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Construction and Building Materials 367 (2023) 130256

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Construction and Building Materials


journal homepage: www.elsevier.com/locate/conbuildmat

Technological and microstructural perspective of the use of ceramic waste


in cement-based mortars
Mariana Gomes Pinto Cherene a, *, Gustavo de Castro Xavier b, Laimara da Silva Barroso a,
Jheyce de Souza Moreira Oliveira b, Afonso Rangel Garcez de Azevedo b,
Carlos Maurício Vieira a, Jonas Alexandre b, Sergio Neves Monteiro c
a
Laboratory of Advanced Materials, State University of the Northern Rio de Janeiro, Rio de Janeiro 28013-602, Brazil
b
Civil Engineering Laboratory, State University of the Northern Rio de Janeiro, Rio de Janeiro 28013-602, Brazil
c
Department of Material Sciences, Military Engineering Institute, Rio de Janeiro 22290-270, Brazil

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

Keywords: The construction sector is constantly growing and, consequently, the increase in the use of building materials. In
Construction sector view of this, the red ceramic industry is responsible for a large amount of waste, through failures in its process
Building materials and thus generating defective parts. Therefore, this work aims to reuse these wastes generated by the red ceramic
Red ceramics
industry in mortars, as a partial substitute for natural sand. The ceramic waste was ground in a crusher mill-type
Ceramic waste
Mortar
crusher for one hour. Mortars were made, in the mix proportion 1:6 (cement: sand) in mass, replacing the sand
with ceramic waste in replacing of 10, 20 and 30% and the mixture reference (0%), using the ordinary portland
cement. The mortars were subjected to tests of workability, water retention, density, incorporated air content,
density in the hardened state, water absorption, flexural strength in bending and compressive strength. Soon
after, microstructural characterization techniques were performed in mixtures, such as isothermal calorimetry,
mercury intrusion porosimetry and X-ray diffraction. The results show that the mixture with 10% improved the
flexural strength in bending and compressive strength, indicating a lower coefficient of capillarity, as they have
fewer pores and a greater amorphous halo. The ceramic waste caused an increase in density in the fresh and
hardened state and a decrease in the content of incorporated air. In the mixtures with 20% and 30% of ceramic
waste, there was a loss in the properties, mainly in the strength. Therefore, the most satisfactory mixtures were
with 10% ceramic waste.

1. Introduction the atmosphere also grows, being responsible for up to 20 % of the total
emission of CO2 [5].
The population has gone through great challenges of how to This fact can be reflected in environmental concerns, where indus­
correctly discard everything that it generates and reuse everything that trial production is high, with greater associated impacts, whether by
has no final destination. In the last years the world production of extraction of raw materials, atmospheric emissions or eventual genera­
different types of ceramic tiles was around 13.7 billion m2 [1]. Typically, tion of waste [5,6].
about 30 % of the materials in the ceramic industry are wasted. In Brazil, In this way, the destination of waste is, therefore, one of the main
ceramics are responsible for 10 % of the production loss [2], which is problems that the world faces today, whether for economic, political or
often improperly deposited, generating some types of contamination, ecological reasons. In recent years, waste recycling has been encouraged
which can be transformed into raw material and solve many industrial as one of the most effective alternatives to reduce the impact of large-
problems [3,4]. scale extraction of raw materials and waste [7,8].
In recent years, due to the development of cities and easy real estate An alternative is the incorporation of waste in construction mate­
investments, there has been a growth in demand for fence blocks rials, which has great potential to minimize environmental impacts,
(bricks). With the increase in civil construction, the emission of CO2 in reduce the amount of waste to be discarded, which most of the times

* Corresponding author.
E-mail address: marianagpc1@yahoo.com.br (M.G.P. Cherene).

https://doi.org/10.1016/j.conbuildmat.2022.130256
Received 23 August 2022; Received in revised form 6 December 2022; Accepted 27 December 2022
Available online 12 January 2023
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

In this way, the partial replacement of materials in civil construction


has grown continuously, in addition to the great environmental
advantage, with the reuse and correct destination of materials, and can
still achieve an equivalent or even better performance in mortars
[12,14].
Several studies evaluated the partial replacement of sand and OPC by
ceramic waste in mortars, such as Cabrera-Covarrubias et al. (2016),
Gayarre et al. (2017) and Mohit and Sharifi (2021). The researchers
concluded that the addition of residue increases the flexural strength in
bending and compressive strength and decreases the porosity of the
mortars, that is, the residue behaves as a filler effect. In the present
study, the partial replacement of sand by ceramic waste in order to use a
larger amount of waste, will be evaluated and lime was not used, due to
its high commercial cost.
In this context, it is emphasized that the main objective of this work
is to evaluate the application of ceramic waste as a partial substitute for
sand, evaluating through workability, water retention, density, incor­
porated air content, density in the hardened state, water absorption,
flexural strength in bending and compressive strength, isothermal
Fig. 1. Waste in the ceramics yard.
calorimetry, mercury intrusion porosimetry (MIP) and X-ray diffraction
(XRD). Most authors use the ceramic waste as a supplement. Further­
remain in the yards without use (Fig. 1) and correct final destination,
more, in Brazil there is only one metakaolin company located in the state
once the waste of one process becomes the input of another, and can also
of São Paulo, far from other regions of the country. The region of the
act as a reduction in production costs, either by saving energy or raw
municipality of Campos dos Goytacazes has a predominance of kaolin­
materials [9].
itic mineral clay, the company researched burns its ceramic bricks be­
In this way, the recycling of any type of waste always brings unde­
tween 600 and 630 ◦ C and turns into metakaolinite, presenting great
niable benefits, reducing the environmental problems that often result in
potential in the region, which has around 100 ceramics [18].
the deposit of these materials in landfills, saving natural resources and
promoting sustainability. The grinding of ceramic waste into fine par­
2. Materials and methods
ticles gives rise to fine aggregates, which can partially replace natural
sand or ordinary portland cement (OPC) and thus contribute to reducing
The ceramic waste used in this research was collected from a ceramic
the extraction of raw mineral, with a great impact on the environment
industry located in the municipality of Campos dos Goytacazes. This
[10].
waste was obtained from the disposal of ceramic blocks that went
In this context, as part of the civil construction chain, the red ceramic
through the firing process at temperatures between 600 ◦ C at 630 ◦ C
industry in Brazil is of great importance, accounting for about 4.8 % of
[19,20]. Soon after, the ceramic waste was properly crushed in a ball
the national industrial production, with about 7400 industries, due to
mill, which contains about 9 steel balls with a diameter of 40 mm for
the expressive national production of ceramic blocks, has great influ­
each 5 kg of waste, with rotation at 750 rpm for 1 h. After this process,
ence. In addition, there is the cultural factor, indicating that ceramic
both the waste and the sand were passed through an 8x2 stainless steel
blocks are still consumer preference in most regions [3,11].
granulometric sieve, 0.85 mm opening, 20 mesh, thus disregarding the
Ceramic blocks can show pozzolanic activity because it is a pre­
effect of moisture on the materials for making the mortars, and properly
dominantly kaolinitic material (Al2O3.2SiO2), they can also be classified
dried in an oven (110 ◦ C for 24 h). The appearance of the ceramic waste
as pozzolan if the total of SiO2 + Al2O3 + Fe2O3 was greater than 70 %,
at each stage is shown in Fig. 2.
as it can also present only filler effect [12]. The pozzolanic reactivity is
Table 1 presents the results of the Chemical Analysis by X-ray
essentially conditioned by the amount of amorphous silica and alumina
Fluorescence (FRX) of the ceramic waste and cement, equipment used
available for the reaction with calcium hydroxide [13].
para análise was Rigaku Primi with a palladium X-ray source, showing

Fig. 2. Ceramic waste process: (a) Ceramic waste (b) Milling (c) Post grinding.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Table 1
Proportions.
Elements SiO2 Al2O3 Fe2O3 K2O MgO CaO P2O5 SO3 Cl

Ceramic waste (%) 51,85 29,37 12,89 2,43 0,79 1,07 0,40 1,10 0,11
Cement (%) 15,75 4,42 4,760 0,97 1,07 67,62 0,39 4,88 0,14

Fig. 3. Result of XRD test of ceramic waste and cement, M (mica); Q (quartz); H (Hematite); F (Feldspar); G (Gypsum); A (C3S); B (C2S); C (C3A).

that the ceramic residue is mainly composed of silica (51.85 %) and their sum represents almost 80 %, also presenting other elements such as
alumina (29.37 %). It also has other elements such as iron oxide, po­ alumina, iron oxide, potassium oxide, magnesium oxide, silver oxide,
tassium oxide, magnesium oxide, calcium oxide, silver oxide, phos­ phosphorus pentoxide, sulfuric oxide and chloride [17,23,24].
phorus pentoxide, sulfuric oxide and chloride [3,12,17,21,22]. There is Fig. 3 shows the results found by X-ray Diffraction of ceramic waste
also a high percentage of iron oxide that gives the reddish color to the and cement. The X-ray Diffraction (XRD) was performed in a Proto
blocks that gave rise to the ceramic waste. The composition of Portland Manufacturing AXRD Powder Diffraction System diffraction meter
cement has silica and calcium oxide as the main components, where operating with a voltage of 30 kV, current of 20 mA and Cu-Kα radiation,

Fig. 4. Granulometry curve of the ceramic waste and sand.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Table 2 (natural sand) [22].


Proportions. Mortars were made with a ratio of 1:6 (cement: sand) [30,31]. The
Mixtures OPC (g) Sand (g) Ceramic waste (g) partial replacement of sand by ceramic waste was used in different
proportions (0, 10, 20 and 30 %) [32], with the use of OPC, according to
CPV00 286 1710 –
CPV10 286 1540 171 Table 2.
CPV20 286 1360 342 The amounts established in Table 2 were used for the preparation of
CPV30 286 1200 513 the mortars according to the procedures using the procedures of Bra­
zilian standard [33]. The percentage of replacement of sand by ceramic
waste was limited to 30 %, after applying the mortar on test walls
with an angular step of 0.02◦ with an interval of 1 s and an angle of 2θ
(Fig. 5), due to the presence of cracks in the walls of red ceramic bricks
ranging from 5◦ to 70◦ . To determine the peaks, the HighScore Plus
in the traces with 20 and 30 % of ceramic waste.
software was used in reference to the PDF-2 database of the Interna­
The tests performed were the consistency index, which consists of
tional Center for Difraction Data (ICDD). In cement there is the presence
determining the amount of water needed to maintain the spread be­
of gypsum, C3S (tricalcium silicate), C2S (dicalcium silicate), C3A (tri­
tween 260 mm ± 5 mm. Still in the fresh state, the mass density was
calcium aluminate) [25]. Identifying that the ceramic waste has
performed using the procedures of Brazilian standard [34]. The incor­
mineralogical phases of quartz, mica, hematite and feldspar [20]. The
porated air content was performed by the pressuremetric method and
hematite peaks must come from the goethite present in the clay and also
the water retention by the modified Buchner funnel method, using the
from other amorphous iron hydroxides, such as limonite, which are not
recommendatios of Brazilian standard [35]. The isothermal calorimetry
identified by X-ray Diffraction (XRD) [2]. The presence of mica in the
test monitors the development of hydration reactions of cementitious
composition of the ceramic residue is confirmed when the K2O content is
pastes through the amount of heat released over time, performed in
above 1.18 %, identified in the chemical analysis, in which the K2O was
accordance with using the recommendations of the American standard
2.43 % [26]. The highest peak was found at 26.6◦ quartz [3], which has
[36], in a two-channel Calmetrix I-CAL 2000 calorimeter. For this, each
a well-defined peak, there are also several mica and hematite peaks. The
sample had approximately 128 g of mortar, which were monitored for
ceramic residue comes from kaolinitic clays from Campos dos
48 h, with a temperature maintained at 22 ◦ C ± 0.02 ◦ C. Before mixing,
Goytacazes-RJ, and the kaolinite (Al2Si2O5(OH)4) transforms into met­
all the materials needed to make the mortars were kept in an environ­
akaolinite (Al2O3⋅2SiO2 + 2H2O) from 550 ◦ C, amorphous phase, so is
ment with a temperature of 22 ◦ C for 24 h. There was a time interval of
not detected by X-ray Diffraction (XRD), as the ceramic residue was
approximately 5 min between the start of mixing and positioning of the
burned between 600 and 630 ◦ C [20,27,28].
sample in the calorimeter. Thus, the registered specific heat flux and the
Fig. 4 show the granulometry of the sand and ceramic waste, which
heat released were obtained.
was carried out using the procedures of Brazilian standard [29], by the
Soon after, prismatic specimens with dimensions 40 × 40 × 160 mm
combined process of sieving and sedimentation, which classifies clay
were molded, each test in the hardened state had three specimens ac­
with dimensions smaller than 0.002 mm, sand has a diameter between
cording using the recommendatios of Brazilian standard [37]. The
0.06 mm and 2.0 mm, being subdivided into coarse, fine and medium,
curing procedure of the specimens was carried out for 28 days at room
boulders with diameter assimilated about 2.0 and 60.0 mm, divided into
temperature of 21 ◦ C and a relative humidity of 78 %. The mass density
fine, medium or thick and silt with diameters between 0.002 mm and
tests in the hardened state were carried out using the procedures rec­
0.06 mm. It is possible to notice through the granulometric curve of the
ommendatios of Brazilian standard [38] and the flexural and compres­
sand, that there is a greater predominance of coarse sand with 46.5 %.
sive strength tests were carried out with the aid of an INSTRON 5582
There is also the presence of 40 % of medium sand, 5.6 % of fine sand,
press with a maximum capacity of 10 tons. The load used in the test was
0.6 % of silt, 0.5 % of medium gravel and 6.8 % of fine gravel. It is also
50 ± 10 N/s at a speed of 1 mm/min in the flexural strength test and in
possible to identify that the sand has 0.2437 mm in d10, 0.6454 mm in
the compressive strength test a load of 500 ± 50 N/s at a speed of 10 mm
d50 and 2.935 mm in d90. As for the ceramic waste, there is a greater
was used /min, according to procedures recommendatios of Brazilian
predominance of silt with 74.9 %, clay with 11 %, 10.9 % of fine sand,
standard [37]. The capillary water absorption test was also carried out
2.4 % of medium sand and 0.8 % of coarse sand, 0.0016 mm in d10,
following recommendatios of Brazilian standard [39]. Finally, micro­
0.023 mm in d50 and 0.080 mm in d90 according to Azevedo et al.
structural characterization tests were carried out at 28 days, through
(2019). Already Hoppe Filho et al. (2021) used the ceramic waste that
porosimetry by mercury intrusion, which allows the analysis of pa­
was fired at 950 ◦ C and ground in a Los Angeles abrasion apparatus
rameters related to porosity, such as: distribution of pore sizes and their
using 12 iron balls (Ø 47 mm, 445 g each) and cycled for 3.5 h at 33 rpm,
average diameter, the test was performed according to the manual of the
indicating that the waste ceramic is 0.0018 mm in d10, 0.0069 mm in d50
equipment. The equipment used for the analysis was the AutoPore IV
and 0.028 mm in d90. Thus, the waste of this research has coarser par­
9500 porosimeter from Micromeritics Instrument Corporation, USA,
ticles than those found by Hoppe Filho et al. (2021), which can be
which uses an automatic mercury injection porosimeter in samples
explained by the difference in milling time. It is important to highlight
measuring approximately 6 × 6 × 6 mm. Mercury intrusion and
that the ceramic waste has finer particles than the fine aggregate

Fig. 5. Appearance of mortars.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Table 3 3. Results and discussion


Workability results.
Mixture Consistency index (mm) Water/dry materials ratio W/C Table 3 presents the results of the workability, respecting the limit
recommended of Brazilian standard [40], which indicates that the
CPV00 257 0.205 1.43
CPV10 263 0.237 1.66 consistency index must be 260 mm ± 5 mm. It is observed that the mixes
CPV20 260 0.276 1.92 that have partial replacement of sand by ceramic waste showed a higher
CPV30 257 0.312 2.18 water/dry materials ratio and, consequently, a higher w/c ratio, in
relation to the reference mixture, even the mixes having a w/c ratio
greater than one, mortars have less pores and water has difficulty
extrusion were investigated under pressures between 0 and 33.000 Psi,
percolating in less porous material, so the permeability is lower. It is
equivalent to 228 MPa, with pore diameters reading between 0.01 µm
noteworthy that as the addition of ceramic waste increases, the mortar
and 100 µm. The X-ray Diffraction (XRD) was performed in a Proto
needs more water during the mixing of the materials to maintain con­
Manufacturing AXRD Powder Diffraction System diffraction meter
sistency, as the ceramic waste comes from burning, therefore, part of the
operating with a voltage of 30 kV, current of 20 mA and Cu-Kα radiation,
material such as the hydroxyls volatilize and lose mass. The ceramic
with an angular step of 0.02◦ with an interval of 1 s and an angle of 2θ
waste has a deficit of OH–, therefore, it absorbs water easily by electrical
ranging from 5◦ to 70◦ . To determine the peaks, the HighScore Plus
attraction with the water, which is an electric dipole [3,41].
software was used in reference to the PDF-2 database of the Interna­
Figs. 6 and 7 show the density and content air content results,
tional Center for Difraction Data (ICDD). The samples were crushed and
respectively. In general, it is possible to notice that the replacement of
passed through a 75 µm sieve (n◦ 200). Afterwards, the samples were
sand by ceramic waste caused an increase in the mass density in the fresh
mixed with isopropyl alcohol for 3 min at a volumetric ratio of 1:10
state of the evaluated mortars, becoming denser and with a lower con­
(sample: isopropyl alcohol) in a glass container with a glass rod. Soon
tent of incorporated air, with a pozzolanic reaction with the finer par­
after, it was filtered and dried in a desiccator at 20 ◦ C until constant mass
ticles and nucleation [16,42]. It can be seen that the mixture with the
was obtained.
lowest density was the CPV00 (reference) with 1.90 g/m3, while the

Fig. 6. Density results.

Fig. 7. Incorporated air content results.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Fig. 8. Water retention results.

mixture with the highest density was the CPV10 with 1.99 g/m3. It is be greater than 95 %, as there may be poor adhesion between the mortar
also possible to observe that the density decreased as the amount of and the substrate [44]. However, all mixtures are within the re­
ceramic waste increased, since the specific mass of the waste (2.59 g/ quirements established by the references, it is a positive result, since
cm3) is smaller than that of the sand (2.64 g/cm3). Density reduction is a water retention is a property that is directly related to the ability of fresh
positive point as long as it does not affect the other properties [4,43]. mortar to maintain its workability when subjected to requests that cause
The amount of incorporated air decreased as the amount of ceramic loss of mixing water, either through evaporation or absorption of water
waste increased, as there are more pozzolanic reactions of finer parti­ [45]. It is also observed that the reference mixture has a higher value
cles, with nucleation occurring. This is also related to the fact that the than the CPV10 and CPV20 mixtures, indicating that mixtures with
residue has a filler effect, that is, it fills the voids between the grains. higher percentages of ceramic waste are more recommended. The
Observing the values found, the mixture with the highest content of CPV30 mix has better water retention with 94.50 %. A possible expla­
incorporated air is the CPV00 with 10 % and the lowest content of nation for the improvement caused by mortars with ceramic waste is
incorporated air is the CPV30 mixture with 4.2 %. As the granulometry attributed to the fact that the ceramic waste comes from the burning of
of the waste at 1.73 µm in d10, 12.74 µm in d50 and 47.20 µm in d90, that clay and the clay presents surface activity due to the clay minerals that
is, fine particles, filled the existing voids, consequently reducing the compose it, which makes this material present electrical attraction to the
content of incorporated air, shown in Fig. 7, and as the waste consumed water particles [46,47].
a lot of water, there was a drop in density, as the specific mass of water is Fig. 9 shows the results of calorimetry through the released heat. It
lower than that of the ceramic waste, as shown in Fig. 6. can be seen that the main hydration of all mortar mixtures occurs in the
Fig. 8 shows the water retention results. It is possible to observe that first 15 h [48]. In stage I, where it occurs in the first minutes, it presents
there is an increase in water retention, as the amount of ceramic waste the first peak of the evolution of the heat of hydration, whose main re­
increases. The water retention of mortars must not be lower than 75 %, action is the dissolution of tricalcium aluminate (C3A) and calcium
as it can impair the mortar’s strength [21]. However, retention cannot sulfate (CaSO4), forming ettringite. The CPV30 mixture has a higher

Fig. 9. Calorimetry results.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

release. This is due to the filer effect resulting from the low granulometry
of the ceramic waste, responsible for providing nucleation points [49].
In stage II, during the dormancy period, the mixtures present very close
values of released heat, which shows that the ceramic waste did not
affect the induction period. In stage III, where the second exothermic
peak occurs, the CPV10 mixture had a large peak at 7.5 h, while the
CPV20 had a large peak between 5.5 and 6 h, thus presenting greater
heat released. In this phase, tricalcium silicate (C3S) and dicalcium sil­
icate (C2S) react with water and rapidly form amorphous hydrated
calcium silicate (C–S–H) and calcium hydroxide (Ca(OH)2) [50]. After
this step, the mixtures entered the final stage of hydration, with low
reactivity, but with gain in strength.
Fig. 10 shows the accumulated heat, the CPV20 and CPV00 mixtures
have more accumulated heat, with 380 and 350 J/g, respectively. As the
Fig. 10. Calorimetry results. amount of ceramic waste increased, there was a decrease in the accu­
mulated heat. This can also be explained by the consistency index test,

Fig. 11. Density results in the hardened state.

Fig. 12. Flexural strength in bending results.

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Fig. 13. Compressive strength results.

[52]. In the study by Gayarre et al. (2017), found a range of 1.5 MPa to
2.5 MPa for flexural strength and a range of 5.5 MPa to 8.5 MPa for
compressive strength. Mohit and Sharifi (2021) was in the range of 2.86
MPa to 3.84 MPa for flexural strength and the best strength was with the
use of 10 % of the waste, a result that corroborates with what was found
in this research.
Fig. 14 presents the results of the capillarity coefficient, indicating
that the mixture with the highest capillarity coefficient is the reference
mixture (CPV00), with 9.33 g/dm2.min1/2, results also found by For­
migoni et al. (2019). As the amount of ceramic waste increased, so did
the capillarity coefficient. The increase in the coefficient may be asso­
ciated with the linear increase in the fine material (ceramic waste), as its
density is lower than the fine aggregate. The fact that the reference
mixtures have higher capillarity coefficients may be associated with the
fact that these mixtures have larger capillary pores and, consequently,
the water can infiltrate more easily and, thus, absorb a greater amount of
water.
Fig. 14. Capillarity coefficient results.
Fig. 15 presents the results of Mercury intrusion (a), Cumulative pore
volume (b) and Pore volume fractions (c). Through Fig. 15 (a) it is
where the mixtures with the highest amount of ceramic waste had the
possible to notice that the mixtures presented pores in the range of 0.1 to
highest water consumption, the highest amount of water or the increase
40.0 µm. The mixtures CPV10, CPV20 and CVP30 had higher mercury
in water contente amount of ceramic waste may be causing the reduc­
intrusion in the smaller pore diameters, while the reference mixture
tion of heat release. It is also possible to notice the exothermic peaks,
(CPV00) had higher mercury intrusion in the pore diameters between 1
indicating that nucleation of the finest particles occurs, converging with
and 10 µm. The CPV20 and CVP30 mixtures had greater mercury
the 11 % clay fraction of the ceramic waste.
intrusion than the CPV10 mixture in pore diameters between 1 and 10
Fig. 11 shows the results found for the bulk density in the hardened
µm. In the pore diameter range between 10 and 100 µm, the mixtures do
state. The mixture with the highest density value is CPV10, with 1.86 g/
not show significant differences. The CPV10 mixture had its highest
m3. The mixture with the lowest density is CPV30, with 1.64 g/m3.
peak in mercury intrusion at 1 µm at 0.12 mL/g. The reference mixture
Values that corroborate with those obtained by Cabrera-Covarrubias et
has larger average pores than the mixtures containing ceramic residue,
al. (2016) e Gayarre et al. (2017). One explanation for the reduction in
that is, the reference mixture is more porous and the CPV20 and CPV30
the values of this test is the density of recycled aggregates being lower
mixtures are more porous in relation to the CPV10 mixture. This can be
than that of natural sand. However, this is not a property that limits the
explained by the fact that the ceramic residue is filling the mortar. The
use of recycled aggregates in the manufacture of mortars [41,42].
decrease in porosity with the increase in the amount of ceramic waste
Fig. 12 presents the flexural strength in bending results, while Fig. 13
may also be associated with the firing temperature of the blocks, as the
presents the compressive strength results. The highest strengths were
high temperature leads to a decrease in porosity [53]. When comparing
with 10 % of the ceramic waste, reaching 3.24 MPa of flexural strength
with the results of water absorption by capillarity and water absorption
and 11.22 MPa of compressive strength, with higher percentages of
by immersion and void index, where the mixtures with waste use had
waste there was a decrease in strength. In general, the behavior of the
higher absorptions, it can be explained, because higher percentages of
loss of flexural and compressive strength related to the increase of the
small pores increase absorption [10]. In the study by Torres et al. (2020),
ceramic waste may be caused by the physical characteristics of the
the reference mortar had a greater volume of pores, staying in a size
ceramic waste, such as lower densities than sand and higher absorptions
range of approximately 10 to 80 µm, while the mortars with ceramic

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M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

Fig. 15. (a) Mercury intrusion; (b) Cumulative pore volume; (c) Pore volume fractions.

Fig. 14 (c) shows a refinement in the pore size for the CPV10 mixture,
containing pore sizes between 0.1 and 50 µm of 0.65 cm3/g, a smaller
value between the mixtures, being more efficient in reducing pore vol­
ume, converging the results of Figs. 12, 13 and 14. This was already
expected to occur because the nucleation of finer particles in the CPV10
mortar was observed in Fig. 9 in the fresh state by calorimetry and, also
in Fig. 15, with the presence of the amorphous halo referring to the
formation of C–S–H and the disappearance of portlandite peaks,
making the CPV10 mortar denser and more resistant.
Fig. 16 shows the presence of ettringite, portlandite, quartz and
calcite [55–58]. The calcite phase, coming from the limestone filler that
composes the anhydrous OPC and the carbonation of the sample, can be
justified by the presence of OPC as a component of the formulation [23].
The amorphous halo in the diffractogram between 18◦ and 29◦ 2θ,
which does not have a well-defined crystal structure, that is, it has
characteristic peaks together with a baseline bump in the aforemen­
tioned region. The ceramic residue consumed portlandite and generated
more calcite formation, the amorphous halo comparing the CPV10
mixture with the reference one (CPV00) has fewer peaks, converging
with the flexural and compression strengths, in which the mortar with
Fig. 16. XRD results. Caption: A/CPV (cement + water), CPV00 (sand +
cement + water), CPV10 (ceramic waste + cement + water), CPV20 (ceramic the highest strengths had 10 % of ceramic residue, the highest density in
waste + cement + water), CPV30 (ceramic waste + cement + water), E the fresh and hardened state, calorimetry, by porosimetry that proved
(ettringite), P (portlandite), Q (quartz), C (calcite). that it has fewer pores. On the other hand, the CPV20 and CPV30 traits
had the presence of ettringite, interfering with the decrease in
residue had a greater volume of pores in intervals of smaller diameters, resistance.
between 0.7 and 3 µm. 0.0 µm. This same trend also occurred in the
study by Grilo et al. (2014), where the reference mortar had a greater 4. Conclusions
volume of pores in the range of 0.5 to 10 µm. This same trend occurred in
Fig. 14, but with larger pore diameters. In Fig. 14 (b) The mixture CPV10 Based on the results obtained, it is possible to conclude that:
showed a lower cumulative volume of mercury intrusion of 0.11 mL/g in
pores from 0.1 to 40 µm, suggesting less pores and greater densification - The use of ceramic waste promotes an increase in water consumption
of this trace, converging with the result of Fig. 11. The other traces in the mortar and an increase in workability. The mixtures with 20 %
showed cumulative intrusion volume between 0.12 mL/g to 0.14 mL/g. and 30 % of ceramic waste showed a decrease in density both in the
fresh state and in the hardened state, proving that the specific mass of

9
M.G.P. Cherene et al. Construction and Building Materials 367 (2023) 130256

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Declaration of Competing Interest [27] M.S. Morsy, H. Shoukrya, M.M. Mokhtara, A.M. Ali, S.A. El-Khodary, Facile
production of nano-scale metakaolin: An investigation into its effect on
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The authors declare that they have no known competing financial Constr. Build. Mater. 172 (2018) 243–250.
interests or personal relationships that could have appeared to influence [28] S.K.B.M. Silva, C.J. Araújo, A.G.B. Lima, Numerical analysis of the dimensional
the work reported in this paper. variation in structural ceramic blocks during the drying process, Research, Society
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[29] ABNT NBR 7181:1984- Determination of Granulometric Analysis of Soils; Brazilian
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[30] P.I. Moreira, J.O. Dias, G.C. Xavier, C.M. Vieira, J. Alexandre, S.N. Monteiro, R.
No data was used for the research described in the article.
P. Ribeiro, A.R.G. Azevedo, Ornamental Stone Processing Waste Incorporated in
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