Ceramic Tile Formulations From Industrial Waste

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J.A. Junkes1, M.A. Carvalho2, A.M. Segades3, D. Hotza1

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Effect of Bi2O3 on Cordierite Formation in Cordierite Based Bodies
Ceramic Tile Formulations from

Industrial Waste
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The authors
The main author, Janana Accordi Junkes, received a MSc
in Materials Engineering from the Federal University of
Santa Catarina, Brazil. She is currently earning her Doctorate in Materials Science and Engineering at the same
university. As part of her research, she has also spent
time at the University of Aveiro in Portugal. Ms. Junkes is
one of 20 young scientists from around the world, who
won the Green Talents 2010 International Forum for
High Potentials in Sustainable Development Competition of the German
Federal Ministry of Education and Research (BMBF) for her work on reusing
mineral waste for tile manufacturing. In her research activities, she is focusing on waste treatment, zeolites, ceramic materials, ceramic processing, and waste management. E-mail: janajunkes@hotmail.com
The corresponding author, Dachamir Hotza, earned his
PhD (Dr.-Ing.) from the Technical University of HamburgHarburg (Germany). During his postdoctoral studies he
did research at the University of Erlangen (Germany),
OMTRI (Japan), and University of Queensland (Australia).
He is currently Associate Professor at the Department of
Chemical Engineering and the Graduate Program on Materials Science and Engineering at UFSC, Brazil. Prof.
Hotzas research interests include recycling of solid wastes, ceramic
processing, nanotechnology, and rheology. E-Mail: hotza@eng.ufsc.br
Maria Arlete Carvalho earned her MSc in Ceramic and

Glass Engineering from the University of Aveiro, Portugal.
She is currently working on her PhD in the Materials Science and Engineering Department of the same university.
Her main research interests are: development of new materials, study and optimization of processes in the area of
ceramic materials/construction ceramic materials, as well
as the behaviour of magnesium phosphates.
E-mail: acarvalho@estg.ipvc.pt
Ana Maria Segades earned her PhD in Chemical Engineering from Sheffield University, UK. After this, she
worked as postdoctoral researcher at the University of
California in Santa Barbara, USA, and in Brazil. At present
she is Associate Professor at the Aveiro University, Por
tugal. The research areas of Prof. Segades are: phase
diagrams and ceramic processing in general, refractory
castables, hydration behaviour of calcium aluminates
and magnesium phosphates, structural porous ceramics with engineered
microstructure, combustion synthesis of ceramic oxide powders, design of
experiments, reuse and recycling of industrial wastes and sub-products.
E-mail: segadaes@ua.pt
Abstract
In recent years scientific issues related to environmental preservation
have acquired great importance and a major challenge to be met is the
recycling of materials discarded by various productive sectors. Due to the
damage caused to the environment by technological development
through the disposal of waste, this study seeks to evaluate the possibility of using industrial waste as alternative raw materials in the manufacture of ceramic tiles. Different industrial wastes that are classified as
non-hazardous were selected: sludge from the crushing process of
gneiss, sludge from the cutting and polishing process of varvite, sludge
from the process of filtration-clarification of potable water and a clay
also classified as waste. As it was generated, all waste was dried and
disaggregated in ball mills, and characterized by X-ray fluorescence, Xray diffraction, differential thermal and gravimetric analysis, optical
dilatometry, and particle size distribution. The applicability of these
wastes in the manufacture of ceramic tiles was guided by the phase dia-
Keywords
waste, tile, ceramic formulation, phase diagrams
Interceram 60 (2011) [1]
Group of Ceramic and Glass Materials (CERMAT), Departments of Mechanical

Engineering (EMC) and Chemical Engineering (ENQ),, Federal University of Santa
Catarina (UFSC), 88040-900 Florianpolis, SC, Brazil. Contact: hotza@eng.ufsc.br
Polytechnic Institute of Viana do Castelo (ESTG-UIDM), 4900-348 Viana do Castelo,
Portugal
Department of Ceramics and Glass Engineering (CICECO), University of Aveiro (UA),
3810-193 Aveiro, Portugal
gram of the system SKA, and four formulations were established. For
initial testing, these formulations were mixed and pressed into pellets,
and sintered at 900C, 950C, 1000 C, 1050C, 1100C, and 1150C.
The plasticity formulations were evaluated by the Casagrande method
with good results. Moreover, based on those preliminary results and after optimization of the processing conditions, the extrusion technique
was used for the shaping process. The extruded samples were fired at
1100C and 1150C for 40 min and characterized by X-ray diffraction,
differential thermal and gravimetric analysis, optical dilatometry, linear
shrinkage, water absorption, and flexural strength. The crystalline phases identified were associated with the sintering conditions (temperature,
time, atmosphere), as well the intrinsic characteristics of raw materials
such as chemical composition, particle size and homogeneity. The wastes
proved to be good alternative raw materials and the corresponding formulations were shown to be viable in the manufacture of ceramic tiles.
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1 Introduction
The ceramic industry covers a diverse range
of compounds, and several products can be
manufactured by different methods. Therefore, this industry presents favourable conditions for the implementation of waste
recovery systems.
Solid wastes are generated as by-products of
industrial processes or as sludge from wastewater treatment plants. It is therefore important to know the operations that generate waste, as well as the factors that affect its
generation in manufacturing processes [1].
It is often overlooked that some wastes are
similar in composition when compared to
raw materials, containing materials that are
not only compatible, but beneficial to the
manufacture of ceramics [2].
The fabrication of products from waste is an
advantage that may give the manufacturer a
highly competitive position in the market
due to economic issues involved and the opportunity of marketing this principle particularly with regard to the ecological aspect
[3]. It is in this context that the use of phase
diagrams becomes a useful tool to guide ceramic production and also to assist in making good choices of composition and
processing parameters.
A great deal of solid wastes, as well as natural
raw materials (whether plastic, fluxing, or
inert) contain, as major components, silica
(SiO2), alumina (Al2O3) and lime (CaO). Minor amounts of other components may be
present, which will mostly affect the colour
of the fired product (Fe2O3, MnO, TiO2,
Cr2O3) but should not play such an important role during ceramic processing in air at
low temperatures. Other minor components
(MgO, K2O, Na2O) will act as fluxes and may
have a strong effect during sintering [4].
The phase diagrams provide a clear and
concise method of graph representation of
the equilibrium state for a given composition, temperature and pressure [5], and this
may provide a valuable estimate of the phase
proportion present during and after sintering, i.e. the presence of liquid phase at sintering temperature and the resulting crystalline phases [6]. Stable phase equilibrium diagrams represent phases that may be expected from reactions occurring under equilibrium conditions and, therefore, provide a
basis for making predictions of the material
behaviour under various conditions of service or processing. Not all reactions reach
complete equilibrium, and consequently,
the phases which are present in a given system may not be the equilibrium phases [7].
Although in normal industrial operating
conditions thermodynamic equilibrium is
usually not reached, the equilibrium phase
diagram of the relevant system can still be

used to foresee the reactions tendency to
completion and be of great assistance for
making appropriate choices of compositions and processing parameters [6].
Although it is a possibility and a priority to
reduce the amount of waste during production and even post-consumer use, waste will
always be generated. Sustainable development requires a reduction in consumption
of natural raw materials that are not renewable. The closure of the production cycle,
generating new products from recycled
waste, is an irreplaceable alternative.
The use of wastes from the beneficiation of
ornamental rocks has been investigated,
usually by the addition of up to 50 mass-%
of waste into clayish products [811]. The
wastes may be used to replace conventional
flux materials, with the advantage of controlling the plasticity and shrinkage of the
ceramic body without producing any negative effect on the product properties, and allowing sintering at low temperatures, thus
resulting in energy conservation.
This work aims to formulate new ceramic
tiles from mineral wastes, based on phase
diagrams, allowing the withdrawal of those
residues from the environment and giving
them a nobler destination.
U1_U4_IC_2_10.indd 2
2 Experimental
Mineral wastes with the potential of being
reclaimed through their use as alternative
raw materials in the ceramic industry were
selected from Santa Catarina state, Brazil.
The selected wastes were: sludge from the
crushing process of gneiss, sludge from the
cutting and polishing process of varvite,
sludge from the process of filtration/clarification of potable water, and an iron-containing residual clay.
Ceramics Forum
A relevant ternary system was chosen to

guide the formulation of products. The
mixtures were prepared with the as-received
raw materials, according to the predetermined amounts.
The formulations were homogenized with a
blender (Gelenski, LIG-05) and molded in
an extruder with a matrix adjusted for producing cylindrical specimens.
After extrusion, the specimens were airdried at room temperature and sintered at
1100C and 1150C with a heating rate of
5C/min for 40 min. For sintering, a laboratory oven (Termolab) with a maximum
working temperature of 1700C was used.
The chemical composition of the wastes
was determined by X-ray fluorescence
(Philips, PW 2400). The mixtures were analyzed by X-ray diffraction (Philips, Xpert),
particle size distribution (laser diffractometer CILAS, 1064L), differential thermal
and thermogravimetric analysis (Netzsch,
409 EP). The Casagrande method was applied to evaluate the plasticity of mixtures,
and tests of linear shrinkage, water absorption and three-point flexural strength were
accomplished in a universal testing machine (Shimadzu AG-25TA). The microstructural analysis of fracture surfaces was
performed by scanning electron microscopy (Shimadzu, SSX-550).
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3 Results and discussion

The chemical compositions of the four
wastes investigated in this work are shown
in Table 1, as well as the average particle sizes as determined by laser diffraction. The
average particle size (d50) is between 4 and
13 m, which may favour obtaining good
mixing and suitable packaging in the forming step.
Table 1 Chemical composition and average particle size

Oxides
Clay /
mass-%
PWS /
mass-%
Gneiss /
mass-%
Varvite /
mass-%
SiO2
63.01
53.30
59.22
74.32
Al2O3
19.55
22.10
16.75
8.79
Na2O
0.05
0.24
4.48
3.12
K2O
2.83
2.11
4.31
1.48
CaO
0.04
0.12
5.98
2.68
MgO
0.77
1.20
1.63
1.74
Fe2O3
6.51
7.02
4.56
2.43
MnO
0.02
0.09
0.14
0.16
TiO2
0.91
0.83
0.43
0.51
P2O5
0.07
0.24
0.75
0.18
Loss on fire
6.30
12.76
1.74
4.59
Particle size / m
5.30
4.37
13.37
7.87
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Fig. 1 SiO2Al2O3K2O phase diagram including the compositions of waste raw materials and
formulations
Fig. 2 X-ray diffraction of the samples sintered at 1100C and 1150C: (a) F1, (b) F2, (c) F3, (d) F4
The wastes are composed predominantly of

silica and alumina, also containing high percentages of iron oxide (III) and potassium
oxide. The waste with the highest loss on firing (~13%) was potable water station
(PWS) sludge due to constitutional water
and organic matter.
From the chemical analysis data, one
point for each waste was traced within the
chosen phase diagram (SiO2Al2O3K2O).
The effect of oxide fluxes on the system
Al2O3SiO2 was discussed in terms of the
junction of the components CaO + MgO +
K2O + Na2O. All formulations set forth in
this study are positioned within the mullite field, as shown in Fig. 1.
According to the diagram, four formulations were chosen. The mass-% of each
waste in the formulations is presented in
Table 2.
To identify the mineralogical phases X-ray
diffraction was used. Figure 2 shows the
X-ray diffraction patterns of the formulations F1, F2, F3 and F4 sintered at 1100C
and 1150C for 40 min. The variations with
the increase of sintering temperature may
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Fig. 3 DTA/TG curves: (a) F1, (b) F2, (c) F3, (d) F4
12.04.10 13:54
Fig. 5 Linear shrinkage (a) and water absorption

(b) of samples sintered at 1100C and 1150C
4
Table 2 Mixture formulations
Fig. 4 Liquid limit plot of according to Casagrandes method: (a) F1, (b) F2, (c) F3, (d) F4
be observed with the superposition of

iffraction patterns.
d
F1 showed peaks of albite (NaAlSi2O8),
anorthite
(CaAl2Si3O8),
orthoclase
(KAlSi3O8) and microcline (KAlSi3O8). The
mullite (3Al2O32SiO2) peaks were formed
as a result of kaolinite transformation during calcination of clay and the PWS sludge
present in the formulation. At 1150C peaks
of quartz, albite, mullite, and hematite
(Fe2O3) are evident.
Peaks of mullite and hematite were found as

well as peaks of quartz and anorthite at
1100C and 1150C in F2.
F3 presents peaks of quartz, albite and
anorthite. Magnesium silicate (enstatite,
Mg2(Si2O6)) was also identified. This silicate
was possibly formed from the decomposition
of clinochlore ((Mg,Fe)5Al(Si3Al)O10(OH)8)
originally present in varvite.
In the diffractogram of F4 at 1100C peaks
of quartz, anorthite and mullite were ob-
Formulation
Waste /
mass-%
F1
F2
F3
F4
Clay
40
20
20
30
PWS
10
65
10
20
Gneiss
45
10
10
Varvite
65
40
served, and at 1150C peaks of quartz, mullite, albite, mayenite (Ca12Al14O33) and hematite were observed.
The diffractograms of the four formulations
presented mullite peaks in accordance with
the provided from phase diagram, but due
to the amount of components present in
these four wastes, this resulted in the presence of several other phases.
The thermal behaviour of the formulations
was analyzed through DTA/TG curves
shown in Fig. 3. In the DTA curve of F1 the
release of free water at 110C and a loss of
organic matter around 280500C may be
observed. The endothermic peak at 570C
corresponds to the release of constitution
water from clays, and a slight exothermic
peak around 982C (without mass loss)
corresponds to the onset of mullite formation (as identified by XRD). The corre-
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Fig. 6 Visual aspect of samples sintered at

1100C and 1150C
Fig. 7 Flexural strength of samples sintered at

1100C and 1150C
sponding mass losses are visible in the TG

curve, with total mass loss of 10%.
In F2 the same peaks found in F1 were identified: water loss at 110C, release of organic
matter around 250520C, and constitution
water from clays at 570C. However, due to
the 65 mass-% PWS sludge content in this
composition, F2 showed an exothermic
peak around 610C due to the sulphate decomposition, which is introduced in the potable water station for particle flocculation.
The total mass loss of this formulation was
16%.
The first three peaks of F3 were also identified in F1 and F2. Besides these peaks, an endothermic peak around 820C was found,
which is probably related to the carbonate
decomposition (dolomite) present in varvite; a component that corresponds to
65 mass-% in this mixture. It is also possible
to observe a slight exothermic peak around
980C (without mass loss) due to the onset
of mullite formation as identified by XRD.
The test result obtained from F4 is similar
to that obtained from F3. However, the
peak corresponding to the carbonate decomposition around 800C is less pronounced due to a decrease of varvite content from 65 to 40 mass-%, which thereby
reduces the amount of carbonate present
in the formulation. In spite of the mullite
detected in the corresponding XRD pat-
Fig. 8 Fracture surface micrographs of samples sintered at 1100C and 1150C
tern, the formation peak of mullite is not

visible in the thermal analysis. The distinct
thermal behaviour was probably due to
different heat cycle employed.
The extrusion was used because it is a lowcost forming technique with a high production output. However, this fabrication
alternative requires that the formulations
exhibit plasticity. The Atterberg method
was used to determine the moisture content corresponding to plastic and liquid
limits. The procedure for determining the
liquid content was performed for several
amounts of water content using Casagrandes method, as shown in Fig. 4. The
plastic limit was measured using the rolls
method. The plasticity index (PI) was then

calculated as the difference between both
limits. PI determines the plasticity nature
of the sample, thus, as high is PI, more
plastic is the raw material. According to
Caputo [12], except for F3, which presented PI=14.4%, and corresponds to a moderately plastic material, all formulations
can be classified as highly plastic since their
PI is higher than 15%.
Samples sintered at 1100C and 1150C
were tested for shrinkage and water absorption, as shown in Fig. 5. After sintering at
1150C, F1, F3, and F4 showed apparent
bubbles and distortion of the specimen. F1
presented 4.6% shrinkage and water ab-
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sorption around 9% when sintered at

1100C; at 1150C the shrinkage was 6%
with a marked decrease in water absorption
to 0.56%. Samples F2 showed shrinkage
around 14% and water absorption around
0.80%, both for 1100C and 1150C. F3
sintered at higher temperature presented severe distortion and pores, which was reflected in the results of linear shrinkage (10.41%
at 1100C and 2.51% at 1150C). In relation to water absorption, the results showed
a slight difference (less than 1%) between
the samples sintered at 1100C (0.46%)
and 1150C (1.27%), despite the number of
pores introduced at higher temperature.
The same occurred with F4 samples sintered
at 1150C, although the distortion and porosity developed with the temperature was
lower in this case.
The water absorption of all samples is below
10%, which is compatible with the range
specified for ceramic tiles. With the exception of F1, all formulations sintered at
1100C were within the values expected for
ceramic tiles, according to Brazilian standard NBR 13818.
Figure 6 shows the visual aspect of the specimens after sintering. Distortion and swelling may be observed in samples F1, F3 and
F4 sintered at 1150C.
The sintering temperature had a significant
influence on the flexural strength, as shown
in Fig. 7. The thermal treatment performed
at 1150C induced the formation of cracks
and internal porosity due to the liquid
phase, causing a decrease in mechanical
strength in samples F3 and F4.
Samples F1 and F2 presented higher flexural
strength at 1150C than 1100C, but the
high temperature affected all samples in the
visual aspect, which is a very important feature for ceramic tiles.
The flexural strength of all samples tested
was in the range of 2158 MPa, which is
within the range required by ISO 13006 for
the manufacture of ceramic tiles. With the
exception of formulation F1, the samples
would even be classified as porcelainized
tiles, corresponding to a higher quality
product.
The morphological characterization of the
formulations was performed by scanning
electron microscopy on fracture surfaces of

samples subjected to mechanical strength
test. Figure 8 shows the micrographs of
samples sintered at 1100C and 1150C. F1
sintered at 1100C presented less porosity
and irregularity when compared to the samples sintered at 1150C. F2 showed a high
linear shrinkage in the samples, resulting in
the formation of cracks. F3 was well consolidated at 1100C but when sintered at
1150C it developed a large amount of
pores of different sizes that were visible even
to the naked eye. F4, sintered at 1100C,
showed a small amount of micropores, but
was as dense as the sample F3 sintered at
1100C, when sintered at 1150C, however,
it developed a large amount of porosity,
which affected its mechanical properties
and visual aspect.
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The mechanical strength of the formulated

samples is within the range of 2158 MPa,
which complies with requirements of ISO
13006. The possible applications of such ceramic tiles may be on floors and walls, indoors and outdoors, for commercial and
residential installations.
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4 Conclusions
The results confirmed the possibility of valorisation and recycling of mineral wastes
from the state of Santa Catarina, Brazil, as
sources of raw materials for the ceramic tile
industry. Thus, these industrial wastes may
be used as products with higher added value
with positive effects with respect to environmental and economical issues.
The four wastes studied are an attractive alternative and renewable source of ceramic
raw materials. Glazing would not be required for these tiles, making the process
even more affordable, since these products
would be classified as natural products,
where the colour of the waste determines
the colour of the finished product.
The phase diagram was used successfully to
guide the formulations and to help choosing
the process parameters. In all cases, it provided a basis for making predictions of material behaviour under several conditions of
service or processing.
Forming by extrusion is feasible for the
processing of these materials because the
amount of plasticity is large enough; the
plasticity index being higher than 14, with
no need for additives. The shrinkage, water
absorption, and mechanical strength tests
indicated that the best firing cycle to be used
with those alternative raw materials is at
1100C for 40 min.

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Acknowledgment
The authors thank CNPq-Brazil for the
financial support.
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Received: 18.11.2010

Ceramic Tile Formulations From Industrial Waste

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Ceramic Tile Formulations From Industrial Waste

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Including Special TILE & BRICK

Tile & Brick

Trade Fairs &

Ceramic Bricks Filling

J.A. Junkes1, M.A. Carvalho2, A.M. Segades3, D. Hotza1

Effect of Bi2O3 on Cordierite Formation in Cordierite Based Bodies