Ceramics International 48 (2022) 10506–10515

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Ceramics composites from iron ore tailings and blast furnace slag
Luana Cechin *, Vsévolod Mymrine, Monica A. Avanci, Ana Ester Povaluk
UTFPR, Federal Technological University of Paraná, Deputado Heitor Alencar Furtado Street, 4900, Curitiba Campus, CEP 81280-340, Ecoville, Paraná, Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: The search for materials and methods capable of reducing human impacts on the environment is of utmost
Iron ore tailings importance nowadays. This study’s primary purpose was to analyze the technical feasibility of ceramic com­
Charcoal blast furnace slag posites production utilizing Fundão Dam’s Iron Ore Tailings (IOT), Blast Furnace Slag (BFS) from charcoal, and
Foundry sand
Foundry Sand (FS) as partial substitutes for the traditional raw materials – sand and clay – for application in
Ceramic composites
Sustainable materials
building industry materials. The composites were molded in rectangular specimens and fired at temperatures of
900, 950, 1000, 1050, and 1200 ◦ C. The developed materials were analyzed and characterized by X-Ray
Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), Thermog­
ravimetry (TGA), and Differential Thermal Analysis (DTA). The obtained materials had flexural strength modulus
of up to 12.19 MPa, water absorption ranging from 2 to 22%, linear shrinkage ranging from 0.02 to 6.50%, and
apparent density ranging from 2.03 to 1.63 g/cm3. The study of the internal structure formation process revealed
the formation of amorphous structures in the composites. The results demonstrated that these waste materials
may be jointly used in construction materials, contributing to the reduction of natural resource extraction, be­
sides enabling their correct disposal, minimizing environmental impacts, and improving the life quality of the
surrounding communities.

1. Introduction industrial activities led to an increase in pollution impact on our planet

[4]. For example, the iron production and the foundry industry
Civil construction is one of the economic sectors which exerts respectively generate Blast Furnace Slag (BFS) and Foundry Sand (FS).
enormous influence on Brazil’s development, creating new technologies Besides, the mining industry is a leading producer of by-products and
and generating income and jobs [1]. However, despite its social and industrial waste.
economic contributions, this is also one of the sectors that most degrade The mineral extraction industry is an important contributor to Bra­
the environment. On a global scale, it consumes up to 40% of the total zil’s gross domestic product. In the first quarter of 2020, the share of iron
energy production, 12–16% of all available water, 32% of renewable ore corresponded to 66.00% of exports by the mining industry. And in
and non-renewable resources, 25% of wood, 40% of all raw material, the first half of 2020, the states with the highest tax revenue from
generates 30–40% of all solid waste, and emits 35% of CO2 [2]. financial compensation for the exploration of mineral resources were
As an example, there is the ceramic tile supply chain, where several Pará and Minas Gerais, which are the largest iron ore producers in Brazil
environmental impacts are generated from the raw material extraction [5].
stage to the industrial process, marketing, consumption, maintenance, Mineral extraction generates a large volume of waste. The demand
and placement of the final product. These environmental impacts are for large deposition areas, the potential for soil contamination, surface
related mainly to the atmospheric emissions incidence – dust particles and underground water and the risk of dam failure are capable of
and gas –, high energy consumption, use of materials with toxic sub­ causing environmental and social damage and are some of the problems
stances, emission of polluting liquids, generation of solid waste, and associated with the extraction and processing of iron ore. Its storage, in
improper disposal of packaging and finished products [3]. addition to its high cost, generates significant environmental liabilities
Moreover, due to various industrial wastes, global environmental and presents a high risk of accidents [6].
pollution continues to grow, despite advances in nature protection In 2015, the Fundão tailings dam at Samarco iron mine, located in
legislation. The world population increase and the waste production by Mariana (BR), collapsed. This incident launched billions of liters of

* Corresponding author.
E-mail address: [email protected] (L. Cechin).

https://doi.org/10.1016/j.ceramint.2021.12.260
Received 13 October 2021; Received in revised form 12 December 2021; Accepted 24 December 2021
Available online 30 December 2021
0272-8842/© 2021 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
L. Cechin et al. Ceramics International 48 (2022) 10506–10515

sludge from iron ore processing tailings, which destroyed the entire In addition, raw materials’ semi-quantitative chemical character­
Bento Rodrigues district, reached the mouth of Doce River and the ization was carried out by X-Ray fluorescence spectroscopy (FRX) in a
Atlantic Ocean, and left 19 dead. More recently, on January 25th of Malvern Panalytical Axios-mAX spectrometer, and the ceramic com­
2019, Feijão brook mine’s dam, owned by the Vale mining company, posites were characterized regarding flexural strength module, water
located in Brumadinho (BR), collapsed, pouring a mudflow that absorption, linear retraction, and density.
destroyed the nearby communities and Vale’s buildings. This accident
killed over 240 people and contaminated the Paraopeba River, one of 2.3. Raw materials’ description
São Francisco River’s tributaries.
Mining operations must be conducted in a sustainable, economically 2.3.1. Raw materials’ chemical composition
viable, and socially acceptable manner [7]. Waste management tech­ IOT mainly contained two primary components – SiO2 (58.6%) and
nologies should be embraced, including the reuse of tailings and other Fe2O3 (35.4%) (Table 1). It also presented small quantities of Al2O3
residues [8]. Iron Ore Tailing (IOT) is a thin, dense, stable, and crys­ (3.2%), alkali metal oxides (Na2O and K2O), and alkaline-earth metal
talline material, composed mainly of iron oxides, silica, and alumina, oxides (CaO and MgO), with a low loss on ignition (LOI).
presenting no risks regarding its use [9–12]. Being a metallurgical process by-product, the BFS presented high
IOT has been successfully employed in cement-based composites levels of SiO2 (39.7%), alkaline earth metals (CaO – 32.8% and MgO –
[10–16]. Furthermore, its chemical-mineralogical constitution suggests 7.2%), and Al2O3 (12.9%), with small amounts of alkaline metals (Na2O
its use in ceramic parts and as a partial replacement for conventional and K2O) and Fe2O3 (Table 1).
raw materials and natural aggregates [10, 14, 16, 17]. FS had a high level of SiO2 (91.2%) and lower contents of Al2O3 and
Granulated BFS is an industrial residue discarded during the iron and Fe2O3 (2.3% and 1.2%, respectively) (Table 1). The Al2O3 content might
steel smelting process, created by the combination of iron ore and be explained by the contact with the clay from the factories’ molds, and
limestone. After smelting at high temperatures, from 1400 to 1600 ◦ C, it Fe2O3 presence is due to the sand’s composition itself. LOI value of 3.7%
is cooled quickly using water, forming granular particles [18]. can be attributed to improper storage of material after its use, having
The slag volume varies according to the raw materials used in the remained outdoors in the factory yard.
production of pig iron; typically 300 kg of blast furnace slag is produced NC was formed by SiO2 (53.3%), Al2O3 (24.7%), and Fe2O3 (6.1%),
per ton of pig iron. According to Companhia Siderúrgica Nacional (Rio with a LOI of 11.5% (Table 1). This value was due to the high organic
de Janeiro, Brazil) the amount of this waste produced is approximately material content in its composition.
1.2 million tons per year. Thus, like iron ore waste, the use of this ma­
terial is a matter of continuing concern for economic and ecological 2.3.2. Raw materials’ mineralogical composition
reasons [19]. Granulated BFS can be used as a binder in the production Quartz (SiO2) is the most widespread mineral in the Earth’s crust,
of alkali-activated cement and ceramic composites[20–26]. and for this reason, it was found in all the raw materials studied,
The use of iron ore tailings and blast furnace slag in construction can differing in amounts (Fig. 1, Table 2). IOT exhibited magnetite, hema­
be considered an effective alternative to deal with the large volume of tite, and goethite as its main minerals (Fig. 1a). BFS displayed an
waste generated and to reduce the consumption of natural resources and amorphous structure (Fig. 1b). The main minerals in FS were cristobalite
non-renewable resources, as it allows the reintroduction of these wastes. and bentonite (Fig. 1c), and in NC, kaolinite and montmorillonite
In other production chains, such as civil construction. (Fig. 1d).
Ergo, the IOT and BFS reuse in civil construction is an advantageous
alternative, which brings us this study’s main purpose, i.e., to analyze 2.3.3. Raw materials’ morphological structure
the technical feasibility of ceramic composites production with the IOT’s SEM photomicrograph at 2.00 kx magnification presented
addition of iron ore tailings and blast furnace slag. different particle sizes with irregular porous fractured surfaces (Fig. 2a).
BFS particles exhibited a wide variety of sizes and shapes, including
2. Materials and methods sharp edges (Fig. 2b), probably due to the material preparation process
(during its grinding and crushing). FS had rounded grains with minor
2.1. Materials surface damage (Fig. 2c). The imperfections only became evident with
the increase in magnification. This occurrence might be related to the
All residues and the Natural Clay (NC) used in this research are thermal shock given to the sand when it was used as a mold, which was
representative samples selected in Brazil. IOT was gathered after the around 1300 ◦ C (Fig. 2d). NC showed a smooth surface with cracks and
Fundão Dam rupture in Mariana, Minas Gerais, and the charcoal BFS rounded grains of different sizes spread over it (Fig. 2e).
was collected in a steelworks company from Belo Horizonte. FS and (NC)
were respectively supplied by a foundry company and a brick factory in 2.3.4. Raw materials’ thermochemical characterization
Curitiba. IOT’s TGA and DSC thermograms (Fig. 3a) showed 3 characteristic
All raw materials were oven-dried at 105 ◦ C for 24 h, then cooled at peaks of the material. The first peak, at 47 ◦ C, demonstrated a 1.4%
room temperature. Also, blast furnace slag was crushed in a pot spray weight loss due to the loss of free water. The second peak, at 299 ◦ C,
mill to reduce its granulometry. coincided with the goethite little crystallized’s (FeO(OH)) dehydrox­
ylation, turning into hematite. At a temperature of 496 ◦ C, a 1.1%
2.2. Methods weight loss was observed, which was related to kaolinite dehydrox­
ylation (Al2Si2O5(OH)4).
The raw materials and the ceramic composite 6 were characterized FS’ DTA thermogram showed a thermochemical process and a 2.3%
by XRD to analyze their mineralogical compositions in a Malvern Pan­ weight loss stage (Fig. 3b). This occurrence may be related to organic
alytical Empyrean diffractometer, with an X’Celeratore detector using λ additives, customarily used as binders, and plasticizer additives, used in
Cu-Kα. Morphological structures were studied by SEM in a Zeiss mi­ the foundry factory before the FS was stored as waste.
croscope, model EVO MA 15, and the chemical composition was NC’s DTA curve displayed 3 endothermic processes, except at 478 ◦ C,
analyzed by EDS in an Oxford Instruments X-Max spectrometer. Ther­ where the heat flow indicated an exothermic process corresponding to
mochemical characterization (TGA for weight changes and DSC for heat the weight loss at this temperature (Fig. 3c). The TGA presented a 1.8%
flow) was conducted on a TA Instruments Simultaneous Thermal weight loss at 54 ◦ C, mainly because of water evaporation. The second
Analyzer, model SDT Q600, in a nitrogen atmosphere, with a heating process occurred at 245 ◦ C due to the removal of hygroscopic water and
rate of 10 ◦ C/min. organic matter from montmorillonite, with a 1.6% weight loss (Fig. 3c).

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Table 1
Raw materials’ chemical composition in % (XRF).
Fe2O3 SiO2 Al2O3 SO3 CaO MgO Na2O K2 O LF*

IOT 35.4 58.6 3.2 <0.1 0.1 0.1 0.1 0.2 2.19
BFS 2.6 39.7 12.9 0.1 32.8 7.2 0.1 0.7 2.35
FS 1.2 91.2 2.3 0.7 0.1 0.2 0.3 0.1 3.70
NC 6.1 53.3 24.7 0.1 0.4 0.7 0.1 1.0 11.5
*
LOI: Loss on Ignition.

Fig. 1. – Raw materials’ mineralogical composition (XRD): a) IOT, b) BFS, c) FS, d) NC.

2.4. Composites preparation

Table 2
– Raw materials percentages in the developed composites.
Seven compositions were set based on each material’s properties
Composite Composition (%) (Table 3).
IOT BFS FS NC After defining the compositions, the test specimens (TS) were molded
1 0 0 20 80
at 60x20 × 10 mm, compacted at a 4 MPa pressure, and oven-fired at
2 0 0 15 85 900, 950, 1000, 1050, and 1200 ◦ C. Five TSs were made for each
3 25 45 10 20 temperature.
4 40 20 20 20
5 15 25
2.4.1. Flexural strength module
6 10 30
7 45 25 10 20 When developing ceramic composites, a practical application was
adopted for them, that is, they should meet the minimum requirements
for ceramic tiles according to the Brazilian Regulatory Standard (NBR)
The peak located at 478 ◦ C denoted a weight loss of 7.3% that repre­ 13818 [29]. For this standard, two main physical characteristics must be
sented kaolinite dehydroxylation and the beginning of the trans­ observed in ceramic coverings: the water absorption and the flexural
formation into metakaolinite (Fig. 3c). According to Dweck [27], strength module. The flexural strength module refers to the strength of
montmorillonite dehydroxylation occurs between 405 and 685 ◦ C, the the ceramic material, allowing the analysis of the internal cohesion of
variation depending on the presence of associated minerals. The last the material. The flexural strength module of the samples was calculated
process, observed at the DTA curve at 1075 ◦ C, revealed a 1.8% weight according to NBR 13818 [29]:
loss, attributed to mullite crystallization, formed from metakaolinite
(Fig. 3c) [28]. 3*F*L
σ= (Eq. 1)
BFS had no significant losses until 1200 ◦ C; therefore, the graph of 2*b*d2
thermochemical characterization was not stated. Where F = applied force (N), L = distance between the two outer sup­
ports (mm), b = sample width (mm), d = sample thickness (mm).

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Fig. 2. –SEM photomicrograph of a) IOT at 2.0 kx magnification; b) BFS at 2.0 kx magnification; c) FS at 100x magnification; d) FS at 10 kx magnification; and e) NC
at 2.0 kx magnification.

2.4.2. Water absorption

MU − MS
Water absorption is the property of the ceramic material to absorb A% = *100 (Eq. 2)
MS
water, this is a direct function of the porosity and permeability of the
ceramic piece, in general, the results of the water absorption test Where MU = sample mass after 24 h of water immersion (g), MS =
correlate with the presence of pores and the formation of similar sur­ sample mass before water immersion (g).
faces to the glass. The water absorption was determined using the pre­
mises of NBR 13818 [29]: 2.4.3. Linear retraction
The linear shrinkage of ceramic pieces is directly linked to their

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Fig. 3. – DTA, TGA, and DSC of a) IOT; b) FS; and c) NC.

Table 3
– Chemical composition of composite 6 sintered at 1200 ◦ C (by EDS).
Points Na Mg Al Si K Ca Ti Mn Fe

1 0.37 2.33 20.81 60.42 5.02 4.87 0.98 0.34 4.85

2 0.00 0.00 0.00 99.02 0.00 0.00 0.00 0.00 0.98
3 0.00 0.00 1.36 95.96 0.45 0.64 0.00 0.00 1.58
4 0.00 0.00 0.00 98.78 0.00 0.00 0.00 0.00 1.22
5 0.42 7.12 13.64 58.01 1.93 11.96 0.29 0.47 6.17
6 0.00 0.00 0.00 98.99 0.00 0.00 0.00 0.00 1.01
7 0.51 2.27 13.03 63.19 0.44 11.24 0.37 0.00 8.96

porosity, that is, the lower their porosity, the lower their coefficient of
M
linear shrinkage. The linear retraction coefficient was calculated ac­ d= (Eq. 4)
a*b*c
cording to the equation:
Lb,f − La,f . Where M = mass of dried sample after firing (g), a = sample length (cm),
CL = *100 (Eq. 3) b = sample width (cm), c = sample thickness (cm).
Lb,f .

Where Laf = sample length after firing (mm), Lbf = sample length before 3. Results and discussions
firing (mm).
3.1. Ceramic composites mechanical and physical properties
2.4.4. Apparent density
The apparent density is linked to the degree of closure of the pores 3.1.1. Flexural strength module
present in ceramic pieces, that is, the more monolithic the ceramic An increase in flexural strength module with the temperature rise
structure, the more compact the structure and the greater its apparent from 1050 to 1200 ◦ C (Fig. 4) was observed for all composites, except
density. The density was determined by the equation: composites 3 and 7, that melted at this transition temperature. This

Fig. 4. – Composites’ flexural strength module for all firing temperatures.

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phenomenon happened probably due to the high percentage of SiO2, above 2.5% at 1200 ◦ C. Composite 5, for instance, shrank 0.04% at 900
Fe2O3, and Al2O3 in all raw materials, as these oxides have a high ◦
C and 4.14% at 1200 ◦ C, evidencing the temperature’s influence on the
melting point – 1728, 1591, and 2038 ◦ C, respectively. TS′ retraction. Likewise, composite 6 displayed a steady growth of linear
Composites 1 and 2, which had no IOT and BFS in their composition, shrinkage between 1050 and 1200 ◦ C, increasing nearly 15 times, from
presented a slight increase in flexural strength modules between the 0.31% to 4.54%.
temperatures previously mentioned, while composites 4 to 6 had a sig­ In general, a tendency is noticed in the developed composites: an
nificant increase. It was observed that by increasing IOT content, there increase in linear shrinkage with growing temperature caused by a more
was a reduction in the flexural strength module. A similar effect was effective sintering process. Besides, BFS acted as a stabilizer for the
found by Mymrin et al. [30], where water treatment sludge with high composites.
content of natural organic materials was used to produce red ceramic.
IOT, FS, and NC showed low contents of alkali metal oxides (Na2O e 3.1.4. Apparent density
K2O) or alkaline earth metals (CaO e MgO), which are more effective in There was no significant variance in the apparent density regarding
liquid phase formation, reducing TSs firing temperature and porosity; the firing temperature growth for composites 1 and 2 (Fig. 7), as noted
therefore, adversities were found in TSs densification as observed in for composite 2, which presented 1.63 g/cm3 at 900 ◦ C and 1.68 g/cm3
research by Dias et al. [31] and Fontes et al. [11]. at 1200 ◦ C.
Comparing the composites’ flexural strength module values with All composites maintained a constant density until 1050 ◦ C. Thereon
NBR 13818 showed that only composite 6 reached the minimum of 12 composites 4 to 6 had a density boost at 1200 ◦ C due to the sample’s
MPa required by the standard. densification with the rising temperature.

3.1.2. Water absorption

3.2. Physicochemical processes of ceramic structure formation
Water absorption is an important property, especially in roof tile
production, for the material should not absorb too much water. Gener­
Composite 6 was selected to analyze the developed ceramic structure
ally, water absorption test results are related to the presence of pores and
formation’s physicochemical processes for presenting better results. It
the glass-like surface formation. All developed composites had water
exhibited the highest flexural strength modules for almost every firing
absorption higher than 10% for temperatures under 1050 ◦ C (Fig. 5).
temperature (Fig. 4), the highest apparent densities (Fig. 7), and one of
However, TSs of composites 4 to 6 at a firing temperature of 1200 ◦ C had
the lowest water absorption coefficients at 1200 ◦ C (Fig. 5). Further­
2% water absorption, indicating a probable formation of less porous
more, this was the only composition that presented the minimum flex­
structures, which directly influenced their flexural strength module
ural strength modulus required by NBR 13818 (12 MPa) [29], allowing
(Fig. 5).
the use of this composition for the production of ceramic tiles.
3.1.3. Linear shrinkage coefficient
3.2.1. Mineralogical composition of composite 6 during the firing process
Linear shrinkage is strongly influenced by the firing temperatures as
Composite 6’s diffractogram (Fig. 8) exhibited quartz (SiO2) and
well as the ceramic composition. The TS initial length of 60 mm and the
mullite (Al4.5Si1.5O9.75) at 900 ◦ C. After its firing, there was an increase
TS length after firing were considered for its calculation.
of quartz and mullite crystalline peaks, formation of hematite (Fe2O3),
Composites 1 and 2 presented the highest linear shrinkage values for
and structural modification of quartz into cristobalite (SiO2). The
all analyzed temperatures, with composite 1 going from a 2.14%
background is above several crystalline peaks for both 900 and 1200 ◦ C,
shrinkage at 900 ◦ C to 4.32% at 1200 ◦ C (Fig. 6). This evidence might be
indicating the predominance of amorphous phases in the composite.
explained by the fact that natural materials such as NC have a higher
Nevertheless, for these temperatures, there is still quartz and mullite.
content of organic components, carbonates, hydrates, and other ther­
This evidence is probably due to the crystalline phases’ structural
mally unstable elements in their composition.
changes, where kaolinite, around 500 ◦ C, turns into metakaolinite,
Composites 4 to 6, on the other hand, exhibited a linear shrinkage
which later transforms into mullite and cristobalite in a process that

Fig. 5. – Composites’ water absorption for all firing temperatures.

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Fig. 6. – Composites’ linear shrinkage coefficient for all firing temperatures.

Fig. 7. – Composites’ apparent density for all firing temperatures.

initiates around 900 ◦ C, reaching its reaction apex at 1300 ◦ C. Moreover, this pore closure increased the density and linear shrinkage,
At 900 ◦ C, the presence of hematite from the IOT was not verified in significantly reducing the water absorption rate.
the composite. However, at 1200 ◦ C, hematite peaks were observed,
probably due to the increase in temperature and the fact that this min­ 3.2.3. Composite 6’s chemical composition after sintering at 1200 ◦ C (by
eral’s peaks have intensity below the sensitivity of the XRD method EDS)
(5%). The carbon element might be related to the stub, and the oxygen
element might have formed oxides with all the elements presented.
3.2.2. Morphological structure of composite 6 Therefore, both elements were disregarded in this analysis.
A comparison of the morphological structures of composite 6 was There was significant heterogeneity between the contents of the
performed, at the firing temperatures of 900 and 1200 ◦ C, obtained by same element at each analyzed point (Table 3), such as seen for Si, which
the SEM method at 500X and 2000X magnification (Fig. 9). There was a displayed a maximum of 99.02% and a minimum of 58.01% content,
reduction in the existing pores in the composite due to its melting, indicating an amorphous structure. Likewise, EDS exhibits every
making the structure almost monolithic. This condition directly influ­ element in the composition of the raw materials: IOT, BFS, FS, and NC,
enced the specimens’ flexural strength module, which exhibited 1.34 corroborating the results presented by the XRD of composite 6 (Fig. 8),
MPa at 900 ◦ C and 12.19 MPa at 1200 ◦ C, increasing nearly ten times. where the main elements were Si, Al, and Fe.

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Fig. 8. – Diffractogram of Composite 6 after sintering at (XRD): a) 900 ◦ C, and b) 1200 ◦ C.

Fig. 9. – Morphology of composite 6 by SEM after sintering at.

3.2.4. Thermochemical characterization of composite 6

Considering the presence of the four raw materials in composite 6, it
could be verified an interaction between the thermochemical processes
discussed in section 2.2.4, altering some stages of weight loss and their
occurring temperatures (Fig. 10).
The first endothermic process took place at 46 ◦ C with a weight loss
of 0.67%. This stage represented water evaporation, which also was
exhibited for IOT, FS, and NC at 47, 44, and 45 ◦ C, respectively.
The second endothermic process occurred at 243 ◦ C due to the
removal of hygroscopic water and organic matter from montmorillonite,
with a weight loss of 1.1%. This process can be seen in NC at 245 ◦ C with
a weight loss of 1.6%.
A third endothermic process was observed at 299 ◦ C and corre­
sponded to the dehydroxylation of the little crystallized goethite (FeO
(OH)), which turned into hematite. The weight loss was 2.7%, and this
process can be verified for IOT at the same temperature with a loss of
0.6%.
There was also a last endothermic process at 458 ◦ C with a weight
Fig. 10. –Composite 6’s thermogram (DTA, TGA, and DTG).

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loss of 1.1%, related to mullite crystallization formed from meta­ [6] C.F. Morais, B.R. Belo, A.C.S. Bezerra, R.M. Loura, M.P. Porto, S.A.L. Bessa,
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Declaration of competing interest
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