Wu 2021 Mater. Res. Express 8 095510
Wu 2021 Mater. Res. Express 8 095510
Wu 2021 Mater. Res. Express 8 095510
PAPER
Keywords: shale, sewage sludge, sustainable brick, compressive strength, thermal conductivity
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Any further distribution of This paper assessed the use of shale collected from western China and the incorporation of sewage
this work must maintain sludge for manufacturing fired shale bricks, which could reduce the environmental impact produced
attribution to the
author(s) and the title of in the mining process of traditional raw materials. Chemical constituents and mineral composition of
shale and sewage sludge were characterized by x-ray fluorescence spectrophotometer (XRF) and x-ray
the work, journal citation
and DOI.
diffractometer (XRD), the analysis indicated that only the shale was a fit bloating material, while the
sewage sludge could only be used as additive. Fired shale brick specimens containing 0%–30% (wt) of
sewage sludge were fired at temperatures ranging from 920 to 950 °C. The tests revealed that with the
increase of replacement ratio of sewage sludge, the water content and shrinkage rate increased,
whereas plasticity index, bulk density and compressive strength decreased. Comprehensively
considering the physical and mechanical properties of specimen, the optimum replacement ratio of
sewage sludge and sintering temperature were determined to be 15% (wt) and 940 °C, respectively.
Scanning electron microscope (SEM) analysis indicated that specimens with sewage sludge contained
higher amounts of micropores, which could improve the thermal insulation properties of the
specimen. Through the analysis of the experimental results, it could be concluded that the addition of
sewage sludge resulted in the successful manufacture of qualified fired shale bricks.
1. Introduction
In order to reduce the impact on the environment, one of the problems that must be solved in modern society is
how to improve resource efficiency. Along with the advancement of urbanization, a lot of resources are used to
manufacture building materials, and the building material industry presents enormous potential for the
sedimentary and low-grade metamorphic rocks (e.g., clays and tuffs) [1–4] and industrial waste (e.g., water
treatment sludge, municipal sludge and tannery sludge) [5–7]. These studies indicated that the industrial waste
could be used as a partial substitute of sedimentary and low-grade metamorphic rocks in the manufacture of
bricks.
Due to the good insulation performance and durability, fired clay brick is widely used as building materials
in the world. However, the exploitation of clay has an adverse effects on the environment, while the use of
industrial waste in the manufacture of building materials could reduce the consumption of natural resources
and the cost of waste treatment. Accordingly, it is interesting to use industrial waste and other materials instead
of clay in the manufacture of construction materials.
In China, wall materials account for about 70% of the whole building materials, and fired clay bricks play a
leading role in wall materials. The annual production of fired clay bricks is about 600 billion pieces in China,
which is equivalent to about 0.47 billion square meters of farmland is destroyed every year [8], so it is necessary
to choose a material instead of clay to manufacture fired bricks. The shale, created by dehydration and
cementation of clay, is gradually being applied in building materials and constructions, such as the use of shale in
concrete [9–14] and construction binder [15–17]. Shale is widely distributed in western China, such as Xinjiang
and Sichuan provinces, and is easy to exploit (shale is generally distributed on the ground surface), which helps
to reduce the cost of raw materials and protect the farmland. At the same time, the constituents of shale are
similar to those of clay, meaning that it is worthwhile to study how to manufacture fired bricks by using shale as
raw materials.
Sewage sludge, a liquid or semi-solid material, is the waste produced by sewage treatment plant. It could be
expected that the amount of sewage sludge increases with the expansion of city size. Currently, Sewage sludge in
China is generally either deposited or burned, no matter which treatment method is used, the negative impact on
the environment is predictable. The sewage sludge mainly consists of organic matter and inorganic composition.
The inorganic composition could be converted into an environmentally benign material by incorporating it into
a ceramic body. Jordán et al [18] investigated the effect of sewage sludge in the manufacturing of traditional
ceramics. The study showed that the bending strength decreased when the addition of sewage sludge increased.
Kizinievič et al [19] examined the effect of water treatment sludge (WTS) on the physical and mechanical
properties of ceramic products. When burned at 1000 °C and 1050 °C temperature, the parameters of 40% of
WTS additive into clay mixture was created: virtual (gross) dry density 1340–1565 kg m−3, compressive strength
14–25.9 N mm−2, effective porosity 31%–39%. Erkliğ et al [20] studied the effects of sewage sludge ash (SSA)
and fly ash (FA) and SiC ceramic particles with different particle content on tensile strength and flexural strength
of the polyester composites. The results revealed that the highest improvement of mechanical properties was
obtained with the addition of 5 wt% SSA, the tensile and flexural strength increased by 4.4% and 5.8%
respectively. Alsaadi et al [21] reported the effect of SSA waste particle on the resistance of glass fabric-reinforced
epoxy composites (GFRPs) against moisture and temperature of ultraviolet (UV) aging. Comparing to the aged
unfilled composite, the deterioration of interlaminar fracture toughness values of composites with SSA inclusion
of 10 wt% increased by 14.3%. The organic matter could generate micro micropores during the firing process.
Zhang et al [22] concluded that the compressive strength of brick decreased from 33.1 MPa to 20.5 MPa due to
the weight loss during sintering. Esmeray et al [23] presented that the heat loss rates of bricks increased as the
sewage sludge content increased, which was related to the decrease of compressive strength.
Although the literature survey presents that shale and sewage could be used separately in the manufacture of
fired bricks. However, to the best knowledge of the authors, the influence of sewage sludge content on the
physical and mechanical properties of fired shale bricks was not adequately investigated by researchers. In this
paper, the chemical, mineralogical and thermal properties of shale and sewage sludge were characterized by XRF
and XRD to investigate whether these two materials were fit bloating materials or not. The water content,
plasticity index, shrinkage rate, bulk density and compressive strength of green bricks or fired bricks with
contents of 0, 5, 10, 15, and 25% (wt) were tested to determine the optimum mixture proportions of raw
materials and the sintering temperature. Microscopic investigation was carried out to analyze the effect
mechanism of sewage sludge in ceramic body.
2.1. Materials
In this study, shale and sewage sludge (figure 1) were used to manufacture fired bricks. Shale was chosen as the
main raw material, while sewage sludge was used as a partial replacement of shale for producing micropores to
improve the self-weight and thermal insulation performance of fired shale bricks. The shale was obtained from
West Mountain area of Urumqi (Xinjiang, China), and was sieved until it reached a particle size 1 mm. Sewage
sludge was collected from Hongqiao Sewage Treatment Plant in Shuimogou District, Urumqi City (Xinjiang,
China). Considering that the sewage sludge was difficult to be completely dried and needed to be broken after
drying process, the sewage sludge was directly used to mix with shale after being compressed dehydration, which
would reduce the production cycle and production cost.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
The fluxing agent could help lower the material’s softening temperature [24]. Due to the fact that the
chemical composition of sewage sludge contained relatively greater amounts of CaO, MgO, K2O and Na2O,
which could be used as fluxing agent in the firing process, the addition of sewage sludge might be an effective
method to lower the softening temperature during the manufacture of fired shale bricks.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
As presented in the table, the specimens are identified as mS-nSS, where S and SS denote shale and sewage
sludge, respectively. In addition, m refers to the proportion of shale and n denotes the replacement ratio of
sewage sludge. For instance, 85S-15SS indicates that the replacement ratio of sewage sludge is 15%.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
100S 100 0
95S-5SS 95 5
90S-10SS 90 10
85S-15SS 85 15
80S-20SS 80 20
75S-25SS 75 25
70S-30SS 70 30
Samples Temperature range (°C) Heating rate (°C min−1) Soaking time (min)
Table 4. The sintering temperature of bricks with different replacement ratios of sewage sludge.
2.2.2. Sintering
In order to determine the sintering temperate of the fired shale brick using sewage sludge as additive accurately,
the optimum sintering temperature (OST) of shale should be investigated. The sintering temperature, heating
rate and soaking time of brick samples for the sintering tests are given in table 3.
The calorific value of sewage sludge was higher, which helped to reduce the sintering temperature of brick.
Therefore, the sintering temperature of specimen should be adjusted based on the replacement ratio of sewage
sludge, as given in table 4. The sintering process of fired shale brick with sewage sludge additive was still in
accordance with the requirements of table 3.
2.3. Methods
2.3.1. Water content and plasticity index test
It was experimentally proved that the effect of water content on the mixture properties should be considered
[25]. According to Chinese code GB/T 50123–2019 [26], liquid limit (LL ) and plastic limit (PL ) experiments
were carried out in this paper to study the influence of water content on mixtures of shale and sewage sludge
physically.
Put the sample into a bowl. A 76 g cone was gently placed on the surface of the mixture and sunk into the
mixture under the action of its self-weight. When the cone sunk into the mixture to a depth of 10 mm after 15 s,
the water content was determined to be the liquid limit value.
For plastic limit experiment, ball-shaped mixture was rolled to the shape of cylindrical pasta. If cracks
appeared when the diameter of cylinder was about 3 mm, the water content of the mixture was established as the
plastic limit value.
The plastic performance of the mixture was expressed by plasticity index (PI ), which was the difference of
the LL and PL, as given in equation (1):
PI = LL - PL (1)
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Mater. Res. Express 8 (2021) 095510 J Wu et al
The optimum sintering temperature of shale was determined firstly. Then in order to promote the industrialized
production of fired shale bricks using sewage sludge as additive, the water content, plasticity index and drying
shrinkage rate of green brick samples, the firing shrinkage rate, bulk density, compressive strength, and thermal
conductivity of fired brick samples were tested. Obvious defects, such as cracking and deformation, were
observed in the brick samples with 30% (wt) of sewage sludge. Therefore, the performance tests were mainly
carried out for brick samples whose replacement ratios of sewage sludge were lower than or equal to 25%.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
The water absorption (WA) and firing shrinkage (FS) of brick samples are given in figure 5. Based on Chinese
code GB 26538–2011 [24], the water absorption of fired bricks should not be larger than 20.0%, indicating that
the minimum sintering temperature was about 850 °C. The firing shrinkage of brick samples was −0.56 and the
water absorption increased significantly at the sintering temperature 1100 °C, showing that the brick samples
were overburned. Therefore, the highest sintering temperature was approximately 1050 °C.
Figure 6 gives the XRD pattern of shale at different sintering temperatures. The contents of quartz and albite
in the brick samples decreased as the sintering temperature increased. Liquid phase appeared at the contact part
of albite and quartz at the temperature 900 °C, and the feldspar and quartz content decreased. Following the
increase of sintering temperatures, quartz content decreased and part of the quartz crystals were melt in the glass
phase of the samples, and mulita would be formed because of the reaction between the quartz and alumina.
Finally, a large amount of glass phase was formed at 1050 °C, indicating that the sintering temperature should
not be higher than 1050 °C.
According to the study of He [32] and figures 4–6, the optimum sintering temperature of shale was
calculated from the equation:
Where Ts is initial sintering temperature and equals to 850 °C, Te is melting temperature and equals to 1050 °C.
It could be obtained that the optimum sintering temperature of shale used in this paper was about 950 °C.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
Figure 7. Effects of sewage sludge content on water content and plasticity index of green bricks.
• The organic fibers in sewage sludge absorbed a large amount of water, which reduced the free water in the
shale-water two-phase system and weakened the attraction between adjacent particles of the shale, thus
reducing the forming ability of the mixture.
• The excessive moisture of the sewage sludge affected the mixing uniformity of the sewage sludge and shale
significantly. Therefore, following the increase of sewage sludge content, the plasticity index of the green brick
decreased.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
Figure 8. Effects of sewage sludge content on drying shrinkage rate and firing shrinkage rate.
Figure 9. Effects of sewage sludge content on bulk density and compressive strength.
3.2.2. Effects of sewage sludge content on the drying shrinkage rate and firing shrinkage rate
The drying shrinkage rate and firing shrinkage rate affected the manufacture of the production mold and the
outer dimensions of the specimen. Figure 8 presents the test results for shrinkage rate. The highest shrinkage rate
was observed in specimens with 15% content of sewage sludge additive. In this case, the drying shrinkage rate
and firing shrinkage rate increased 16.6% and 58.8%, respectively. This was due to the fact that the water content
required for brick forming increased with the increase of replacement ratio of sewage sludge, and the
evaporation of water led to the shrinkage of brick during the drying and sintering process.
3.2.3. Effects of sewage sludge content on bulk density and compressive strength of brick
Smaller bulk density of brick helped to reduce the building self-weight and construction cost, and adequate
compressive strength of brick was a necessary condition for its application in engineering. The test results of bulk
density and compressive strength of bricks are given in figure 9. The bulk density produced with 0% sewage
sludge exhibited a value of 1770 kg m−3, this value reduced to 1230 kg m−3 at the 25% replacement ratio. This
revealed that the high loss on ignition of sewage sludge resulted in a large number of pores after firing, which
effectively reduced the bulk density of bricks.
The compressive strength of the brick decreased rapidly with the increase of sewage sludge content. The
compressive strength was 13.95 MPa for the 0% replacement ratio, and when the sewage sludge content was
25%, the compressive strength decreased to 3.00 MPa. This situation was due to the reason that the number of
pores increased with the increase of sewage sludge content, which reduced the cross-sectional stress area of the
brick.
According to Chinese code GB 50003–2011 [33], the compressive strength of fired bricks should not be less
than 5.0 MPa, while the compressive strength was 4.42 MPa for the 20% replacement ratio. Therefore the
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Mater. Res. Express 8 (2021) 095510 J Wu et al
Figure 10. Microstructure images of (a) brick without sewage sludge, (b) brick with 15% replacement ratio of sewage sludge.
replacement ratio of sewage sludge should not be more than 15%. Considering that the other parameters
satisfied the requirements of manufacturing and application of fired brick, the optimum replacement ratio of
sewage sludge was determined to be 15%.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
4. Conclusions
The effect of different content of sewage sludge on the properties of green or fired shale bricks were examined
experimentally. It was found that the physical, mechanical and thermal performances as well as microstructure
of the bricks were affected apparently by the additive of sewage sludge. The main observations are summarized as
follows:
1. According to the analysis of XRF, shale (large amount of SiO2 and Al2O3) was a fit bloating material for
manufacturing fired bricks independently, while the sewage sludge could only be used as additive to
improve the properties of the bricks.
2. After the introduction of fired shale bricks without the sewage sludge additive at 800 °C–1100 °C
temperature, the ceramic body with the following parameters was created: the firing shrinkage 0.51–
(−1.16)% and water absorption 22.05%–13.86%. Taking into account of the XRD and thermal
characteristics, the optimum sintering temperature of shale was determined to be 950 °C.
3. After the introduction of 0%–30% of sewage sludge additive into shale mixture and the burning of the
bricks at 920 °C–950 °C temperature, the following parameters of green or fired bricks was created: the
water content 19.00%–24.21%, plasticity index 12.22%–7.02%, drying shrinkage 4.22%–5.15%, firing
shrinkage 0.97%–1.36%, bulk density 1770–1260 kg m−3 and compressive strength 13.95–3.00 MPa.
Considering the requirements of manufacture and engineering application of bricks, the optimum
replacement of sewage was determined to be 15%.
4. As could been seen from the SEM images of the bricks, the microstructure of the brick was disrupted by the
sewage sludge. The microstructure of reference specimen was denser than the microstructure of specimen
containing 15% of sewage sludge, the results could also be seen from the results of the physical and
mechanical tests.
Acknowledgments
This research was supported by the Natural Science Foundation of Shaanxi Province (2021JQ-876) and
Scientific Research Foundation for High-level Talents (XJ17T08). The authors would like to thank Shaanxi Key
Laboratory of Safety and Durability of Concrete Structures for the project testing.
The data generated and/or analysed during the current study are not publicly available for legal/ethical reasons
but are available from the corresponding author on reasonable request.
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Mater. Res. Express 8 (2021) 095510 J Wu et al
We declare that we do not have any commercial or associative interest that represents a conflict of interest in
connection with the work submitted.
ORCID iDs
Jian Wu https://orcid.org/0000-0001-5698-3657
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