Hindawi

Advances in Materials Science and Engineering

Volume 2019, Article ID 4609353, 15 pages
https://doi.org/10.1155/2019/4609353

Research Article
Effects of Incorporation of Marble Powder Obtained by Recycling
Waste Sludge and Limestone Powder on Rheology, Compressive
Strength, and Durability of Self-Compacting Concrete

Rayed Alyousef ,1 Omrane Benjeddou ,2,3 Chokri Soussi,1,2

Mohamed Amine Khadimallah,1,4 and Abdeliazim Mustafa Mohamed1
1
Prince Sattam bin Abdulaziz University, College of Engineering, Civil Engineering Department, Alkharj, Saudi Arabia
2
Higher Institute of Technological Studies of Sfax, Department of Civil Engineering, Sfax, Tunisia
3
University of Tunis El Manar, National Engineering School of Tunis, Civil Engineering Laboratory, Tunis, Tunisia
4
University of Carthage, Polytechnic School of Tunisia, Laboratory of Systems and Applied Mechanics, Tunis, Tunisia

Correspondence should be addressed to Omrane Benjeddou; benjeddou.omrane@gmail.com

Received 26 October 2018; Revised 26 January 2019; Accepted 26 February 2019; Published 4 April 2019

Academic Editor: Pietro Russo

Copyright © 2019 Rayed Alyousef et al. This is an open access article distributed under the Creative Commons Attribution
License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.

Marble has been commonly used as a building material since ancient times. The disposal of waste materials from the marble
industry, consisting of sludge that is composed of powder mixed with water, is one of the current worldwide environmental
problems. This experimental study aims to valorize marble powder, which is achieved by grinding the sludge as filler added to the
cementitious matrix of self-compacting concrete (SCC). The main purpose of this work is to evaluate the marble filler effects on the
rheology in the fresh state and on the hardened properties of SCCs compared to those of limestone filler. To this end, two SCCs,
SCCM and SCCL, manufactured using marble powder and limestone filler, respectively, were prepared and tested. The fresh
properties of the two SCCs’ mixtures were determined by slump flow, L-box, V-funnel, sieve stability, bulk density, and air
content. Tests on hardened SCCs included compressive strength, homogeneity, and quality in terms of ultrasonic pulse velocity
and durability against carbonation and water penetration. In addition, scanning electron microscope (SEM) and X-ray diffraction
(XRD) were used to analyze the specimens.

1. Introduction recycling materials leads to a significant reduction in the cost

of SCC.
Self-compacting concrete (SCC) was first developed in Japan There are many types of mineral additions used in SCC
in 1988 [1] and is a new concrete that is fully compacted composition but the most common is the limestone powder
without external energy. SCC provides economic, social, and [6–8]. Having a property of physical improvement of the
environmental benefits compared to conventionally vibrated cement paste matrix, limestone filler is one of the materials
concrete. SCC is made from the same basic constituents as that have extensively been studied in the literature. The
conventional concrete, but with the addition of high levels of effects of limestone powder on the rheological and me-
superplasticizer (SP) admixtures in order to obtain high chanical properties of SCC have been widely studied. The
workability [1, 2]. The self-compactabilty of SCC is defined results of these studies show that when adding limestone
as the capability of the concrete to be uniformly filled and powder to the cementitious matrix of SCC, the workability
compacted in the formwork corners by its self-weight improved with reduced cement content, the segregation
without vibration during placement [3]. resistance increased, and the pore distribution was modified
Singh et al. [4] and Sharifi et al. [5] indicated that the [6–10]. Another research [11] indicate that limestone
addition of inert, pozzolanic/hydraulic or waste and powder decreases both plastic viscosity and yield stress. In
2 Advances in Materials Science and Engineering

addition, the incorporation of limestone powder increases tested: SCCM was manufactured using marble filler and
the density of the paste, which is particularly important in SCCL was manufactured using limestone filler. The fresh
improving the compressive strength [12]. Marble ranks the properties of the two SCCs’ mixtures were determined by
largest produced natural stone in the world, and it accounts slump flow, L-box, V-funnel, sieve stability, bulk density,
for 50% of the world’s natural stone production [13]. The and air content. Tests on hardened SCCs included com-
marble industry produces a lot of waste in the form of pressive strength, homogeneity, and quality in terms of
powder, sludge, and pieces of irregular size. Marble powder ultrasonic pulse velocity and durability against carbonation
is a waste material generated in considerable amounts in the and water penetration. In addition, the experimental results
world [14]. For example, during the cutting process alone, were analyzed by the scanning electron microscope (SEM)
20–30% of a marble block becomes waste marble powder and X-ray diffraction (XRD).
[14]. It was also reported that about 50% of the marble blocks
is wasted during the production process; 90% of the waste 2. Experimental Program
particles are below 200 μm [15].
The considerable amounts of marble powder waste cause The main purpose of this study is to highlight the possibility
serious environmental problems [14]. The main solution is of using marble powder, obtained by grinding the sludge, as
to recycle and reuse this inert powder in construction and filler added to the SCC cementitious matrix.
building materials. This method offers certain advantages, The experimental program is composed of three main
such as protecting natural resources, saving energy, con- parts: the first part presents a description of the different
tributing to the economy, decreasing waste materials, and steps in the preparation of the marble and limestone fillers,
investing for the future [16]. obtained by grinding the marble waste sludge and crushing
Marble filler materials can be successfully and eco- limestone blocks, respectively. The second part presents the
nomically utilized to improve certain fresh and hardened results of the identification of the properties of the marble
SCC properties [17]. The effects of substituting cement with filler, limestone filler, and other used materials.
marble powder on the rheological and mechanical properties The third part presents a comparison of the effects of the
of self-compacting mortar (SCM) have been studied [18–25], marble and limestone fillers on the fresh and hardened
and the results indicated an improvement in the workability properties of the SCC. In order to achieve this, two SCCs
and compressive strength of SCM with the use of marble were prepared and tested: SCCM was manufactured using
powder. marble filler and SCCL was manufactured using limestone
Research on SCC has focused on improving both its filler. The order of testing in the fresh state was as follows: 1,
fresh and hardened properties. Okamura and Ouchi [1] slump flow test; 2, V-funnel test; 3, sieve stability test; 4, bulk
demonstrated that the self-compactability of SCC may be density test; 5, L-box test and air content measurement [28].
affected by various parameters, such as the material prop- The hardened properties studied included the compressive
erties, mix proportions, and mix-design method. Further- strength, the evaluation of homogeneity and quality in terms
more, they indicated that the self-compactability is highly of ultrasonic pulse velocity, and durability against carbon-
sensitive to the water-filler ratio and coarse and fine ag- ation and water penetration. Finally, microstructural anal-
gregate sizes. They demonstrated that the paste in the SCC ysis was carried out on the prepared samples.
requires high viscosity as well as high deformability.
Moreover, this deformability is affected by the water-filler
ratio, which is preferred over the water-cement ratio because
3. Materials and Experimental Methods
most filler materials are not reactive. Furthermore, Singh 3.1. Materials
et al. [4] indicated that the SCC rheology depends on the
ambient temperature, mixer type, and mixing efficiency. 3.1.1. Marble and Limestone Powders
Shindoh and Matsuoka [3] indicated that a superior SCC
should deform effectively under its own weight, without (1) Preparation of Powders. In this study, the limestone filler
segregation of ingredients. They also demonstrated that the was prepared by crushing limestone blocks, and its char-
slump flow test is applied only as an evaluation test for acteristics are presented in the relevant section.
estimating the SCC deformability. In order to achieve this, The marble sludge, which is a waste product from the
they developed a new test method for evaluating the SCC marble cutting industry, was collected from local marble
deformability and resistance to segregation. cutting plants. Grains of marble sludge clump together into
Attachaiyawuth et al. [26] develop a new mixing method lumps; thus, marble sludge grains were not homogeneously
that enables entrained air bubbles to be suitable for en- distributed throughout the mixture.
hancement in self-compactability. In the same case, Ouchi The procedure for preparing the marble powder con-
et al. [27] improved SCC properties in the fresh state with the sisted of the following steps:
addition of an antifoaming agent during the mixing step.
(i) The marble sludge was air dried for two days
The present experimental study aims at valorizing the
sludge, which is the waste from the cutting operation of (ii) The dried sludge was crushed with a hammer to
marble blocks and evaluating the marble filler effects on the create small blocks
fresh and hardened properties of the SCCs compared to (iii) The marble sludge waste was dried in an oven at
those of limestone filler. Two SCCs were prepared and 80°C for 24 h to remove moisture
Advances in Materials Science and Engineering 3

(iv) The dried sludge was ground to obtain a fine powder (4) Reactivity Tests. This section consists of determining
(v) Finally, the marble filler was created by passing the whether the two powders have hydraulic properties with
powder through the desired sieve to filter the 63 μm water. In order to achieve this, two reactivity tests were
particles performed on two pastes, each prepared by 500 g of a type of
powder added to 250 g of water in a thermostatically isolated
Characterization of the marble sludge filler was carried flask. The reactivity tests consist measuring the temperature
out using a number of experimental techniques in order to evolution of the two pastes.
confirm its composition. Figure 2 shows that the temperature of the two pastes
should be adjusted very slightly (from 18 to 20°C) for a
(2) Chemical Analysis of Fillers. The chemical analysis of the period of more than 6 h. This result indicates that the two
two fillers was performed using atomic absorption spec- powders exhibit no hydraulic properties in the presence of
trometry (AAS), according to the requirements of NF EN water; therefore, the marble and limestone powders can be
ISO 15586 [29]. The chemical analysis results of the marble considered as inert components in concrete. In fact, the
and limestone powders are presented in Table 1. The results hydraulic reaction of SCC prepared by one of the two
indicate that the two powders are excessively rich in calcite, powders will not be modified or influenced.
CaCO3 � 94.88% for marble powder and 97.29% for lime- In addition, the reactivity of the two powders with ce-
stone powder. In addition, the results indicate that the two ment was verified by measure of setting time of cement
fillers are devoid of all clay and organic matter. This last paste, limestone-cement paste, and marble-cement paste.
result was confirmed by measurement of calcium carbonate The setting time measurement test was carried out, using
(CaCO3), according to the requirements of NF P94-048 [30], vicat apparatus, according to the standard NF EN 196-3 [36].
which indicate that both limestone and marble powder The curves depicted in Figure 3 indicate the setting times of
samples contain 95% CaCO3. the three pastes. The results demonstrate that the addition of
Finally, the results of the methylene blue test, performed the two powders to the concrete has almost no influence on
according to the requirements of NF P94-068 standard [31], the cement setting time. This confirms the result already
demonstrated that the methylene blue value (MBV) of the demonstrated in the previous section: the marble and
limestone and marble powders was 0.11 and 0.45, re- limestone powders are inert components in SCC and does
spectively. This indicates that the two powders do not not lead to much change in the phase composition of the
contain any clay. resultant mix.
There many studies showing that the limestone and
(3) Particle Size Analysis. Grain size distribution charac- marble powder are inert or having low reactivity with the
terization of the two powders was carried out in two steps: other components of pastes, concrete, or mortars. For ex-
the granulometry test by wet sieving, according to the ample, the microstructure analysis, determined using
standard NF P94-056 [32], for particles with diameters scanning electron microscopy (SEM) and X-ray diffraction
superior than 80 μm and granulometry test by the sedi- (XRD) on different pastes, of Aliabdo et al. [23] show that
mentation method, according to the standard NF P94-057 marble waste powder does not possess any pozzolanic ac-
[33], for quantifying fractions of particles with diameters tivity. It will act as an inert and filler material rather than a
lower than 80 μm. pozzolanic one. Also, Khodabakhshian et al. [37] and Omar
Figure 1 shows the particle size distribution curves for et al. [38] indicate also that marble powder is an inert or
the limestone and marble powders. quasi-inert material, being noncementitious from hydraulic
The results indicate that the Hazen coefficients of the points of view.
marble and limestone powders are 6.33 and 10.6, re- In the same case, Liu and Yan [39] and Chaid et al. [40]
spectively, and the curvature coefficients of the marble and indicate that limestone powder has no pozzolanic activity
limestone powders are 0.43 and 2.09, respectively. These and then it was an inert cementitious addition. But it im-
results prove that the granular distribution of the two proves the performance of concrete.
powders are effectively graded and graduated, and their
masses consist of different particle size ranges. (5) Results Interpretation. Table 3 presents the physical and
chemical properties of the fillers according to the standard
(4) Physical Properties. The results presented in Table 2 NF EN 206-1 [41]. Table 3 is reproduced from Benjeddou
indicate that the two powders have almost the same abso- et al. [2] (under the Creative Commons Attribution License/
lute density (2.69 g/cm3 and 2.71 g/cm3). On the contrary, public domain).
the results show that the marble powder is excessively light According to the obtained results, the physical and
compared to the limestone powder since the bulk density is chemical properties of the two analyzed powders correspond
0.61 g/cm3 for the marble powder and 0.90 g/cm3 for the to the cited standard criteria. The two tested powders can be
limestone powder. added as fillers in SCC formulation.
The Blaine specific surface (BSS) values of the two
powders were determined using the Blaine air permeability 3.1.2. Cement. The cement used was CEM I 42.5, in con-
apparatus. According to the results presented in Table 2, the formity with the standard NF EN 197-1 [42]. The physical
BSS values of the marble and limestone powders are and mechanical characteristics of this cement are displayed
4405 cm2/g and 9459 cm2/g. in Table 4.
4 Advances in Materials Science and Engineering

Table 1: Chemical compositions of marble powder and limestone powder (%).

Component LOI CaO MgO SiO2 Fe2O3 Al2O3 Na2O K2O SO3 P2O5 MgCO3 S Moisture
Marble powder 42.60 52.28 0.50 3.00 0.39 0.14 — — — — 1.04 0.03 0.20
Limestone powder 43.09 54.20 0.69 0.37 0.17 0.11 0.02 0.07 0.06 0.03 — — —

100
90
80
Cumulative % 70
60
50
40
30
20
10
0
1 10 100 1000
Diameter (µm)

Marble filler
Limestone filler
Figure 1: Particle size distribution curves of the limestone and marble fillers.

Table 2: Physical parameters of two powders.

Parameters Particle size (mm) Absolute density (g/cm3) Bulk density (g/cm3) Blaine specific surface (BSS) (cm2/g)
Standard NF P94-056 [32] NF EN 1097-7 [34] NF EN 196-6 [35]
Limestone filler 0/0.125 2.71 0.90 4405
Marble filler 0/0.063 2.69 0.61 9459

22 40

21 35

30
20
Penetration (mm)
Temperature (°C)

25
19
20
18
15
17
10
16 5

15 0
0 1 2 3 4 5 6 7 0 20 40 60 80 100 120 140 160 180 200 220 240
Time (h) Time (min)
Ambient temperature Cement
Limestone paste Cement + marble
Marble paste Cement + limestone
Figure 2: Paste temperature measurement. Figure 3: Measurement of setting time of the different pastes.

3.1.3. Aggregates. Natural sand 0/2, crushed sand 2/4, ravel chains of modified polycarboxylate, especially conceived for
4/8, and gravel 8/12 were used as aggregates. The physical self-compacting concrete and certified in conformity with
characteristics of these aggregates are displayed in Table 5. standard NF EN 934-1 [46]. The density of this SP is about
1.06, and its pH is between 4.5 and 6.5. In addition, this used
SP has a dry extract percentage varying from 28 to 31%.
3.1.4. Admixture. The employed admixture is a super- Finally, the CI− and Na2OEq percentages of this SP do not
plasticizer (SP); it is a new generation product based on exceed 0.1 and 1%, respectively.
Advances in Materials Science and Engineering 5

Table 3: Physical and chemical properties of fillers according to Benjeddou et al. [2].
Properties BSS CaCO3 content Methylene blue value Sulphate content
Criteria >2000 cm2/g >62% <1.3 g/100 g <0.15%

Table 4: Physical and mechanical properties of cement.

Properties Absolute density (g/cm3) Bulk density (g/cm3) BSS (cm2/g) True class of strength (MPa)
Standard NF EN 196-1 [43] NF EN 196-1 [43] NF EN 196-6 [35] NF EN 196-1 [43]
Value 3.08 1.03 3100 44.5

Table 5: Physical characteristics of aggregates.

3
Aggregates Bulk density (g/cm ) Absolute density (g/cm3) Absorption (%) Finesse module Equivalent of sand (%)
Standard NF EN 1097-6 [44] — NF EN 933-8/IN1 [45]
Gravel 4/8 2.55 1.42 0.32
Gravel 8/12 2.55 1.40 0.32
Sand 0/2 2.42 1.47 1.85 91
Crushed sand 2/4 2.43 1.32 0.32 4.8 100

According to the saturation point obtained from the flow (1) Slump Flow Test. This test is the simplest and most widely
time-admixture dosage curve, in accordance with the used test method for quantifying the SCC workability [53].
standard NF P18-507 [47], the optimal SP/cement ratio is This test, measured according to the standard NF EN 12350-
equal to 1.2% [48, 49]. 8 [54], indicates the horizontal flow of the SCC, and it is a
good indicator of the self-compacting properties of the SCC.

3.2. Formulation of a Self-Compacting Concrete. This part of (2) L-Box Test. This test is used to investigate, according to
our experimental investigation consists of evaluating the the requirements of NF EN 12350-10 [55], the SCC flow rate
marble filler effects on the SCC properties compared to those and passing ability in confined spaces. It measures the
of the limestone filler. For this purpose, two SCCs were reached height of fresh SCC after passing through the
prepared and tested: SCCM was manufactured using marble specified steel bar gaps flowing within a defined distance.
filler and SCCL was manufactured using limestone filler.
The two self-compacting concretes, SCCM and SCCL, (3) V-Funnel Test. This test gives, according to the re-
were formulated by using the excess paste method [50–52] quirements of NF EN 12350-9 [56], the flow time of SCC
and based on the requirements of the standard NF EN 206-1 which is the period required for a defined volume of SCC to
[41]. It is an SCC of the SF2 class with a 28-day compressive pass through a narrow opening. It can indicate the SCC filing
strength of 30 MPa (SS30). For the slump class SF2, the ability, provided that blocking and/or segregation do not
slump test values must be between 66 and 75 cm. The dosage take place, and the flow time of the V-funnel test is related to
adopted for manufacturing the SCC30, using limestone or the plastic viscosity to a certain extent.
marble filler, is presented in Table 6.
(4) Sieve Stability Test. This test was carried out according to
the requirements of NF EN 12350-11 [57]. A sample of 10 L
3.3. Test Procedures. Two series of experimental tests were of concrete was allowed to rest for 15 min; then, 2 L thereof
carried out on the two self-compacting concretes SCCM and was poured onto a 5 mm sieve from a height of 500 mm, and
SCCL: the first series of tests were carried out on the fresh the sample percentage passing through the sieve was
state and the second were carried out in the hardened state. recorded. It has been reported that the variability of such test
All tests were performed according to international results is poor, particularly when the segregation is severe
standards, and each experimental test was carried out in 3 [58].
different samples at different times, with different persons,
and under somewhat different experimental conditions. (5) Air Content Test. This test was required for checking air-
entrained concrete, the testing method for which is provided
in NF EN 12350-7 [59].
3.3.1. Experimental Tests in the Fresh State. The tests carried
out on the fresh state of the two SCCs were the slump flow,
L-box test, V-funnel, sieve stability, and bulk density tests as 3.3.2. Experimental Tests in the Hardened State. The ex-
well as air content measurement. These rheological tests perimental tests carried out on the hardened state of the two
were carried out after a nominal interval of 15 min following SCCs are the compressive strength test, the pulse velocity
the first contact of water with cement in the SCCM and test in order to evaluate the homogeneity and quality of the
SCCL [3]. two SCCs, the measurement of the carbonation penetration
6 Advances in Materials Science and Engineering

Table 6: Composition of 1 m3 of SCCM and SCCL.

Cement (kg) Filler (kg) Sand 0/2 (kg) Sand 2/4 (kg) Gravel 8/12 (kg) Gravel 4/8 (kg) Water (L) SP (kg)
400 100 720 180 720 180 200 4.4

depth test, the water penetration depth test, and micro-

structure analysis.

(1) Compressive Strength Measurement. 18 cylindrical

specimens of 16 × 32 cm were prepared for each of the two
SCCs, the formulations of which are presented in Table 6.
Thereafter, the test pieces were crushed at the ages of 3, 7, 14,
and 28 days in order to determine the compressive strengths
of the two concretes at these ages.

(2) Pulse Velocity Test. The object of this method is to

measure the velocity of the pulses of longitudinal waves
passing through concrete in order to evaluate the homo-
geneity and quality of the tested concrete [60]. This is due to
the effect of the concrete properties on the velocity of an
ultrasonic pulse. Indeed, the pulse velocity increases or
decreases as the concrete matures or deteriorates or changes Figure 4: Ultrasonic pulse velocity test method.
with time.
The equipment consists essentially of an electrical pulse
generator, a pair of transducers, an amplifier, and an elec- and remains colorless in carbonated concrete as shown in
tronic timing device for measuring the wave velocity between Figure 5.
the transmitting transducer and the receiving transducer. The carbonation depth was measured at the age of
The ultrasonic pulse velocity measurements have been 90 days on three cylindrical specimens of 16 × 16 cm of
determined with the direct transmission mode (Figure 4) SCCM, SCCL, and ordinary concrete.
on three cylindrical specimens of 16 × 32 cm of SCCM,
SCCL, and ordinary concrete at the age of 28 days, in (4) Determination of Water Penetration Depth. The mea-
accordance with the requirements of EN 12504-4 [61]. The surement of water penetration depth, of the ordinary con-
ordinary concrete specimens were prepared with the same crete and the two self-compacting concretes SCCM and
composition presented in Table 6 but without the addition SCCL, is carried out according to the requirement of the
of filler. standard NF EN 12390-8 [64] on three cylindrical specimens
of 16 × 16 cm aged 28 days.
(3) Measurement of the Carbonation Penetration Depth. The apparatus used to determine the water penetra-
Durability is a major concern for concrete structures ex- tion depths is presented in Figure 6. Once the specimens
posed to aggressive environments. Many environmental were assembled in the test cells, a water pressure of 5 bars
phenomena are known to significantly influence the dura- was applied for 72 hours. The specimen was then split in
bility of reinforced concrete structures. Carbonation is one half, perpendicularly to the face on which the water
of the major factors to cause structure deterioration. pressure was applied. As soon as the freshly exposed
The carbonation is a chemical phenomenon linked to surface dried and the water penetration front can be clearly
the emission of carbon dioxide into the atmosphere. In- seen, the maximum depth was marked as presented in
deed, carbonation is the reaction of carbon dioxide CO2 in Figure 5. The maximum depth is called water penetration
the environment with the calcium hydroxide Ca(OH)2 in durability.
the cement paste. This reaction produces calcium car-
bonate CaCO3 and lowers the pH to around 9 [62]. The (5) Microstructure Tests. Microstructural analysis using SEM
carbonation front advances progressively from the facing, and XRD was carried out to compare the SCCM and SCCL
and then the protective oxide layer surrounding the properties in the fresh and hardened states [65–69]. Three
reinforcing steel breaks down and corrosion becomes control pastes, a cement-marble powder paste, and a
possible [62]. cement-limestone powder paste were analyzed. The control
A simple test can be used to determine the depth of pastes, denoted CP, MP, and LP, were made from 400 kg of
carbonation penetration. Phenolphthalein is prepared as a cement, 400 kg of marble powder, and 400 kg of limestone
1% solution in 70% ethyl alcohol, and the solution is sprayed powder, respectively. The other pastes, denoted CMP and
onto the concrete surface which has been cleaned of dust and CLP, were prepared from 400 kg of cement and 100 kg of
loose particles, according to requirement of NF EN 14630 marble powder and limestone powder, respectively. The
[63]. Phenolphthalein turns noncarbonated concrete red cement-to-water weight ratio was equal to 0.26.
Advances in Materials Science and Engineering 7

Figure 5: The measurement of carbonation penetration and water penetration depths: (a) SCCM; (b) SCCL; (c) ordinary concrete.

(a) (b)

Figure 6: Apparatus for determination of water penetration depth.

Table 7: Properties of two SCCs in fresh state.

4. Results and Discussion
Test Standards value for SF2 SCCL SCCM
4.1. Effects of Marble and Limestone Filler on Rheology of SCC Slump flow (cm) 66 75 67 55
L-box h2/h1 ≥ 0.8 0.89 0.5
4.1.1. Self-Compacting Properties. All the self-compacting
Sieve stability (%) <15 0.6 2.6
concrete mixes with limestone and marble powder had a Bulk density (kg/m3) 2400 2440
satisfactory performance in the fresh state. From the test V-funnel (s) 8 ≤ time ≤ 14 9.08 2.59
results, it was concluded that the workability of fresh SCC Air content (%) ≤5 2.7 1.2
was not affected for certain percentages of added marble
powder. However, the mechanical properties of hardened
SCC have degraded.
Previous research assessed the mechanical properties of (i) First, the water absorption ratio of the fine marble
SCCs where filler materials such as limestone powder, fly grain is higher compared to the limestone grain. It
ash, and silica fume were used [18]. Literature results are in should be noted that the SSB value of the marble
good agreement with the results obtained here. Additional filler (9459 cm3/g) is almost 2.5 times that of the
aspects are addressed in the present study, such as the limestone filler (4405 cm3/g). Moreover, the particle
durability and rheology in the fresh state of the SCC as well size curves of the two fillers (Figure 1) indicate that
as its microstructural characterization. the marble filler grain size is less than 63 μm, whereas
According to the results presented in Table 7, the slump that of the limestone filler grains are less than
flow values of the SCCM and SCCL are 55 cm and 67 cm, 125 μm. The particle size curves also demonstrate
respectively. Indeed, the SCCM concrete is of flow class SF1, that the percentages of the grains with a size of less
while SCCL is of flow class SF2. SCCL concrete has good self- than 2 μm are 29% for marble grains and 12% for
compacting properties compared to SCCM. The low slump limestone grains. This difference in the two filler
test value for the SCCM concrete is due to the increase in its grain sizes makes the marble filler absorb more
viscosity. water, reducing the workability and consequently
The difference in the slump test values for the two the viscosity of the final concrete. In fact, the slump
concretes is a result of two main factors: flow value of the SCCM is less than that of the SCCL.
8 Advances in Materials Science and Engineering

(ii) The second factor can be explained by the added The low air content percentage of the SCCM is a result of
amount of marble filler (100 kg). This quantity must its compactness, which is a consequence of the granulometry
be reduced, because it is actually necessary to add an of the marble filler used. This filler exhibits a high percentage
equivalent quantity to that of the limestone filler in of fine grains: 29% and 66% of the grains have sizes smaller
terms of the fine grain percentage. Finally, it can be than 2 μm and 10 μm, respectively. This marble filler fineness
concluded that the addition of such amount of leads to the majority of the grains being interposed between
marble filler to the SCC cementitious matrix affects the cement grains, and later the compactness increasing,
the horizontal flow of this type of concrete. which reduces the air content.
The results show that as the air content reduces, the fresh
The second test that identified the self-compacting
concrete density increases. This is due to the grain sizes of
properties of SCCS is the L-box test. According to the re-
the two fillers which make the marble filler consume water in
sults presented in Table 7, the h2/h1 ratio of SCCM and
terms of absorption and then make the SCC paste denser.
SCCL are 0.5 and 0.89, respectively. According to the re-
Consequently, the workability of SCC was affected by the air
quirements of NF EN 12350-10 [55], only SCCL exhibits an
content percentage. Thereafter, an increase in density
acceptable self-compacting ability to be classified as SF2 flow
conducts to an increase in viscosity and then to a decrease in
class, since the ratio is higher than 0.80. This is a conse-
workability [71]. Indeed, a higher SCC density results in a
quence of the increase in the SCCM viscosity due to its large
lower slump test value and in a slower horizontal flow. In
specific surface. It is also a result of the high density of the
addition, a lower air content percentage with the same water
SCCM (2440 kg/m3) compared to that of SCCL (2400 kg/
amount gives a lower segregation resistance [70].
m3). Indeed, a higher SCC density results in a slower
horizontal flow in the L-box and therefore a low h2/h1 ratio.
4.2. Effects of Marble and Limestone Filler on Compressive
4.1.2. Self-Leveling Properties. The self-leveling properties of Strength of SCC. This part of the study involves comparing
the two SCCs were identified by the V-funnel test. According the compressive strength of the concrete made with the
to the requirements of NF EN 12350-9 [56], the flow time marble filler to that of the concrete made with the limestone
must be between 8 and 14 s. Nonuniform concrete flow from filler. The purpose of this comparison is to evaluate the
the funnel suggests a lack of segregation resistance. effects of the marble filler on the SCC hardened properties,
A lengthy flow time may be a result of high paste vis- and more precisely, its compressive strength.
cosity, high interparticle friction, or flow blockage by coarse From the results displayed in Table 8, it is noted that the
aggregates. The V-funnel results are related to the concrete compressive strength values of the SCCM and SCCL are very
viscosity, passing ability, and segregation resistance; there- close at both young age and middle age. The compressive
fore, the test results may not identify the true cause of a strengths at 28 days are higher than the desired compressive
lengthy flow time [70]. strength of 30 MPa (39 MPa and 41 MPa for SCCL and
The results displayed in Table 7 indicate that the flow SCCM, respectively).
times of the SCCL and SCCM are 9.08 and 2.59 s, Furthermore, from the obtained results, high com-
respectively. pressive strength values were observed at a young age for
The rapid flow time of the SCCM is essentially a result of both concrete types (18 MPa and 21 MPa SSCL and SCCM,
its density. In fact, a higher SCC density leads to a faster respectively, at the age of 3 days). This increase is mainly
vertical flow. The difference in vertical flow between the two owing to the SP used, which provides the secondary function
concretes can also be explained by the difference in the paste of hardening acceleration.
volume. The SCCM has a lower paste volume than the SCCL Regarding long-term resistance, it is noted that SCCM
due to the differences in grain sizes and finesse of the two exhibits a higher compressive strength than the SCCL
fillers. Finally, it can be concluded that concrete with a (41 MPa vs 38 MPa). This can be explained by the results of
smaller paste volume has a faster flow velocity. Moreover, the tests carried out on the two concretes in the fresh state.
the addition of marble filler to SCC increases its vertical flow. The SCCM is less manageable than the SCCL, and therefore
On the other hand, the results presented in Table 7 its water-cement ratio was reduced, which allowed for its
indicate that the two tested concretes exhibit a high re- compressive strength to increase.
sistance to segregation, due to their milt loss percentages of However, the density value as well as air content per-
less than 15% (NF EN 12350-11 [59]). centage in SCCM allows us to conclude that this concrete is
more compact than the SCCL, and consequently, its com-
pressive strength is higher.
4.1.3. Air Content. Various adjustments are made to provide Likewise, as indicated in the previous section, the
the true air content, and the air content percentage of an granulometry as well as fineness of the marble filler plays a
SCC should not exceed 5%. very important role in improving the compactness in the
The results presented in Table 7 indicate that the two granular and cement matrix.
concretes, SCCL and SCCM, exhibit air content percentages Finally, the small difference in compressive strengths of
equal to 2.7% and 1.2%, respectively. These values dem- the two studied concretes is a result of the differences in the
onstrate that the two formulated SCCs have maximum fineness, particle size, and fine grain percentage of the two
compactness, without vibration or clamping. used fillers.
Advances in Materials Science and Engineering 9

Table 8: Compressive strengths of four SCCs at different ages. volume of capillary pores in concrete and significantly affects
Compressive strength (MPa)
the carbonation depth.
Concrete type In addition, the results show that the carbonation depth
1 day 2 days 3 days 7 days 14 days 28 days
of SCCM is lower than the carbonation depth of SCCL. This
SCC (limestone) 11 16 18 29 34 38 is can be explained by that when specific surface of filler
SCC (marble) 12 18 21 30 36 41
increases, porosity is decreased which results in decrease of
carbonation penetration depth.
4.3. Effects of Marble and Limestone Filler on Homogeneity and Finally, it can be concluded that the porosity affects the
Quality of SCC. The homogeneity and quality of the SCCM carbonation penetration depth of concrete and then its
and SCCL were evaluated by measuring ultrasonic pulse durability will be influenced. Also, the incorporation of
velocity. The velocity of an ultrasonic pulse is influenced by mineral filler in self-compacting concrete increases the
the properties of concrete. Indeed, the pulse velocity increases carbonation resistance of SCC compared to the ordinary
or decreases as the concrete compaction and the voids in concrete and their durability increase [73].
concrete change and thereafter the homogeneity and quality
change. The classifying of concretes are excellent, good, 4.4.2. Water Penetration Depth. Figure 5 shows how the
doubtful, poor, and very poor for (4500 m/s and above), penetration depth is taken into the one test specimen of each
(3500–4500 m/s), (2500–3500 m/s), (1700–2500 m/s), and tested concrete. The results show that the average water
(1700 m/s) and below velocity values, respectively [72, 73]. penetration depth values of the ordinary concrete, SCCL,
The results show that the ultrasonic pulse velocity values and SCCM are 22, 11, and 7 mm.
for the ordinary concrete, SCCL, and SCCM are 3820, 4535, Based on the obtained water penetration depth values,
and 4746 m/s, respectively. However, based on the pulse the ordinary concrete has the highest value of water pen-
velocity values, the ordinary concrete presents a good ho- etration depth, while the concrete SCCM has the lowest one.
mogeneity and quality but the two self-compacting con- This behavior also depends on the porosity of the concrete.
cretes SCCL and SCCM present excellent qualities and then Indeed, the water penetration depth increases with the
excellent homogeneities. This is due to the increase of the concrete porosity.
velocity value with the decrease of the concrete porosity. This Finally, there is a linear relationship between the water
can be deduced from the air content percentages of the penetration depth and the carbonation penetration depth of
tested concrete which is very low for SCCL and SCCM (2.7 concretes. Indeed, the two penetration depths increase with
and 1.2%, respectively) compared to that of the ordinary the concrete porosity. In addition, it can be concluded that
concrete which is about 8%. It can be clearly noted the the two self-compacting concretes SCCM and SCCL have a
beneficial use of marble powder and limestone powder as high durability compared to the ordinary concrete [74].
fillers in the SCC composition.
On the other hand, the higher velocity value of SCCM
compared to then of SCCL is also due to the low air content 4.5. Microstructure Analysis. Figure 7 presents the scanning
percentage compared to then of SCCL (Table 7) which led to electron microscopy (SEM) micrographs and energy-
increase in speed of ultrasonic pulse velocity wave. In ad- dispersive X-ray spectroscopy (XRD) patterns of cement
dition, the reason may be due to the lower porosity of SCCM paste at 28 days. According to the presented results, the
due to the higher Blaine specific surface of marble powder, hydrating in time of cement paste is composed mainly of
9459 cm2/g, compared to that of limestone powder, hydrated silicates of calcium (CSH) phase accompanied with
4405 cm2/g. a hydration products of calcium aluminate (ettringite) and
Higher specific surface of filler resulted in lower porosity calcium hydroxide (portlandite). The obtained portlandite
hence high compressive strength (Table 7). creates massive, hexagonal crystals.
In addition, researches have shown that CSH is the main
component and the most important factor affecting the
4.4. Effects of Marble and Limestone Filler on mechanical strength of hardening cement paste [66, 68].
Durability of SCC Figures 8 and 9 present SEM images and XRD patterns of
marble powder paste and limestone powder paste, re-
4.4.1. Carbonation Penetration Depth. The results show that spectively, at 28 days. According to the chemical analysis
the average carbonation penetration depths of the ordinary presented in Table 1, the major component of marble
concrete and the two self-compacting concretes SCCL and powder and limestone powder is the calcium oxide which
SCCM are 12, 4, and 1 mm, respectively. It can be seen that demonstrate the carbonate nature of these two powders.
the carbonation penetration depth of ordinary concrete is XRD patterns of marble and limestone pastes show that as
very higher than of the two SCCs. This is due to the higher expected calcite is the main crystalline mineral both in
volume of cement paste of SCCL and SCCM compared to marble and in limestone pastes, with significant peaks. In
the ordinary concrete. Indeed, the porosity of concrete addition, according to Figures 8 and 9, quartz is also
decreases when increasing the cement paste volume. It can identified in very low concentration for the two pastes.
be concluded that the carbonation depth increases with an Thereafter, according to the results of Table 1 and Fig-
increase of concrete porosity. Also, incorporating filler in ures 8 and 9, it is clear that marble and limestone powders do
self-compacting concrete tends to decrease the porosity and not possess any pozzolanic activity. Consequently, marble
10 Advances in Materials Science and Engineering

220
C2S
200 C3S
C4AF P
180 CSH C2S
C3S
C4AF
160 C CSH
140
Intensity (arb. units)

120 P
C3S
E
100 C2S
C3S
80
P E
60 C C3S
C C4AF
P E
40 E
E CSH
20

0
0 10 20 30 40 50 60
2θ (°)

C: calcite
E: ettringite
P: Ca(OH)2

Figure 7: SEM micrographs and XRD pattern of cement paste.

1600
C
1400

1200

1000
Intensity (arb. units)

800

600

400

C
200 C C C
C
C C
C Q
0
0 10 20 30 40 50 60
2θ (°)

C: calcite
Q: quartz

Figure 8: SEM micrographs and XRD patterns of marble powder paste.

and limestone powders can be considered as inert fillers, and and 11), it was remarked that CMP and CLP specimens are
so the hydraulic reaction of SCCM and SCCL will not be denser and less porous than cement paste specimen. This
modified or influenced. This last result confirms the ob- result indicates the refinement of the pore structure in CMP
tained results presented in Section 3. and CLP compared to the cement paste. In addition, it was
SEM micrographs and XRD patterns of cement-marble remarked that the microstructure of cement paste is a highly
paste (CMP) and cement-limestone paste (CLP) at 28 days porous with irregular micropores in cement matrix.
are presented in Figures 10 and 11, respectively. It was remarked also that CMP paste is more dense
According to SEM micrograph of cement paste (Fig- and less porous than CLP paste and even the concrete
ure 7) and SEM micrographs of CMP and CLP (Figures 10 SCCM is more denser and less porous than SCCL concrete.
Advances in Materials Science and Engineering 11

1600

1400 C

1200

Intensity (arb. units) 1000

800

600

400
C C
C CC
200
C
Q C
C
0
0 10 20 30 40 50 60
2θ (°)

C: calcite
Q: quartz

Figure 9: SEM micrographs and XRD patterns of limestone powder paste.

320
C
280

240
Intensity (arb. units)

200 P
C2S
C3S
160 C4AF
P

120 C
P
C4AF
80 E
C CSH
E C C C2S
CSH C3S P
40 E C3S E C
C2S

0
0 10 20 30 40 50 60
2θ (°)

C: calcite
E: ettringite
P: Ca(OH)2

Figure 10: SEM micrographs and XRD patterns of cement-marble powder paste “CMP.”

Consequently, the experimental values of the bulk densities marble powder or limestone powder in cement paste. As a
and the air content percentages of the two SCCS, presented conclusion, marble and limestone powders are inert mate-
in Table 7, are confirmed. Indeed, the rheological properties rials, and consequently, they do not lead to much change in
of SCC and more precisely the self-compacting and the self- the phase composition of the resultant mix of SCCM and
leveling properties depend on the fineness of the used filler. SCCL.
This confirms the obtained experimental data of slump test, XRD patterns show also that cement pastes and CMP
flow time, bulk density, and L-box (Table 7). and CLP pastes have the same portlandite peak. In addition,
In addition, the comparison of XRD patterns of the five the very fine needles of ettringite of CMP and CLP are less
pastes (Figures 7–11) indicate that there is no important than those of paste with cement alone. Also, the presence of
difference in calcium hydroxide (CH) contents for all pastes. fine needles in CMP is lesser than for CLP. This is due to the
Also, the comparison shows that there is no change in the high fineness of marble powder compared to that of lime-
phase composition qualitatively when incorporating both stone powder.
12 Advances in Materials Science and Engineering

320
C
280

240

Intensity (arb. units) P

200 C2S
C3S
C4AF
160
P
120 C
P
C4AF
80
C E CSH
E C C C2S
CSH C3S P E
40 E C3S C2S C

0
0 10 20 30 40 50 60
2θ (°)

C: calcite
E: ettringite
P: Ca(OH)2

Figure 11: SEM micrographs and XRD patterns of cement-limestone powder paste “CLP.”

Finally, the use of marble powder as a filler in the SCC (vii) Porosity affects the carbonation penetration depth
composition increases intruded pore volume, reduces per- of SCC and its durability. Additionally, the in-
centage of fine pores, and then increases compressive corporation of mineral filler in SCC increases its
strength of the SCCM compared to these of SCCL. This is carbonation resistance and its durability.
due to the fundamental relation between compressive (viii) There is a linear relationship between the water
strength and the void space and porosity distribution of penetration depth and the carbonation penetration
concrete [23]. This last result confirms the experimental depth of concretes. Indeed, the two penetration
compressive strength values, presented in Table 8, of the two depths increase with the concrete porosity. In
concretes SCCM and SCCL at different ages. addition, SCCM and SCCL have a high durability
compared to the ordinary concrete.
5. Conclusion (ix) XRD patterns indicate that marble and limestone
powders are inert since they did not lead to a
As a result of this experimental study, the following con- change in the composition of the resultant mix of
clusions can be made: SCCM and SCCL.
(i) The powder obtained from the sludge of marble (x) SEM micrographs show that the use of marble
blocks can be used as marble filler added to the powder as a filler in the SCC reduces porosity and
SCC cementitious matrix. thus increases the compressive strength especially
(ii) The two concretes, SCCM and SCCL, exhibit in the SCCM compared to SCCL.
satisfactory self-compacting properties in the fresh
state, thanks to their adequate filling capabilities Data Availability
and passing abilities.
(iii) The marble filler has a significant effect on fresh The data used to support the findings of this study are in-
concrete properties since it improves the vertical cluded within the article.
flow and increases the air content.
(iv) The two fillers have significant effects on the Conflicts of Interest
compressive strength, which was higher in the
The authors declare that they have no conflicts of interest.
SCCM.
(v) A strong correlation was observed between the fresh
and hardened SCC properties with the marble filler.
Acknowledgments
(vi) The speed of the ultrasonic pulse wave is higher in This project was supported by the Deanship of Scientific
the SCCM due to its low air content, compared to Research at Prince Sattam bin Abdulaziz University under
the SCCL. the research project no. 2017/01/7296.
Advances in Materials Science and Engineering 13

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