Applied Clay Science xxx (2016) xxx-xxx

Contents lists available at ScienceDirect

Applied Clay Science

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journal homepage: www.elsevier.com

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Note

Clay bricks added with effluent sludge from paper industry: Technical, economical
and environmental benefits
Carlos Maurcio F. Vieira a, Regina M. Pinheiro a, Ruben J. Sanchez Rodriguez a, Veronica S. Candido b,

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Sergio N. Monteiro b,
a
State University of the Northern Rio de Janeiro (UENF), Advanced Materials Laboratory (LAMAV), Av. Alberto Lamego, 2000, 28013-602 Campos dos Goytacazes, RJ, Brazil
b
Military Institute of Engineering (IME), Department of Materials Science, Praa General Tibrcio, 80, Praia Vermelha, Urca, RJ, 22290-270 Rio de Janeiro, RJ, Brazil

ARTICLE INFO ABSTRACT

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Article history: Recently, it was indicated that a feasible industrial alternative to valorize the sludge obtained from the treatment of waste
Received 26 February 2016 water effluent of paper fabrication in Europe is its use as raw material in the production of clay bricks. The present tech-
Received in revised form 26 June 2016 nical note is an open report, probably first in Americas, on a Brazilian industrial-scaled solution for this kind of sludge.
Accepted 2 July 2016
As a novelty, the sludge was added to a mixture of clays for improved technical properties of construction bricks. Both
Available online xxx
bricks, added with 10 wt% of sludge and conventional pure clay bricks for comparison, were simultaneously fired at a
relatively low temperature of 750 C according to the ceramic fabrication procedure. The technical characterization was
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Keywords: performed by linear shrinkage, water absorption and mechanical compression tests as per Brazilian standards. The brick
Paper sludge
consolidated structure was analyzed by optical microscopy. Environmental impact was evaluated by solution test and at-
Mixture of clays
Industrial fabrication mospheric emission by monitoring the release of SO2, NOx, TOC, CO and particulate material, according to Brazilian
Technical properties standards. The results showed that, owing to its composition and firing temperature, the addition of paper sludge into clay
Energy saving bricks contributes to a substantial reduction in price associated with a saving of 3% of fuel similar to that reported for
Spanish kilns, during the industrial firing stage. The paper sludge added clay bricks attended the technical and environ-
mental standards.
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2016 Published by Elsevier Ltd.

1. Introduction ally, earlier initiatives in Hungary (Szucs and Badasconyi, 1994),

France (Pera and Amrouz, 1998) and Slovenia (Ducman and Kopar,
According to the Brazilian Association of Pulp and Paper 2001) as well as recent works in Spain (Cusid et al., 2015; Monte
(BRACELPA, 2015) since the year 2000 the country production of pa- et al., 2009), Austria (Walter and Tesar, 2009) and UK (Smith, 2006,
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per grew almost 30% and today holds the world tenth position, with 2014) strengthened an European tradition in the incorporation of
about 10.5 million tons. The paper industry generates wastes that may sludge and other residues from the paper industry into materials for
cause a serious burden to the environment if not properly treated be- civil construction. It is worth mentioning that heavy metals (Boni et
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fore disposal. In particular, a primary sludge is obtained after the in-
dustrial treatment of the paper processing wastewaters at the effluent
treatment station. This effluent sludge from the paper industry (pa-
per sludge for short), depending on the content of heavy metals and
other substances, might be considered toxic by the Brazilian stan-
dards (ABNT, 2004a) and must be correctly disposed. Usually this is
done in a landfill, and could be associated with environmental prob-
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al., 2004; Hamm and Gottsching, 1989) were not found to represent a
major threat for the environment after convenient treatment of the pa-
per mill effluent (Thompson et al., 2001). These points were also ad-
dressed in the European IPPC document (2007).
In cement-based products for civil construction, Frias et al. (2015)
reviewed the use of paper sludge as an environmentally friendly al-
ternative for eco-efficient cement production. Buruberri et al. (2015)

lems, such as underground water contamination and soil degradation.
In general, a fresh paper sludge contains about 50 wt% of water as
well as kaolin, cellulose pulp, calcite (calcium carbonate) and resid-
ual heavy metals (Cusid et al., 2015). Industrial alternatives have,
since past decades, been proposed for its possible use in Europe. In
particular, initial works in Germany (Geller and Bienert, 1993; Junge,
2000; Khler, 1988) and Italy (Tenaglia et al., 1992; Zani et al.,
1990) contributed to establish the current state of the art. Addition
tested pulp and paper waste as secondary raw material to produce
clinker for mortar. Wong et al. (2015) applied paper sludge ash to fab-
ricate low-cost hydrophobic powder as water repellent surface coat-
ing for concrete. Raut et al. (2012, 2013) indicated that cement bricks
incorporated with recycled paper mill residues are light-weight and
meet requirements for construction materials. Modolo et al. (2011)
demonstrated the viability of producing fiber-cement roof sheets by
incorporating cellulose primary sludge generated on paper and pulp
mills. Ismail et al. (2010) investigated cement bricks fabricated from
paper sludge and palm oil ashes. Garcia et al. (2009, 2010) recy-

Corresponding author. cled metakaolinite from paper sludge as complementary cementing

Email address: snevesmonteiro@gmail.com (S.N. Monteiro) materials as well as blended cements. De Alda (2008) re

http://dx.doi.org/10.1016/j.clay.2016.07.001
0169-1317/ 2016 Published by Elsevier Ltd.
2 Applied Clay Science xxx (2016) xxx-xxx
viewed the recycling of pulp and paper mill sludge in other paper mills
to produce boards. Ahmadi and Al-Khaja (2001) found that a maxi-
mum 5% content of paper sludge might be incorporated into concrete
bricks as a replacement to fine sand. Liaw et al. (1998) proved that pa-
per sludge has a potential to replace natural aggregates to make con-
crete bricks that conform to the Chinese standards.
The reader is also referred to a general overview (Monte et al.,
2009) on the use of pulp and paper wastes for energy recovery, py-
rolysis, gasification, land spreading, composting and reuse as building
material. This latter alternative appears to be the most promising for
using paper sludge. Indeed, recycled paper residue and kraft pulp were
investigated as addition in clay brick (Demir et al., 2005; Sutcu and
Akkurt, 2009; Sutcu et al., 2014). However, these wastes associated
with the paper industry are not the same of the present work. Only
the sludge obtained in the industry treatment station of waste water
effluents shall be here considered. As for this specific paper sludge,
review articles (Cusid et al., 2015; Dondi et al., 1997; Monteiro and
Vieira, 2014; Vieira and Monteiro, 2009) discussed results of exper-
imental works on brick addition (Asquini et al., 2008; Cernec et al.,
2005; Chemani and Chemani, 2013; Likon and Trebse, 2012; Maschio
et al., 2009; Mymrin et al., 2009; Pera and Amrouz, 1998; Pinheiro
et al., 2008; Vieira et al., 2008). As aforementioned, not only labora-
tory investigations but also industrial-scaled experiences on addition
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of paper sludge in clay bricks have been conducted in several Euro-
pean countries, mainly Germany (Khler, 1988; Junge, 2000), Italy
(Tenaglia et al., 1997), UK (Smith, 2006, 2014) and Spain (Cusid et
al., 2015) that contribute to the present state of the art.
The first Brazilian experience is reported in the present work. It
can also be considered as the first in the Americas, since no similar
industrial case was found after a thorough search in the scientific and
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technical literature. This is rather surprising, especially regarding the
United States (US) and Canada, where several paper industries oper-
ate. In particular, the renowned National Brick Research Center, a US
reference associated with Clemson University, was not able to inform
on industrial experiences concerning this kind of paper sludge addition
into clay bricks. Moreover, the National Academy of Sciences (1999)
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and Usherson (1992) indicated that disposal options for paper sludge
in the US are landfilling, incinerating and landspreading. Reference
documents, such as the European IPPC Bureau (2007) only mentioned
addition of sludges inside the own ceramic industry. However, Euro-
pean industrial experiences on paper sludge addition have, as afore-
mentioned, been conducted since the end of the last century. In a re-
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cent review article, Cusid et al. (2015) indicated that the addition of
up to 15 wt% of sludge is a viable practice for the industrial produc-
tion of bricks for building construction. They concluded that a clay
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brick added with paper sludge is a feasible material for civil construc-
tion due to the major technical advantages, including mechanical, ther-
mal and acoustic properties as well as no remarkable hazardous inor-
ganic and VOC emissions during firing.
Based on this European case reviewed by Cusid et al. (2015), the
present work reports for the first time in the Americas, to the best of
our knowledge, an industrial case of recycling paper sludge by addi-
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tion into clay bricks. In this work, the use of paper sludge produced
in Brazil, added to clay bricks, is discussed both in terms of saving in
energy and cost as well as environmental benefits.
2. Experimental procedure
The raw materials used in this work were: a kaolinitic clay body,
based on a mixture of two distinct clays, used for bricks fabrication in
the state of Rio de Janeiro (RJ), Brazil, and a primary paper sludge,
containing about 54 wt% of water, generated in the effluent treatment
station of the COPAPA (Companhia de Papel Paduense), which fab-
ricates toilet tissue paper, both from recycled paper and virgin pulp,
located at the city of Santo Antonio de Pdua, also in RJ.
Both clay body and paper sludge were chemically and mineralog-
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ically characterized respectively by X-ray fluorescence (XRF) in a
Philips PW 2400 equipment and X-ray diffraction (XRD) in a model
URD 65 Sheifert diffractometer operating with CuK radiation and
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2 in the interval of 5 to 40. Thermal differential (DSC) and ther-
mogravimetric (TG/DTG) analyses of the clay body and the paper
sludge were performed in a model SDT 2960 TA Instrument from 25
to 1200 C, with heating rate of 10 C/min under air. Mixture of the
sun-dried paper sludge (until 30% of remaining water) with neat clay
body (moisten with similar amount of water) were prepared for ade-
quate brick forming. The extrusion of the 10 wt% (wet) sludge added
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clay body as well as its firing were carried out at the Rodolfo Gama
industry, in the municipal area of Campos dos Goytacazes, RJ.
Prismatic perforated bricks with dimensions of
190 190 90 mm were prepared for industrial production at the ce-
ramic industry and fired at 750 C in a modified dome type of kiln.
The water absorption and compression strength were determined ac-
cording to the Brazilian standards (ABNT, 2005). In particular, com-
pression tests were performed in a model 5582 Instron machine. Air
samples were collected during the firing process of the bricks to de-
termine the concentration and the emission of particulate material
(PM), sulfur dioxide (SO2), nitrogen oxides (NOx), total organic car-
bon (TOC) and carbon monoxide (CO) according to the Brazilian leg-
islation (CONAMA, 2002). For this purpose, it was used a Train of
Sampling Model CIPA II - Collector Isocinetic of Atmospheric Pol-
lutant type of equipment. Fig. 1 shows the kiln used in the indus-
trial-scaled production and a finished lot of paper sludge added bricks.
These paper sludge-added bricks were subjected to X-ray diffrac-
tion (XRD), microstructural analysis and solution test. The XRD
equipment was the same already described. Optical microscopy was
carried out in a model Motic Aga Scientific microscope. The solution
test was conducted according the standard (ABNT, 2004b) in order to
investigate the presence of harmful elements to the environment, such
as Al, Cd, Pb, total Cr, Fe, Mn, Zn, surfactants, cyanides and fluorides,
with limits determined by the Brazilian legislation (CONAMA, 2012).
3. Results and discussion
3.1. Materials characterization
The clay body used for addition of paper sludge was a mixture
in equal proportion of two natural kaolinitic clays found in Campos
dos Goytacazes. Table 1 presents the XRF chemical composition of
these clays, locally known as weak and strong (Vieira et al., 2006)
due to the corresponding different, low and high, amount of kaolinitic
mineral. In this table, it is also shown the composition of the clay
body, which is consistent with the fifty-fifty mixture of weak and
strong, respectively Y and G clays in Vieira et al. (2008). Moreover,
the SiO2/Al2O3 ratio of 2.13 denotes a refractory clay body. The mix-
ture of the distinct clays (Monteiro and Vieira, 2002) and the addition
of paper sludge, by its characteristics (Pinheiro et al., 2008), contribute
to improve the ceramic body workability.
Table 2 presents the XRF chemical composition of the paper
sludge that is mainly composed of CaO, SiO2, Al2O3 and carbon in
comparable amounts to a previous work (Pinheiro et al., 2008). The
 Applied Clay Science xxx (2016) xxx-xxx 3

and TG/DTG curves presented in Fig. 2 reveal that cellulose combus-

tion releases heat from 175 to 450 C, with a peak at 343 C. More-
over, at temperatures above 625 C, the gradual decomposition of cal-
cite occurs in association with a peak around 760 C and extending
further beyond. This proves that the calcite in the paper sludge still

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participates as a reactive hydraulic component, together with SiO2 and
Al2O3, for the ceramic firing consolidation. In the present work, fir-
ing was conducted at 750 C, which was sufficient to allow complete

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solid state sintering by bonding activation of the kaolinitic clay min-
eral (Monteiro and Vieira, 2004). In addition, this relative lower firing
temperature might be associated with saving in fuel and contributes to
reduce the final cost of the ceramic.

3.2. Clay brick properties

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Fig. 3 shows the XRD patterns of the neat clay brick and the
10 wt% paper sludge added brick. In both bricks, three crystalline
phases are commonly observed: muscovite mica (M), quartz (Q), and
microline (Mi). The original kaolinite of the clay was transformed
into the amorphous metakaolinite after firing at 750 C (Monteiro and
Vieira, 2004).
The 10 wt% added brick, Fig. 3(b), also exhibits XRD peaks cor-
responding to portlandite and calcium silicate, which are products of

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calcite decomposition. As shown in Fig. 2 calcite decomposition starts
to occur at 625 C. Therefore, one would expect both portlandite and
calcium silicate to occur at the industrial firing temperature of 750 C.
Table 3 presents the values of linear shrinkage, water absorption
and compression strength of the neat clay bricks and bricks added with
10 wt% (wet) paper sludge. The value of the linear shrinkage below
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1% is not a problem for the brick dimensions and prevents the forma-
tion of cracks by size contraction. The established values by Brazilian
technical standard for compression strength and water absorption are
1.5 MPa and 22%, respectively (ABNT, 2005). It is observed that
both water absorption and compression strength of the neat clay bricks
attend the standard. However, the water absorption of bricks added
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Fig. 1. (a) Modified kiln for clay brick firing and (b) a lot of fired bricks incorporated
with paper sludge.
total carbon content of 17.7% is due to cellulose in the sludge. Trace
elements, such as Cd, Pb and Zn were not detected by XRF.
The XRD analysis of the clay body showed a pattern with promi-
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with paper sludge is slightly above the maximum allowed value. Since
the water absorption is a property related to the open porosity of the
material, its change to the specified standard range of 22% can be
achieved by either reducing the amount of paper sludge or modifying
the type of clays in the body composition or even increasing the fir-
ing temperature. As for the mechanical resistance, Table 3, although
the compression strength of bricks added with paper sludge is lower

nent peaks of kaolinite, Al2Si2O5(OH)4, as well as quartz, gibbsite and in comparison with that of the neat clay bricks, the obtained value
mica. The major peaks in the pattern of the paper sludge are those of 2.6 MPa is 73.3% above the minimum of 1.5 MPa required by the
of calcite (CaCO3). Other minor peaks are associated with quartz and standard (ABNT, 2005). The small differences in water absorption and
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kaolinite. These XRD results are consistent with the chemical compo-
sition in Tables 1 and 2.
The TG/DTG curves for the clay body indicated a total weight
loss of 13.4% at 772 C. An endothermic reaction around 470 C is
associated with the formation of metakaolinite by dihydroxylation.
This favors surface bonding between clay particles above this tem-
perature (Monteiro and Vieira, 2004). As for the paper sludge, DSC
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compression strength can be assigned to phases and pores introduced
in the clay ceramic structure by the thermal decomposition, Fig. 2, of
cellulose (carbon in Table 2) existing in the paper sludge.
Fig. 4 shows optical micrographs of ceramics (a) without as well
as (b) and (c) with addition of paper sludge. Both ceramics show a

Table 1
Chemical composition (wt%) of the natural clays and clay body used in this work.

Material SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O N2O SiO2 +/Al2O3a LoIb

Weak clay 55.9 21.5 8.6 1.2 0.4 1.0 2.3 0.7 2.58 8.3
Strong clay 48.7 25.9 9.1 1.3 0.3 0.8 1.9 0.5 1.88 12.1
Clay body (50% mixture) 51.7 24.3 8.9 1.3 0.4 0.9 2.0 0.6 2.13 9.9
a
Pure kaolinite ratio: 1.18.
b
LoI = loss on ignition.
4 Applied Clay Science xxx (2016) xxx-xxx

Table 2 Table 3
Chemical composition (wt%) of paper sludge. Properties of bricks without and with 10 wt% paper sludge incorporation.

CaO SiO2 Al2O3 MgO Fe2O3 N2O TiO2 K2O Cr2O3 MnO C Properties Pure clay brick Paper sludge incorporated brick

38.1 23.4 17.0 1.9 0.8 0.2 0.7 0.1 0.1 0.1 17.7 Linear shrinkage (%) 0.83 0.02 0.81 0.03
Water absorption (%) 21.1 0.4 22.8 0.7

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Compression strength (MPa) 3.1 0.5 2.6 0.8

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Fig. 2. DSC and TG/DTG curves for the paper sludge. CT
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Fig. 3. XRD patterns of 750 C fired brick samples: (a) neat clay and (b) clay with
10 wt% added paper sludge. Fig. 4. Optical micrographs of the bricks: (a) neat clay, (b) clay added with 10 wt% pa-
per sludge and (c) CaO particle from the paper sludge incorporated in the ceramic.
rough texture with small cracks, indicated by arrows. Well-dispersed
 Applied Clay Science xxx (2016) xxx-xxx
quartz particles, surrounded by black ellipses, are also observed in
both neat (a) and incorporated (b) ceramic in Fig. 4. A light phase,
surrounded by an ellipse in Fig. 4(c) is associated with calcium sil-
icate generated during the decomposition of calcite, initially present
in the sludge (Pinheiro et al., 2008). Additionally, a relatively greater
amount of pores (arrows) was observed by defocusing procedure in
the clay brick added with paper sludge of Fig. 4(b). These pores, due
to cellulose combustion, might be responsible for the water absorption
and compression strength values presented in Table 3.
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Fig. 5. Atmospheric emissions results from collected data of (a) PM, SO2 and NO2, as well as (b) TOC and CO during the firing stage of the ceramic.
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3.3. Environmental tests
Fig. 5 presents the emission results of PM, SO2, NO2, TOC and CO
during the industrial firing of bricks incorporated with 10 wt% of pa-
per sludge. For the industrial firing, eucalyptus firewood was used as
fuel. In this figure, it is also shown the maximum allowed value of the
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five monitored parameters as per the Brazilian legislation (CONAMA,
2002). According to the obtained results, the monitored parameters in
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the gaseous effluent, MP, SO2, NO2, TOC and CO, are within the le-
gal established patterns.
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6 Applied Clay Science xxx (2016) xxx-xxx
Table 4 displays the results of the determination of potentially
toxic metals in the leaching extracts of the 10 wt% incorporated in-
dustrial brick. Regarding to all investigated metals and compounds,
the incorporated brick fulfill the standard requirements According to
Brazilian standard for solid residue classification (ABNT, 2004a), the
brick produced with 10 wt% of paper sludge, when transformed into
a demolition residue, will be classified as non-dangerous and non-in-
ert. Therefore, in principle, clay bricks incorporated with 10 wt% of
paper sludge can be recycled after service life in Brazil. However, in
European countries lower incorporated values should be considered to
attend the legislation (Khler, 1988).
3.4. Saving in energy
In the decade-long Spanish industrial experience of paper sludge
incorporation into clay bricks, Cusid et al. (2015) mentioned that ad-
dition in clay takes advantage of a 3% contribution of energy obtained
from organic matter in the sludge. Even though this fuel saving could
be within the operational variation of the kiln, it is worth mentioning
as a value similar to that found in the present note.
In the current Brazilian case, the paper sludge from COPAPA
was found (ISO standards conditions of 15 C, 1.013 bar of pressure
and 60% of relative moisture) to have an average wet heat power
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of 1100 kJ/kg. The Rodolfo Gama ceramic industry uses eucalyp-
tus wood at a cost of about US$ 40/ton and a wet heat power of
11,000 kJ/kg. The modified Dome kiln of the ceramic industry con-
sumes around 3.8 106 kJ of firing energy from wood (pile seen
in the bottom left side of Fig. 1(a)), to fabricate 1000 kg (1 ton) of
clay bricks, Fig. 1(b). If the paper sludge is being incorporated in an
amount of 10 wt% (100 kg per ton) the sludge is contributing with
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1100 kJ/kg 100 kg = 110,000 kJ.
This simple evaluation indicates that, in principle, the industrial
incorporation of 10 wt% (wet) paper sludge from COPAPA is sav-
ing 110,000 kJ/3.8 106 kJ = 0.029, i.e., about 3% in firing energy
for the ceramic industry. This value is surprisingly similar to that for
Spanish industries, as reported by Cusid et al. (2015), in spite of
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different types of kilns and the fact that 3% saving might be within
the operational variation of any particular type of kiln. Neverthe-
less, this energy saving could represent an economy of 110,000 kJ/
11,000 kJ/kg = 10 kg of wood per ton of paper sludge incorporated
ceramic. By considering a production of 36,000 tons/year of bricks
added with paper sludge in the aforementioned Brazilian ceramic, a
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total of 360 tons of wood would be saved every year, corresponding to
360 40 = 14,400 dollars/year.
Different from Europe, where fossil fuels are mainly used for fir-
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ing, wood from natural forest is still used as fuel in Brazil. There-
fore, the incorporation of paper sludge in wood fired clay ceramics is
an environmental benefit by contributing to preserve Brazilian forests
Table 4
Potentially toxic elements in the solution extract of the incorporate ceramic.
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Toxic element content Maximum allowed limit (mg/L)
Parameter (mg/L) (CONAMA, 2002)
Aluminum 0.189 0.2
Total 0.050 0.05
chromium
Iron 0.175 0.3
Manganese 0.012 0.1
Zinc < 0.004 5.0
Surfactants < 0.031 0.5
Cyanides < 0.005 0.07
Fluorides < 0.210 1.5
that absorb CO2 responsible for global warming. Furthermore, a theo-
retical prediction of costs based on weight rationalized embodied en-
ergy (kWh/kg), used as a parameter (Manfredini and Sattler, 2005;
Monteiro and Vieira, 2014; Yohanis and Norton, 2002; Zhang, 2013)
revealed significant economical advantages of the Brazilian industrial
case. Indeed, Manfredini and Sattler (2005) indicated that clay bricks,
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depending on the country, are associated with different parameter.
For instance, 1.361 kWh/kg in North America and 0.379 in Campos
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dos Goytacazes, Brazil. As a simple theoretical comparison, based on
the cost of industrial energy of US$ 0.106 per kWh in Brazil (EBC,
2015) and US$ 0.064 in the United States (EIA, 2016), one thousand
of paper sludge added clay bricks fabricated in Campos dos Goyta-
cazes would cost 0.379 106 = US$ 40.20, while in the US might
cost 1.320 64 = US$ 84.5, which is more than twice the price in
Brazil. By contrast, one thousand concrete bricks with a parameter of
1.5 kWh/kg (Zhang, 2013), usually produced in the US for building
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construction, would cost 1.5 64 = US$ 94. This is more expensive
than possible clay bricks added with paper sludge if ever fabricated in
the US.
As a final remark, this Brazilian industrial experience might be re-
garded as a local contribution to the world state of the art on the in-
corporation of paper sludge into clay bricks, which started in Germany
and Italy as well as other European countries. Relatively lower fir-
ing temperature (750 C), appropriate blend of clays, easy-controlled
dome type of kiln and overall cost saving are the contributions of the
present reported experience.
4. Conclusions
Industrial-scaled addition of 10 wt% (wet) paper sludge into clay
body as a mixture of two distinct clays, followed by firing at
750 C, disclosed an accepted compression strength for civil con-
struction, according to Brazilian norms.
Evaluation of atmospheric emission attested SO2, NOx, TOC, CO
and particulates within established limits by legislation. Solution
tests attended specifications and indicates that clay brick addition is
an environmentally correct solution for the large industrial genera-
tion of Brazilian paper sludge.
Similar to the European state of the art, this Brazilian indus-
trial-scaled experience of paper sludge addition into clay bricks,
probably the first case in the Americas, revealed an energy saving
of 3%. The theoretically estimated cost of sludge added clay bricks
is significantly lower in Brazil and, if fabricated in the US, would
be even lower than concrete bricks.
Uncited references
Banfill and Frias, 2007
Ducman and Kopar, 2007
Acknowledgements
The authors thank the Brazilian agencies CNPq, proc. 302930/
2014-0, CAPES and FAPERJ, proc. E-26/201.192/2014 for support-
ing this research. The authors are also thankful to the facilities pro-
vided by the Rodolfo de Azevedo Gama Ceramic and COPAPA in-
dustries.
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