HBRC Journal (2018) 14, 309–315

Housing and Building National Research Center

HBRC Journal

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FULL LENGTH ARTICLE

The use of sewage sludge in the production of

ceramic floor tiles
Sh.K. Amin a,*, E.M. Abdel Hamid b, S.A. El-Sherbiny b, H.A. Sibak b, M.F. Abadir b

a
Chemical Engineering and Pilot Plant Department, Engineering Research Division, National Research Centre, Giza, Egypt
b
Chemical Engineering Department, Faculty of Engineering, Cairo University, Egypt

Received 21 August 2016; revised 18 January 2017; accepted 6 February 2017

KEYWORDS Abstract Scientists proved that municipal sewage sludge contains many dangerous pathogens,
Sewage sludge; toxic heavy metals, endocrine disruptors, drains, storm water runoff, hospitals, and industrial
Ceramic; plants. Sewage sludge represents an extremely high ecological hazard to the environment. Due to
Floor tiles; the increasing amount of sludge generated from the wastewater treatments plants a strong demand
Standards for environmentally and effective safe reuse has arisen. One potential use of that waste is its incor-
poration in the production of ceramic tiles. The main aim of present work was to study the possi-
bility of usage of this hazardous waste in floor ceramic tiles industry. A dried sludge waste was
added in percentages from 5% up to 35% to a standard floor tile mix, molded, pressed uniaxially
at 30 MPa and then fired at temperatures reaching 1150 °C for 15 min soaking time. The properties
of both green and fired tiles were investigated as function of percent waste added. The vitrification
parameters, which are linear firing shrinkage, water absorption, apparent porosity, and mechanical
property, were determined and compared with ISO standards. Fired samples of the proposed mix-
tures were investigated by scanning electron microscope (SEM). It was possible to obtain tiles that
abided by ISO standards for maximum addition of 7% sludge fired at 1150 °C (for water absorp-
tion < 10%), and 10% sludge or 5% sludge for tiles fired at 1150 °C and 1100 °C, respectively (for
water absorption > 10%), which are recommended for both their economic and environmental
benefits.
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* Corresponding author at: Chemical Engineering and Pilot Plant Department, Engineering Research Division, National Research Centre, 33 El
Bohouth St. (Former El Tahrir St.), PO box 12622, Dokki, Giza, Egypt. Affiliation ID: 60014618. Fax: +20 2 33370931.
E-mail addresses: [email protected], [email protected] (S.K. Amin).
Peer review under responsibility of Housing and Building National Research Center.

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310 S.K. Amin et al.

Introduction Table 1 Raw mix tile body composition.

Raw materials Source wt%
Sanitary landfills are commonly used for disposal of sewage
sludge and rapid urbanization and it is difficult to find any Ball clay Aswan (upper Egypt) 35
Aswan clay Aswan 25
suitable landfill sites so that incineration has become one of
Bentonite Burg El – Arab, Alexandria 2
the few alternatives available for disposal sewage sludge [1].
Potash feldspar Eastern desert 28
In a comprehensive review, Donatello and Cheeseman [2] Glass sand Zaafarana, Suez Gulf 10
have enumerated actual and potential uses of incinerated sew-
age sludge ash (ISSA). These included, among other uses, their
inclusion in mixes in the brick, tile and paving industry, man-
ufacture of light weight aggregate, glass ceramics, and partial Eastern Cairo. It was dried at 110 °C for 24 h in a muffle dryer
substitute for cement, beside applications related to their high before usage.
phosphate content. The mineralogical composition of both materials was
In the clay brick industry, an early work was conducted by assessed using X-ray diffraction Brukur D8 advanced comput-
Tay [3] who noticed a slight regular decrease in compressive erized X-ray diffractometer apparatus with mono-chromatized
strength following addition of ISSA. The same trend was Cu Ka radiation, operated at 40 kV and 40 mA.
observed later by Trauner [4] although the drop in compressive On the other hand, chemical composition was determined
strength on adding 30% ISSA was spectacular. It was con- using X-ray fluorescence technique type. The used machine
cluded that the effect of using ISSA in clay bricks preparation was Axios, panalytical 2005, wavelength dispersive (WD–
depends mainly on the chemical composition of the waste, so XRF) sequential spectrometer.
that no general trend could be established [5]. A limited num- Thermal analyses (TGA – DTG – DTA) were performed on
ber of studies addressed the use of ISSA as substitute for clay both materials using Netzsch STA 409 C/CD apparatus at a
in the manufacture of ceramic tiles. Jordán et al. [6] investi- heating rate of 10 °C/min. Runs were performed in air.
gated the substitution of clay by sewage sludge in different pro- The grain size distribution was determined according to the
portions not exceeding 10% in a ceramic wall tile body. They standard sieving procedure described by ASTM D 422 [10].
could not find any clear relation between the values of linear Finally, the powder densities of basic mixture of floor tiles
contraction and the percentage of sludge. However, the (raw mix) and sludge waste were measured using the standard
increase in water absorption with the increase in the sludge Pycnometer method (density flask). This method is a very pre-
percentage was clear. On the other hand, the addition of sludge cise procedure for determining the density of powders, gran-
gave rise to a decrease in the bending strength. Göl [7] investi- ules and dispersions that have poor flowability characteristics
gated the use of the marine sludge as additives in production of [11].
ceramic tiles. The results of his work indicated that blending
marine sludge into the ceramic powder mixtures in the 20– Samples preparation
50% range was beneficial for tile production. On the other
hand, Baruzzo et al. [8] studied samples using not only dredg-
ing spoils alone, but also mixtures with other waste materials The dried unfired sludge was blended in different proportions
such as bottom ashes from an incinerator of municipal solid (up to 35% by weight) with the basic mixture powder in a lab-
waste, incinerated sewage sludge from a municipal sewage oratory horizontal tumbler for two hours. The plasticity of the
treatment plant and steelworks slag. They concluded that the different blends was determined using the Pfefferkorn method
firing shrinkage was too high for the production of tiles. Also, [12].
Montero et al. [9] investigated the effect of the addition of mar- Rectangular tile specimens of approximate dimensions of
ble sludge and urban sewage sludge in different proportions to 110.4  55.4  8 mm3 were prepared from the blends by dry
clay in a ceramic body. They deduced that incorporation of pressing using automatically laboratory hydraulic press under
these residues has to be limited due to increase in water uniaxial pressure of 30 MPa and 5% water. Tile specimens
absorption and decrease in the bending strength. were then dried on a laboratory dryer for 24 h at (110 ± 5) °C.
In the present work, sewage sludge was taken from the resi- The following properties for green dried samples were
due of a municipal water plant located in Eastern Cairo and determined: Linear drying shrinkage and dry modulus of rup-
added in various proportions to ceramic floor tile mixes in a ture. Each sample consisted of three specimens and the average
contribution to limiting their harmful environmental effect value was calculated.
and at the same time realizing a positive economic benefit by Samples were then fired in a laboratory muffle furnace fol-
decreasing the amount of clay in the mixes. lowing a programmed schedule that takes into account the
evolution water from the dehydroxylation of kaolinite by fix-
ing the temperature at 750 °C for 30 min. The maximum tem-
Materials and methods
peratures attained had varied from 1050 °C to 1150 °C with a
soaking time of 15 min to simulate fast firing conditions.
Raw materials characterization
The following tests were performed to determine the char-
acteristics of fired samples: Percent of linear firing shrinkage
Two components were used. First, the raw mix was used to [13], percent of water absorption and apparent porosity [14],
manufacture ceramic floor tile bodies (supplied by Ceramica breaking strength and modulus of rupture [15]. SEM was also
Royal Company located in a Cairo suburb) the composition used to provide micrographs of some chosen sections. The
of which is displayed in Table 1, and the sewage sludge that used SEM apparatus was of type JEOL–JSM 6510 apparatus
was collected form a municipal treatment plant located in with maximum zoom magnification power = 300,000.
Production of ceramic floor tiles 311

Results and discussions in sludge which have lower densities than their inorganic coun-
terparts present in tile mix.
Raw materials characterization
Characteristics of unfired mixes
The XRF results for both raw materials are shown in Table 2.
The high value of LOI for sewage sludge is due to its ele- Effect of addition of sludge on the plasticity of mixes
vated organic matter content, while most LOI for raw mix is The plasticity of the studied tile mixes of different proportions
due to de-hydroxylation and water releasing of clay. of sludge was determined using the Pfefferkorn apparatus. The
On the other hand, XRD analysis has shown that the main final results illustrating the effect of waste addition on plastic-
phases constituting the raw mix were as follows (Fig. 1): ity are shown in Fig. 4-a. There is an almost linear increase in
quartz, albite, kaolinite and calcite. The XRD analysis of plasticity with the addition of sludge. The plasticity number
sludge displayed low crystallinity and only two phases were was practically doubled when the percent sludge was increased
obtained: quartz and albite. from 0% to 35%. This can be understood in light of the dual
Thermal analyses of both materials disclosed the following effect of finer particle size and organic matter on plasticity [16].
information (Fig. 2a and b): In Fig. 2-a there is a slight early
decrease in weight due to elimination of physical water fol- Effect of addition of sludge on the percent linear drying
lowed by a small exothermic peak at about 425 °C due to oxi- shrinkage
dation of organic impurities. An extended endothermic peak Since the moisture content used (5%) is lower than the critical
follows at about 485 °C presumably due to loss of lattice water moisture content of ceramic–water mixtures, which usually
of clays present in the raw mix that is practically completed at ranges from 10% to 30% [17], then, there will be no shrinkage
about 650 °C. The percent weight loss accompanying that step for as much as 35% sludge addition [18].
(about 6%) fairly agrees with the expected theoretical loss of
6.19% (Table 1).
Fig. 2-b displays the TG – DTA patterns for the used Effect of addition of sludge on the green strength
sludge. Owing to the absence of any decomposable compounds Although the green strength is by no means a standard require-
except for organic components, there were no definite peaks on ment of ceramic tiles, it nevertheless affects the proportion of
the graph. The endothermic peaks encountered below 136 °C rejected dry tiles due to losses on handling. There is no recom-
are probably due to evaporation of physical water. This mended figure for green strength (or alternatively, modulus of
accounts for about 17.4% of the floor mix. A larger weight loss rupture) although values of MOR lower than 0.5 MPa are
can be seen starting at about 260 °C and practically ending at commonly associated with minor losses on handling. It
about 500 °C associated with oxidation of organic compounds appears from Fig. 4-b that there is a steady decrease in bending
and accounting for more than 40% of the weight loss over that strength on adding sludge. One possible reason is the low dry-
range. Above 500 °C, there is a slight gradual loss reaching 5% ing shrinkage associated with adding sludge, as it is known
at 1000 °C. The overall loss in weight = 62.66% matches with that shrinkage imparts more cohesive character to the mix. It
the measured percent loss on ignition of 65% given in Table 1. hence appears that the recommended percentage of sludge
The screen analyses of raw materials (Fig. 3) have shown addition should be less than 20% to avoid serious losses on
that dried sewage sludge is much finer than the raw mix. The handling.
median diameter of the former was 0.13 mm compared to
0.42 mm for the latter. Characteristics of fired tile samples
The powder density of floor tiles mix and sewage sludge
waste is 1.73 and 0.92 g/cm3, respectively. It appears that the Effect of addition of the sludge on linear firing shrinkage
density of tile mix is significantly higher than that of waste Fig. 5-a displays the effect of sludge addition on linear firing
sludge. This is related to the nature of the organic components shrinkage. While increasing the firing temperature had a pre-
dictable effect of increasing shrinkage, the effect of adding
sludge was insignificant at all firing temperatures. The main
Table 2 Chemical analysis of the used raw materials (by wt reason for shrinkage is the elevated amount of feldspar in
%). the original mix which, by lowering vitrification temperature
Elemental oxides Floor mix Sewage sludge enhances liquid phase sintering [19]. As the percentage of
sludge is increased there is a subsequent decrease in raw mix,
SiO2 58.53 9.46
meaningless feldspar. This could explain the decrease in
Al2O3 22.97 2.62
Fe2Otot. 3.68 5.73
shrinkage observed in all curves when the level of sludge
3
TiO2 1.06 0.54 exceeds 15%. It is to be noted that all samples resulted in fired
MgO 1.4 0.87 tiles of thickness lower than 7.5 mm owing to firing shrinkage.
CaO 1.34 6.02
Na2O 2.59 0.31 Effect of addition of the sludge on water absorption
K2O 1.37 0.53 Water absorption is a main property to be considered when
P2O5 0.21 3.81
characterizing ceramic tiles of any type. Its percentage reveals
SO3 0.41 4.06
Minor oxides 0.404 1.381
the open porosity of the tile that reflects the degree of vitrifica-
L.O.I 6.19 65.00 tion. According to the International Standard [19], ceramic
Total 100.154 100.331 tiles are classified as either having percent water absorption
higher than 10% or lying between 6% and 10%. Floor tiles
312 S.K. Amin et al.

Figure 1 XRD patterns of the used raw materials, (a) floor mix, and (b) sewage sludge waste.

(a) Floor Mix (b) Sewage Sludge Waste

Figure 2 DTA and TGA patterns of (a) floor mix, and (b) sewage sludge waste.

Figure 3 Cumulative fraction retained for different raw materials.

Production of ceramic floor tiles 313

(a) Plasticity Number (b) Green Modulus of Rupture

Figure 4 Effect of sludge addition on unfired mixes properties, (a) plasticity number, and (b) green modulus of rupture.

Figure 5 Effect of sludge addition on characteristics of fired tile samples, (a) linear firing shrinkage, (b) water absorption, and (c)
apparent porosity.
314 S.K. Amin et al.

Table 3 Minimum permissible values for breaking strength and MOR [20].
Thickness < 7.5 mm Thickness  7.5 mm
6% < WA  10% WA > 10% 6% < WA  10% WA > 10%
Breaking strength, (N) 500 200 800 600
MOR, N/mm2 (MPa) Minimum 18 15 Minimum 18 12
Individual minimum 16 Individual minimum 16

Effect of addition of the sludge on apparent porosity

This property is not a standard requirement although it is
indicative of the percentage of open pores and hence extent
of vitrification in more direct way than water absorption, to
which it is strongly related. As expected, in case of floor tiles,
adding waste caused an increase in open pores following oxi-
dation of organic components present in waste as can be
shown in Fig. 5-c. The SEM micrograph of the surface of a
transversal section in a tile containing 15% sludge fired at
1150 °C is shown in Fig. 6. It indicates a clear reduction in
porosity owing to the apparent glassy phase that has been
formed [21].

Effect of addition of the sludge on mechanical strength

According to the International Standard [20], the mechanical
strength of ceramic tiles has to be formulated as two values:
Figure 6 SEM micrograph of a specimen containing 15% waste
The breaking strength and the modulus of rupture. The mini-
fired at 1150 °C (1600).
mum values of breaking strengths and MOR are related to the
tile thickness as shown in Table 3.
usually lie in the latter category [20] although cheap articles The effect of adding waste to floor tiles mix on mechanical
commonly have absorption values > 10%. As can be seen properties was established as being one of the most important
from Fig. 5-b, it is clear that water absorption is strongly properties governing the viability of using the tiles. In this
affected by the presence of waste, its values reaching 40% respect, the breaking strength and the modulus of rupture
for high level of sludge addition. To abide by ISO standard serve to assess the mechanical strength of the tile body. Other
for water absorption < 10%, it is necessary to add no more properties such as abrasion resistance and skid resistance are
than 15% waste and fire at 1150 °C. If the tiles are categorized concerned with the finished glazed surface rather than the
as having a water absorption > 10%, then more waste can be body are were not consequently considered in this work. Actu-
added and lower firing temperatures can be used. ally, breaking strength and modulus of rupture are closely

Figure 7 Effect of sludge addition on mechanical strength, (a) breaking strength, and (b) modulus of rupture.
Production of ceramic floor tiles 315

related as can be seen in Fig. 7-a and -b. Values of breaking [6] M.M. Jordán, M.B. Almendro-Candel, M. Romero, J.M.
strength and MOR for floor tiles displayed in the aforemen- Rincón, Application of sewage sludge in the manufacturing of
tioned figures show that for floor tiles of thickness < 7.5 mm ceramic tile bodies, Appl. Clay Sci. 30 (3–4) (2005) 219–224.
and water absorption < 10%, the minimum breaking strength [7] C. Göl, Production of ceramic tiles by using marine sludge
additives MSc. Thesis, IZTECH, Turkey, 2006.
of 500 N was achieved for tiles fired at 1150 °C and containing
[8] D. Baruzzo, D. Minicelli, S. Bruckner, L. Fedrizzi, A.
less than 7% waste. For water absorption higher than 10% the Bachiorrini, S. Maschio, Possible production of ceramic tiles
permissible waste percent can reach 10% or 5% for tiles fired from marine dredging spoils alone and mixed with other waste
at 1150 °C and 1100 °C respectively. As for thick tiles, any materials, J. Hazard. Mater. 134 (1–3) (2006) 202–210.
addition of waste makes the breaking strength drop below [9] M.A. Montero, M.M. Jordán, M.S. Hernández-Crespo, T.
the minimum standard value of 600 N. Sanfeliu, The use of sewage sludge and marble residues in the
manufacture of ceramic tile bodies, J. Appl. Clay Sci. 46 (2009)
Conclusions 404–408.
[10] ASTM D 422/1963 (Reapproved 2007), Method for particle–size
analysis of soils, ASTM Annual book, U.S.A., 4(8), 2016.
Dried sewage sludge was mixed with a standard mix of ceramic [11] ASTM B 311/2013, Standard test method for density of powder
floor tiles at percentages reaching 35%, molded and pressed metallurgy (pm) materials containing less than two percent
uniaxially at 30 MPa. Firing was performed for a soaking per- porosity, ASTM Annual book, U.S.A., 2(5), 2016.
iod of 15 min to simulate industrial fast firing conditions. It [12] F.A. De-Andrade, H.A. Al-Qureishi, D. Hotza, Measuring and
was possible to obtain tiles of thickness around 7.5 mm that modeling the plasticity of clays, Mater. Res. 13 (3) (2010) 395–
abided by standards for maximum addition of 7% sludge fired 399.
at 1150 °C (for water absorption < 10%), and 10% sludge or [13] ASTM C 326/2009 (Reapproved 2014), Standard test method
for drying and firing shrinkages of ceramic white–ware clays,
5% sludge for tiles fired at 1150 °C and 1100 °C, respectively
ASTM Annual book, U.S.A., 15(2), 2016.
(for water absorption > 10%). [14] ASTM C 373/2014, Standard test method for water absorption,
bulk density, apparent porosity, and apparent specific gravity of
Conflict of interest fired white ware products, ASTM Annual book, U.S.A., 15(2),
2016.
[15] ISO 10545 – 4 / 2014, Ceramic Tiles – Part 4: Determination of
None declared.
Modulus of Rupture and Breaking Strength, International
Organization for Standardization (ISO), Geneva, 2014, pp. 1–
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