance with the previous study [49]. Note that the
3.4. Pore structure characterization
non-identified reflections on the XRD patterns should be deeply
probed into in the future for more precise and comprehensive
The cumulative pore volume and differential pore volume dis-
explanations.
tribution of MOC-solidified sludge by series of MIP tests are shown
In Fig. 6(b), an increase in molar ratio of MgO/MgCl2 for MOC-
in Figs. 7–9, whereas, the total pore volume, total porosity and
solidified sludge is prone to enhance the peak intensity of phase
average pore diameter are quantitatively listed in Table 4. It can

0.30
Sludge 10P7M28d
0.30
5P7M90d 10P7M60d
0.25 10P7M90d
10P7M90d
Cumulative volume (mL/g)

0.25
Cumulative volume (mL/g)

15P7M90d
20P7M90d 0.20
0.20

0.15
0.15

0.10
0.10

0.05 0.05

0.00 0.00
10-2 10-1 100 101 102 10-2 10-1 100 101 102
Pore diameter (µm) Pore diameter (µm)
(a) MOC content (b) Curing time

0.30
10P6M90d
10P7M90d
0.25 10P10M90d
Cumulative volume (mL/g)

0.20

0.15

0.10

0.05

0.00
10-2 10-1 100 101 102
Pore diameter (µm)

(c) Molar ratio of MgO/MgCl2

Fig. 7. Cumulative pore volume of MOC-solidified sludge.
8 D. Wang et al. / Construction and Building Materials 250 (2020) 118933

be seen that the pore structure of MOC-solidified sludge is greatly 0.1001 mm via. 0.1060 mm to 0.1048 mm. As a matter of fact, the
influenced by MOC content, molar ratio of MgO/MgCl2 and curing growth in phase 5 (pore-filling and cementation) and Mg(OH)2
time. (volumetric swelling and cementation) contributes together to
In Fig. 7(a), if the MOC content increases from 0 to 20%, the total the mechanical and microstructural behaviour of MOC-solidified
intruded pore volume of solidified sludge with molar ratio of MgO/ sludge.
MgCl2 of 7 at 90 d decreases from 0.2821 ml/g to 0.1948 ml/g Figs. 7 and 8 demonstrate respectively the pore size distribution
because of the generation of more hydrated phases, filling the curve and percent volume of pores in various size classes of MOC-
interparticle pores, which is in accordance with the variation of solidified sludge. The bimodal pore size distribution is typical for
total porosity. The curing time extended from 28 d to 60 d and solidified sludge with major peaks distributed in the pore size
90 d, as seen in Fig. 7(b), causes an increase in the total pore vol- range of 0.1–5 mm. According to Figs. 7(a) and 8(a), higher MOC
ume from 0.2046 ml/g (10P7M28d) to 0.2570 ml/g (10P7M60d) content induces an increase in the volume of pores larger than
and 0.2513 ml/g (10P7M90d). It can be explained by the continu- 10 mm and with size interval of 0.01–0.1 mm and a reduction in
ous formation of Mg(OH)2 as identified in XRD patterns, which the volume of 0.1–10 mm pores. It means a transformation of large
brings a volumetric expansion. However, the minimum average inter-particle (1–10 mm) and medium inter-particle (0.1–1 mm)
pore diameter of 0.0773 mm is reached at 60 d, and this agrees well pores to small inter-particle (0.01–0.1 mm) and inter-aggregate
with the evolution of UCS, i.e. reaching the maximum at 60 d. This (>10 mm) pores occurs. Especially, the evident increase in the vol-
is to say, besides the total porosity and pore volume, the average ume of small inter-particle pores up to 19.89–21.66% exhibits the
pore diameter can also be used to evaluate the pore structure char- pore-filling effect of hydrated phases such as phase 5.
acteristics of solidified sludge. In Figs. 7(b) and 8(b), the pore diameter greater than 10 mm and
Fig. 7(c) indicates that the total pore volume of 90-day sludge smaller than 0.1 mm shifts to be within a range of 0.1–10 mm with
solidified with 10% MOC rises from 0.2487 ml/g to 0.2688 ml/g, curing time varying from 28 d to 60 d, while the pore diameter of
since more reactive MgO are incorporated with molar ratio of 1–10 mm further shifts to be greater than 10 mm and in the range of
MgO/MgCl2 from 6 to 10. This is accompanied by the variation of 0.01–1 mm after 90-day curing. Therefore, the dominant cause for
total porosity from 13.57% via. 16.44% to 13.11%, which is in good growth in total pore volume is closely associated with the volume
agreement with the average pore diameter ranging from increase of large inter-particle and medium inter-particle pores for

0.21 0.14
Sludge 10P7M28d
0.18 5P7M90d 0.12 10P7M60d
10P7M90d
Log-differential volume (mL/g)
Log-differential volume (mL/g)

10P7M90d
15P7M90d
0.15 0.10
20P7M90d

0.12 0.08

0.09 0.06

0.06 0.04

0.03 0.02

0.00 0.00
10-2 10-1 100 101 102 10-2 10-1 100 101 102
Pore diameter (µm) Pore diameter (µm)
(a) MOC content (b) Curing time

0.14
10P6M90d
0.12 10P7M90d
10P10M90d
Log-differential volume (mL/g)

0.10

0.08

0.06

0.04

0.02

0.00
10-2 10-1 100 101 102
Pore diameter (µm)
(c) Molar ratio of MgO/MgCl2
Fig. 8. Pore size distribution of MOC-solidified sludge.
 D. Wang et al. / Construction and Building Materials 250 (2020) 118933 9

60 50
Sludge 10P7M28d
5P7M90d 10P7M60d
50 10P7M90d 10P7M90d
40
15P7M90d
20P7M90d

Pore in percentage
Pore in percentage

40
30

30

20
20

10
10

0 0
>10 1-10 0.1-1 0.01-0.1 <0.01 >10 1-10 0.1-1 0.01-0.1 <0.01
Pore diameter (μm) Pore diameter (μm)
(a) MOC content (b) Curing time
50
10P6M90d
10P7M90d
10P10M90d
40
Pore in percentage

30

20

10

0
>10 1-10 0.1-1 0.01-0.1 <0.01
Pore diameter (μm)
(c) Molar ratio of MgO/MgCl2
Fig. 9. Pore volume percentage of MIP results.

Table 4 trigger the volumetric swelling, but also produce more cementi-
Total pore volume, total porosity and average pore diameter. tious products such as phase 5 and brucite.
Materials Total pore volume Total porosity Average pore diameter
(ml/g) (%) (mm) 3.5. Microstructure
Sludge 0.2821 17.36 0.1414
10P6M90d 0.2487 13.57 0.1001 The representative MOC-solidified sludge specimens were cho-
5P7M90d 0.2728 19.59 0.1299 sen for SEM observation, and the typical morphology is presented
10P7M28d 0.2046 11.08 0.0956 in Fig. 10. The micrographs reveal that raw sludge in Fig. 10(a) and
10P7M60d 0.2570 16.51 0.0773
MOC-solidified sludge in Fig. 10(b)–(h) have the fabric with big
10P7M90d 0.2513 16.44 0.1060
15P7M90d 0.2106 12.63 0.0986 packets of particles/aggregates, and large pore spaces gradually
20P7M90d 0.1948 11.23 0.1159 vanish due to the interference of MOC. For 5P7M90d, the needle-
10P10M90d 0.2688 13.11 0.1048 like and columnar crystals are identified as phase 5 hydrates,
which facilitate to a certain extent the refinement of pore struc-
ture, although few large pores still exist in virtue of the limited
amount of hydrated products. As the MOC content goes up to
60-day curing samples and the volume increase of inter-aggregate, 10–20%, an evidently denser microstructure is formed in Fig. 10
small inter-particle and medium inter-particle pores for 90-day (c)–(h), and the majority of sludge aggregates are covered by
curing samples. As observed from Figs. 7(c) and 8(c), the volume hydrated phases including phase 5 and brucite. This without doubt
of pores with diameter between 0.1 mm and 10 mm decreases from contributes to the reduction of total porosity and the strength
71.42% to 59.1% for 90-day samples with molar ratio of MgO/MgCl2 improvement of solidified sludge. At higher MOC contents of 15%
from 6 to 10. Meanwhile, the volume of pores with diameter and 20%, a number of brucite crystals with ellipsoid shape, which
greater than 10 mm is raised from 9.03% to 21.58%, and this implies remain unreacted with MgCl2, are clearly detected over the surface
that the large inter-particle and medium inter-particle pores are of clustered aggregates in Fig. 10(g) and (h).
almost completely transformed to the inter-aggregate pores. With increasing molar ratio of MgO/MgCl2 up to 7 and 10, more
Hence, the incorporation of abundant reactive MgO can not only brucite products appear for 10P7M60d and 10P10M90d in Fig. 10
10 D. Wang et al. / Construction and Building Materials 250 (2020) 118933

Sludge 5P7M90d

Phase 5

Sludge aggregates
Phase 5

Phase 5

(a) Raw sludge (b) 5P7M90d

10P6M90d 10P7M28d

Brucite

Phase 5
MgO

Phase 5

Brucite

Crack

(c) 10P6M90d (d) 10P7M28d

10P7M60d 10P10M90d

Brucite

Brucite

Phase 5 Phase 5

Brucite
Phase 5
Phase 5

(e) 10P7M60d (f) 10P10M90d

15P7M90d 20P7M90d

Brucite
Cracks
Phase 5
Phase 5

Brucite Brucite

Phase 5

(g) 15P7M90d (h) 20P7M90d

Fig. 10. SEM images of MOC-solidified sludge.

(e) and (f), compared to 10P6M90d in Fig. 10(c) where the evident Besides abundant flake-like brucite, the polymerized gel-like phase
microcracks are generated. In other words, the formation of brucite 5 is found to be widely distributed in Fig. 10(e) and (f) in inter-
can not only densify the microstructure, but also produce some particle and inter-aggregate pore spaces, reducing the porosity
microcracks which prevent potentially the strength development. and binding the particles/aggregates to create an interconnected
 D. Wang et al. / Construction and Building Materials 250 (2020) 118933 11

structure. This interesting finding, which coincides well with the mal analysis, Writing - original draft. Xiangyun Gao: Formal anal-
XRD analysis, can provide a reasonable explanation for the ysis, Investigation, Visualization. Ruihong Wang: Writing - review
strength gain of MOC-solidified sludge. & editing. Zhengguang Chen: Writing - review & editing.
For 28-day curing specimen 10P7M28d in Fig. 10(d), it is
already difficult to find out the large pores throughout the solidi- Declaration of Competing Interest
fied matrix, and the surface of sludge particles/aggregates is cov-
ered with brucite and phase 5. Some unreacted MgO particles The authors declare that they have no known competing finan-
that have spherical shape disappear completely at a longer curing cial interests or personal relationships that could have appeared
period of 60 d for 10P7M60d. As illustrated in Fig. 10(e), the brucite to influence the work reported in this paper.
and phase 5 interlock with each other and bind sludge particles/ag-
gregates to form a dense network. It is worth mentioning that the Acknowledgement
continuation of brucite formation with curing time can be con-
firmed by specimens at 90 d in Fig. 10(f)–(h), and this is the dom- This work was supported by the National Natural Science Foun-
inant reason why the aforementioned strength degradation of dation of China (Grant no. 51879202, Grant no. 51979151), Science
MOC-solidified sludge occurs if the curing time is longer than 60 d. and Technology Program of Wuhan (Grant no.
2018060402011257) and Nature Science Foundation of Hubei Pro-
4. Conclusions vince (Grant no. 2018CFB453).

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