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Construction and Building Materials 165 (2018) 321–332

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Construction and Building Materials


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Utilization of marble powder as fine aggregate in mortar mixes


K.I. Syed Ahmed Kabeer ⇑, Ashok Kumar Vyas
Department of Civil Engineering, Malaviya National Institute of Technology, Jaipur 302017, India

h i g h l i g h t s

 Dried marble slurry waste was evaluated as a potential substitute of river sand in mortars.
 Marble slurry helps reduce required water content to prepare cement sand mortars.
 Marble slurry hastens the hydration reaction and forms calcium carboaluminates.

a r t i c l e i n f o a b s t r a c t

Article history: The construction industry has been responsible for plaguing the environment due to ecological imbalance
Received 26 September 2017 caused during the extraction and production of building materials. To make this production of construc-
Received in revised form 24 December 2017 tion materials cleaner, the dependency on natural resources has to be reduced. With this aim, marble
Accepted 9 January 2018
powder which is a waste product generated during cutting and shaping of marble blocks has been eval-
uated as a replacement of conventional river sand in cement mortars. For this, four different mix propor-
tions of mortars were evaluated in terms of workability, drying shrinkage, compressive strength, bond
Keywords:
and adhesive strengths, density, water absorption and dynamic Young’s modulus. Results show that mor-
Mortar
Marble powder
tar mixes with 20% substitution of river sand by marble powder can be used for masonry and rendering
Masonry purposes. Such mortars have a distinctively dense microstructure which is a consequence of reduced
Rendering water requirement and formation of superior quality of hydration products. These were confirmed by
Sustainability scanning electron microscope, thermogravimetric analysis and Fourier transform infrared spectroscopy
techniques. Hence, by replacing sand to the tune of 20% by marble powder, would enable the construction
industry to reduce their dependency on river sand. Additionally, by utilizing this non-biodegradable mar-
ble waste as a building material, would reduce the burden on landfills and therefore help the marble
stone industry to be more sustainable.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction endangered aquatic biodiversity and cause skin, eye and kidney
diseases in humans [5]. On understanding the gravity of this prob-
For a country like India which has 1931 Mega tonnes of marble lem, researchers all over the globe have tried to provide a possible
resources still left to be exploited [1] has already been plagued solution for such waste disposal issues in their respective
with waste disposal problems associated with the marble mining countries.
and processing [2]. Based on the mechanism used for sawing, Usage of marble fines in production of concrete has been dealt
grinding and polishing, the marble slurry generated is about extensively. Alyamac and Aydin (2015) reported that the marble
10%–22% of the stone block [3]. The generated slurry is indiscrim- sludge can be used in place of river sand for up to 40% in concrete
inately dumped on vacant lands, river banks or forest areas. These with a w/c ratio of 0.6. They pointed out that workability reduced
slurry particles are fine enough to fill the pores of the soil, which with increase in marble incorporation. Compressive strength had a
can prevent water percolation and reduce its fertility. On drying, peak at 20% substitution which was 5% more than control mix [6].
these particles are lifted by air and can result in respiratory prob- For concrete mixes with a w/c of 0.5, Hebhoub et al. (2011) had
lems in humans [4]. Uncontrolled disposal of marble industrial presented that maximum compressive strength was obtained at
effluents had also led to increase in pollutants in groundwater, 50% substitution of river sand by marble waste (23.65% more than
the concrete mix made with conventional fine aggregate) [7].
Demirel in 2010 used marble waste of dolomite origin which
⇑ Corresponding author. was finer than 0.025 mm to replace sand of same size in concrete
E-mail address: 2014rce9549@mnit.ac.in (K.I. Syed Ahmed Kabeer).

https://doi.org/10.1016/j.conbuildmat.2018.01.061
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
322 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

with w/c of 0.51. Compressive strength of mixes with marble sub- centages (0–100%) in place of river sand. By finding an optimum
stitution showed a positive trend with 100% substitution showing substitution percentage of sand by marble powder in mortars apart
the best performance [8]. The pioneer of incorporating marble from concrete alone would enable the construction industry to fur-
waste in concrete products, Hanifi Binici in his work Binici et al. ther reduce sand mining and hence minimize the environmental
(2007) investigated the effect of using marble dust in a concrete problems associated with it [17]. This would also help the marble
of mix ratio 1:1.5:2. On testing, it was seen that compressive processing industry to be more sustainable by finding an additional
strength increased with increase in substitution, with 15% substi- utilization of such non bio-degradable waste. With the above set
tution recording the highest value [9]. targets, mortars were prepared with aim of utilizing the same for
Studies of inclusion of marble powder as fine aggregate in med- rendering and masonry purposes. Evaluation was done in terms
ium strength concrete have been carried out by Aliabdo et al. of workability, compressive strength, bond and adhesive strength,
(2014) and Silva et al. (2013) [10,11]. Compressive strength for water absorption capacity, fresh and hardened density, stiffness
all substitutions decreased, the maximum reduction was for and drying shrinkage. The experimental program of these tests is
100% substitution with a difference of 20% when compared to river detailed in the following section.
sand [11]. On the contrary Aliabdo et al. (2014), quoted that com-
pressive strength was more than control (the concrete mix with 2. Materials and methods
conventional materials) for the maximum substitution of 15% for
sand replacement, peak was obtained at 10% substitution for both Portland pozzolana cement complying with IS 1489 (1991) [18]
w/c ratios of 0.4 and 0.5 [10]. Ural et al. (2013) replaced sand in was used. The specific gravity was found to be 2.9 with loose bulk
proportions 5, 10, 15%. Peak values of compressive strength (17% density 1100 kg/m3 and specific surface area of 0.361 m2/g. Fine
than concrete mix made with river sand) was obtained at 5% sub- aggregate in the form of river sand was procured from a local
stitution which was due to the filler effect of marble dust [12]. dealer in Jaipur, Rajasthan, India. In Fig. 1, an analysis of particle
With regard to mortars, Khyaliya et al. (2017) had tested the size distribution is presented, where it can be seen that river sand
utilization of marble fines (mining waste) as a replacement for fine used in this study satisfies the stipulations of fine aggregate
aggregate in a lean mortar mix of 1:6. Due to thixotropic property required for plaster [19] and masonry mortar [20].
of marble, a substitution of 50% of river sand by marble powder Wet marble sludge was acquired from a firm which processes
required lesser water than the control mix. Eventually the same marble slabs in an industrial area of Jaipur. The slurry was sun
mix gave best performance in terms of compressive strength. How- dried, hammered to reduce the dried blocks to a powder passing
ever, drying shrinkage and water absorption of these mixes were through 1.18 mm sieve. The physical properties like specific grav-
same. This was because of increased porosity of marble substituted ity, bulk density and water absorption [21] and fineness modulus
mix when compared to the control mortar. Consequently this [22] (as a percentage of oven dried weight) of sand are presented
increase in porosity also meant utilisation of marble powder had in Table 1. For marble powder in addition to specific gravity and
to be limited to only 25% when there is susceptibility of attack bulk density, specific surface area and plastic limit [23] were iden-
from sulphate and acidic agents [13]. Earlier in 2014, Kelestemur tified and listed in the same table. Table 2 lists out the chemical
et al.’s study directed at evaluating the utilisation of marble sludge composition of river sand and marble powder used. The X-ray
of both dolomite and calcite origin, proved that marble aggregates diffraction pattern for marble powder is shown in Fig. 2. SEM
finer than 0.25 mm help increase compressive strength of mortars micrographs were also be taken to study the particle shape and
[14]. Rai et al. (2011) investigated the effect of marble granules as a texture also Fig. 3.
replacement of fine aggregate in mortar and concrete. Replacement On particle size analysis, 50% of marble powder particles were
was done by weight in variations of 5, 10, 15 and 20%. Mix ratio of found to be smaller than 49.68 mm with a surface area of 0.35
mortar was 1:3 and concrete mix was designed for a 28th day char- m2/g. This shows that marble powder is as fine as conventional
acteristic strength of 38 MPa. On testing, mortars and concrete mix cement. The oxide compositions of sand and marble presented in
specimens attained a peak compressive strength for 10% and 15% Table 2 shows that marble has significant amount of magnesium
substitution respectively [15]. Corinaldesi et al. (2010) character- and calcium ions.
ized marble powder generated from marble shaping and cutting On conducting X-ray diffraction analysis marble powder was
industry with a view of using the same in mortars and concrete. found to consist of calcium and magnesium carbonate predomi-
Rheological parameters of this slurry were evaluated by preparing nantly in the form of dolomite crystals indicated by the peak at a
cement pastes in which cement was replaced by 10 and 20% levels diffraction angle of 31.027°. The Indian Bureau of Mines (2015),
with and without super-plasticizing admixture with two w/c ratios classifies marble to be of crystalline nature. From the SEM micro-
of 0.4 and 0.5. It was reported that presence of marble powder
improved cohesiveness necessary for self-compacting concrete.
Marble powder also improved segregation resistance. Thixotropy
100
values of cement pastes with marble powder are high too, indicat-
ing better flow through narrow sections was possible when the
80
Percentage Passing

fresh mixes are set in motion. They also evaluated compressive


strength of cement sand mortars of 1:3 proportions. Marble slurry
60
was used in place of cement and sand, 10% by mass. These mixes
Sand
had the same flow value. There was fall in compressive strength
40 Upper limit
by 20% when cement was replaced, and 10% when sand was
replaced. They concluded that marble slurry played the role of filler Lower limit
20
and showed no sign of taking part in the hydration process [16].
From the above literature survey it can be safely pointed out
0
that marble slurry has been tested as fine aggregate relatively to
0.1 1 10
a lesser extent for utilization in mortars than concrete. Hence there
Particle size (mm)
is scope for evaluation of performance of mortar mixes with a wide
range of mix proportions (1:3, 1:4, 1:5 and 1:6) with dried marble Fig. 1. A comparative statement of particle size distribution of river sand with the
slurry (in the form of marble powder) at different substitution per- required specifications.
K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332 323

Table 1
Physical properties of river sand and marble powder.

Fine aggregate Apparent Specific gravity Loose bulk density (kg/m3) Water absorption (%) Fineness modulus Plastic limit (%) Specific surface area (m2/g)
River sand 2.67 1560 9.89 2.13 – –
Marble powder 2.7 1380 – – 18 0.35

Table 2 Flow value was measured using the vibrating flow table. Mortar
Chemical composition of river sand and marble powder. mixes were filled in a mould of standard size in three layers. The
Radical River sand Marble powder mould was lifted and vibrating table was dropped 25 times in 15
SiO2 94.97 1.57
s. The resulting increase in diameter of the mortar represented as
CaO 1.4 32.19 a percentage of original inner base diameter of the mould was rep-
MgO 0.3 19.85 resented as the flow value. Water content for all the four series of
Al2O3 – 0.18 mortars was so adjusted such that all mixes attained a flow value
Fe2O3 1.99 1.18
of 105% to 115%. With this water content, quantities of other mate-
rials to produce 1 m3 of mortar are listed in Table 3.
Fresh bulk density, compressive strength, porosity, dynamic
modulus of elasticity, tensile bond strength, adhesion to substrate
and drying shrinkage were evaluated. Compressive strength,
porosity and dynamic modulus of elasticity were evaluated after
twenty-eight days of water curing. Specimens for evaluating dry-
ing shrinkage were moist cured (maintained at a temperature of
23 ± 2 °C and a minimum relative humidity of 95%) for 72 h after
which initial reading was noted. Drying shrinkage was monitored
every seventh day from the day of casting for four weeks, then
every month subsequently for five months. Bond strengths were
determined by conditioning the samples to a temperature 20 ± 2
°C and a RH of 50 ± 5% for 28 days. Details regarding the specimen
size and numbers with the applicable standards for these tests are
listed in Table 4.
Characterization of the microstructure of the mortar mixes (A0,
A20, A40 and A60) was done by scanning electron microscopy
(SEM), Fourier-transform infrared spectroscopy (FTIR) and
thermo-gravimetric analysis techniques (TGA/DTA). FTIR was con-
ducted on pellets made by powdered mixtures of mortars samples
and potassium bromide using a PerkinElmer Spectrum with a scan
Fig. 2. X-ray diffraction pattern of marble powder. range of 4000–400 cm 1. TGA/DTA was conducted in a nitrogen
atmosphere on the powdered mortar mixes using a PerkinElmer
where the samples were heated up to 900 °C with a rate of 10
graphs it is clearly seen that sand particles are smooth and round °C/min. The results of all the above conducted tests are discussed
whereas marble powder have rough texture with irregular shape in the following section.
[1].
Mortar mix proportions of 1:3, 1:4, 1:5 and 1:6 (cement: fine 3. Results and discussions
aggregate) by volume were chosen. These proportions are named
A, B, C and D respectively. Sand was replaced by marble powder 3.1. Workability
from 0% to 100% in steps of 20%. Substitution percentage of river
sand was suffixed to the series name. For e.g. B0 would indicate The water requirement of mortars to attain the desired flow is
proportion 1:4 with no marble powder and C40 would indicate shown in Fig. 4. For the mix A, w/c ratio for control mix is 0.9,
proportion 1:5 with 40% substitution of sand. One mix proportion but when sand is completely replaced by marble powder (mix
with 0% to 100% marble powder constitute a series. A100), the w/c ratio has increased to 1.61 which is 79% more than

Fig. 3. SEM micrographs of a) marble powder and b) river sand.


324 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

Table 3
Quantities of materials required to produce 1 m3 of mortar.

Designation Substitution of sand (%) Cement (kg) Sand (kg) Marble powder (kg) Water (kg)
A0 0 356 1517 0 320
A20 20 356 1213 268 303
A40 40 356 910 536 360
A60 60 356 607 804 434
A80 80 356 303 1072 509
A100 100 356 0 1340 573
B0 0 274 1556 0 334
B20 20 274 1245 275 304
B40 40 274 934 550 351
B60 60 274 623 825 416
B80 80 274 311 1100 490
B100 100 274 0 1375 562
C0 0 220 1562 0 352
C20 20 220 1250 276 297
C40 40 220 937 552 328
C60 60 220 625 828 403
C80 80 220 312 1104 477
C100 100 220 0 1380 552
D0 0 190 1619 0 342
D20 20 190 1295 286 287
D40 40 190 971 572 314
D60 60 190 648 858 399
D80 80 190 324 1144 475
D100 100 190 0 1430 551

Table 4
Details of the tests carried out on mortar mixes.

Parameter Reference standard Specimen size No. of specimens


Flow value [24] – –
Bulk density of fresh mortar [25] – –
Compressive strength [26] 50 mm cube 3
Bulk and apparent density, water absorption by immersion, percentage of permeable voids [27] 70 mm cube 3
Ultrasonic pulse velocity and dynamic modulus of elasticity [28] 160  40  40 mm prism 3
Tensile bond strength [29] Brick couplets 6
Adhesion to substrate [30] Bricks 3
Drying shrinkage [31] 25  25  250 mm prism 5

tution is greater than 20% for these two series. Whereas for series C
2.80 and D, a substitution greater than 40% results in greater water
demand when compared to the corresponding control mixes.
The characteristic variation in water required to attain the
2.30 required workability of marble incorporated mortar mixes can be
because of a distinguishing thixotropic nature of marble powder
[16]. This would be the reason why mortar mixes with 20% to
w/c

1.80 40% substitution of river sand appear to be stiff but flow easily
when a force is applied. This fall in water requirement is actually
a consequence of fall in rheological parameters of the mortar
1.30
mixes, where this dolomitic marble powder plays a role of a weak
super-plasticizer [32]. The reduction may also be due to the fact
that marble powder fills in the voids which were previously occu-
0.80
0 20 40 60 80 100 pied by water, hence imparting necessary consistency at lower w/c
Substituion of sand by marble powder
ratios [33].
Beyond 20–40% substitution of river sand, the thixotropic prop-
A B C D
erty and pore filling effect seem to be overcome by fineness of mar-
Fig. 4. Water requirement of mortars to attain the desired flow value of 105% to ble powder. Initially the voids left between the large sand particles
115% provide large internal friction resulting in high plastic viscosity.
When powder is added, these occupy the voids helping reduce
internal friction and consequently plastic viscosity. When the pow-
the control mix A0. However mix A20 requires 5.6% lesser amount der content is increased further, their surface area starts playing a
of water to attain the same flow value. The same pattern of results dominating role which in return increases plastic viscosity. Hence
are obtained for the other three mix proportions also. Here too, mixes with fines content greater than 20% for series A and B and
least amount of water is required when marble powder is used 40% for series C and D require more water to achieve consistency
to substitute 20% of river sand which is lesser by 9%, 15.6% and equal to that of mortars with coarser river sand [34].
16% for B0, C0 and D0 control mixes respectively. When compared Water absorption (represented as plastic limit) of the marble
to control mortars A0 and B0, more water is required when substi- powder is high when compared to the river sand. This could also
K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332 325

be responsible for the increase in water requirement when incor- tively. For all the mixes, drying shrinkage has increased when mar-
poration of marble powder is increased. A similar case of reduced ble content has been increased from 0 to 100% substitution. This
flow diameter has been reported where fly ash with higher water performance is noticed from the beginning of the exposure period.
absorption capacity was used to replace sand [35]. It is also under- At 20% substitution, drying shrinkage of mortar mixes is equal to
stood that when spherical and smooth river sand particles are the control mortar A0, B0 and D0. For the series C, at the same per-
replaced by marble powder particles which are rough and irregular centage utilisation of marble powder, drying shrinkage is greater
in shape, aid in increasing mortars’ viscosity [36]. This is another Figs. 7 and 8.
contributing factor to increased water demand. Since, drying shrinkage is a consequence of loss of water from
the mortar mixes, marble incorporated mixes have greater water
3.2. Fresh bulk density content when compared to their corresponding control counter-

The variation of fresh bulk density with increase in substitution


of river sand by marble powder is as shown in Fig. 5. For all the four
0.0018
mixes, maximum density is obtained at 20% replacement of river
0.0016
sand. This peak might be because of the fact that, marble powder

Drying Shrinkage (%)


has the ability to fill the voids formed between sand and cement. 0.0014
Also water content for this mix is the least when compared to other 0.0012
substitutions. At 40% incorporation of marble powder, the density 0.001
is equal or greater than the corresponding control mixes. On fur-
0.0008
ther increase there is steady decline, and the least fresh density
is seen at complete substitution of river sand. This decrease is a 0.0006
consequence of variation in water content, which increases with 0.0004
increase in marble powder content. Molnar & Manea (2016) have 0.0002
also reported that the least density was obtained when sand was 0
completely substituted by marble slime [37]. 0 20 40 60 80 100 120 140 160
Days
3.3. Drying shrinkage B B20 B40 B60 B80 B100

Variation of drying shrinkage with increase in marble powder Fig. 7. Drying shrinkage of series B.
utilisation has been plotted in Figs. 6–9 for series A to D respec-

2.25 0.0018
0.0016
2.20
Drying Shrinkage (%)
Fresh Bulk Density (g/cc)

0.0014
2.15
0.0012
2.10 0.001
2.05 0.0008
2.00 0.0006

1.95 0.0004
0.0002
1.90
0
1.85 0 20 40 60 80 100 120 140 160
0 20 40 60 80 100 Days
Percentage substitution of sand by marble powder
C C20 C40 C60 C80 C100
A B C D
Fig. 8. Drying shrinkage of series C.
Fig. 5. Variation of fresh bulk density of mortar mixes.

0.002 0.0016
0.0018 0.0014
0.0016
Drying Shrinkage (%)

Drying Shrinkage (%)

0.0012
0.0014
0.001
0.0012
0.001 0.0008
0.0008 0.0006
0.0006
0.0004
0.0004
0.0002
0.0002
0 0
0 20 40 60 80 100 120 140 160 0 20 40 60 80 100 120 140 160
Days Days
A A20 A40 A60 A80 A100 D D20 D40 D60 D80 D100

Fig. 6. Drying shrinkage of series A. Fig. 9. Drying shrinkage of series D.


326 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

parts, and this might be the reason why their drying shrinkage is Finally, these considerations direct us to evaluate the reactive
greater than the corresponding control mixes [35]. However, mixes nature of marble powder. Marble in the form of dolomite mineral
with 20% substitution of river sand of all mixes have water content can also aid in reducing the nucleation barrier for the formation of
lesser than that of corresponding control mixes. This should have calcium hydroxide which accelerates the hydration process [32].
made these perform better than the corresponding control mixes. This calcium hydroxide thus formed has the capacity to react with
But since drying shrinkage is also dependent on aggregates surface carbonate rock to form carbonate hydrates [42]. Additionally, with
area [38], the positive effect due to reduced water content has been the primary hydration reaction accelerated, calcium hydroxide is
negated by powder’s fineness. The fall in drying shrinkage from available sooner for the fly ash in the PPC to react and form calcium
rich (A) to lean (D) series can be because of lesser cement content aluminatesilicate hydrates [43]. The strength gain by these reac-
[39]. tions is so significant that it overcomes the negative effect of
greater water cement ratio in mortar mixes up to 60% substitution
3.4. Compressive strength of marble powder as fine aggregate. The nature of the products
formed are discussed under the microstructure subhead. But when
The compressive strength values of mortar mixes after twenty- marble powder is used to substitute more than 60% of sand, the
eight days of water curing is plotted graphically in Fig. 10. Maxi- pores formed due to excess of water is sufficient enough to reduce
mum resistance to compression is exhibited by mixes having 20% the compressive strength. Similar results were reported by Khya-
substitution of river sand by marble powder. The increase in com- liya et al. (2017) where mortar mixes with dolomitic limestone
pressive strength at this substitution for mixes A20, B20, C20 and marble had recorded greater strength despite the fact that they
D20 is 24%, 49%, 53% and 91% when compared to their control mor- had greater water content in them [13].
tars A0, B0, C0 and D0. At complete substitution the compressive
strength of mixes A100, B100, C100 and D100 is lesser than the
corresponding control counterparts (A0, B0, C0 and D0). 3.5. Tensile bond strength between brick and mortars
The variation in strength across a same series for various sand
replacement ratios may be because of combination of several fac- The change in tensile bond strength is similar to the variation
tors. Primarily as seen from Fig. 10 mixes A20, B20, C20 and D20 seen in compressive strength with increasing proportion of marble
have lesser water cement ratios than their corresponding control powder in mortars. This variation is plotted in the form of a graph
mortars. It is very well understood that for a given cement content, in Fig. 11. For mixes of proportion of 1:3 and 1:4, maximum
lesser the water cement ratio greater is the strength [34]. Thus this strength was obtained for mixes A20 and B20. For lean proportions
gain in strength is noticed. The subsequent fall in strength of mixes of 1:5 and 1:6 best performance was obtained at 40% substitution
with marble content greater than 20% can hence be justified for the of sand by marble powder. When marble powder content was
same reason of higher water content in these mixes. However a increased beyond 20% for A and B series and 40% for C and D, ten-
good number of marble incorporated mixes having same or greater sile bond strength reduced. This fall was gradual for series A, while
water cement ratio have greater compressive strength when com- for series B, C and D it was significant. For series A, any substitution
pared to the mortars with only sand. greater than 20% had strength lesser than the control mortar,
It has been reported that when marble powder is used to whereas for series B, B0 and B60 had almost similar strength. Jus-
replace cement [40] or sand [14], has the ability to fill pores which tifiably, for series C and D all mixes with marble powder have
in turn improves compressive strength. But this effect is only pos- strengths greater than C0 and D0 respectively.
sible at lower substitutions of cement to the range of 5% to 15% The rise and fall of this parameter can be correlated to three
[40]. In case of sand, 50% of fine sand which is a part of larger grad- controlling parameters: fineness of aggregate [44], water content
ing curve could be substituted to achieve pore filling effect [14]. In and water retention capacity of mortar mixes [45]. It has been
the present study greater strength is achieved even at 60% to 80% reported that by increasing the fineness of aggregate, tensile bond
substitutions also. At such high proportions, marble powder parti- strength reduces. Hence incorporating marble powder in place of
cles are in excess of the voids which exist between cement and sand can be one of the reasons behind reduction in performance.
sand particles. Also, sand used here contains sufficient fines Secondly, the strength of this bond is dependent on the ability of
already. When in excess these sand and marble fines would push hydration products to develop a mechanical bond by penetrating
apart each other leading to reduction in packing density and lesser into the brick due to its water absorption capacity [45]. Since the
compressive strength [41]. Hence the pore filling effect has to be bricks used here were pre-wet before application of mortar, water
downplayed. Voids calculation data presented in subsequent sec- retention capacity of mortar mixes should play a dominant role. It
tion substantiate this claim. can be concluded that, by incorporating marble powder in the

14.00 0.30
Compressive strength (MPa)

Tensile bond strength (MPa)

12.00 0.25

10.00
0.20
8.00 A A
0.15
6.00 B B
C 0.10 C
4.00 D D
2.00 0.05

0.00 0.00
0 20 40 60 80 100 0 20 40 60 80 100
Percentage substituion of sand by marble powder Percentage substituion of sand by marble powder

Fig. 10. Twenty-eighth day compressive strength of mortar mixes. Fig. 11. Variation of tensile bond strength for all mixes.
K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332 327

mixes, water retention capacity of mortar mixes must be increas- 2.10


ing. Conversely the accelerated hydration due to the inclusion of
marble has taken a toll on free water available. This would have 2.00

Bulk density (g/cc)


negatively affected the growth of bond between mortar and the
brick. 1.90
A
1.80
3.6. Adhesive strength of renderings on substrates B

1.70 C
The variation of adhesive strength of mortars when applied as a D
rendering on substrates is similar to compressive strength and ten- 1.60
sile bond strength. The strength values are tabulated in Table 5.
Here the type of failure of brick – mortar bond is also noted. As 1.50
0 20 40 60 80 100
we move from rich to lean mixes, mode of failure changes from
failure of mortar to failure at interface. This might be because of Percentage substituion of sand by marble powder
insufficient hydration products developed at the interface due to
Fig. 12. Variation of hardened bulk density of mortar mixes.
a lower cement content. For a given series, with varying substitu-
tion of marble powder, strength seems to peak out at 20% substitu-
tion. Further increase in marble powder content in mortar mixes 2.70
reduces the adhesive strength. For series A, B, C and D, comparable
strengths are obtained between A0, B0, C0 and D0 and A40, B60, 2.65

Apparent density (g/cc)


C80 and D80. Farinha et al. (2012) had evaluated the effect of cera-
2.60
mic wastes on adhesive strength. They had concluded that ceramic
wastes improved the penetration of the hydration products into A
2.55
the substrate and hence at a substitution level of 20% of river sand, B
improved adhesive performance was achieved [33]. Hence here too 2.50 C
the performance advantage can be credited to the ability of the D
hydration products to penetrate into the bricks. With marble’s 2.45
capacity to accelerate hydration process, the strength gain of the
hydration products as well as the mechanical bond between the 2.40
0 20 40 60 80 100
mortar and brick has improved. Molnar and Manea (2016) has also
recorded a 160% increase in adhesive strength to the support layer Percentage substituion of sand by marble powder
when calcite marble was substituted in place of 25% of river sand Fig. 13. Variation of apparent density of mortar mixes.
[37]. Adhesive strengths could not be determined for mixes C100
and D100 mixes because the specimens were damaged during
the operation of core cutting or even before the load could be 35.00
applied.
30.00
Water absorption (%)

3.7. Density, water absorption and porosity 25.00


A
The variations in hardened bulk density, apparent density, 20.00
B
water absorption by immersion and permeable pore space of mor-
C
tar mixes due to substitution of sand by marble powder are graph- 15.00
ically represented in Figs. 12–15 respectively. It can be seen that D

bulk density (includes volume taken up by permeable voids also) 10.00


is maximum at 20% substitutions for all mix proportions as pre-
5.00
dicted by fresh density values shown in Fig. 5. This increase in bulk 0 20 40 60 80 100
density can be because mortars with this percentage of marble
Percentage substituion of sand by marble powder
powder have lesser water cement ratio or greater extent of hydra-
Fig. 14. Variation of water absorption capacity of mortar mixes.
Table 5
Variation of adhesive strength of mixes on substrate.
50.00
Mix/Substitution Adhesive strength (MPa)
45.00
A B C D
Permeable voids (%)

0% 0.33 0.16 0.12 0.10 40.00


F F E E
20% 0.46 0.38 0.28 0.20 35.00 A
F F E E
30.00 B
40% 0.41 0.27 0.20 0.18
F E E E C
60% 0.27 0.26 0.20 0.13 25.00 D
E E E E
20.00
80% 0.26 0.13 0.12 0.09
F E E E
15.00
100% 0.18 0.14 Cannot be 0 20 40 60 80 100
E E determined
Percentage substituion of sand by marble powder
E Adhesive fracture: fracture at the interface of mortar and substrate.
F Cohesive fracture: fracture in the mortar itself. Fig. 15. Variation of permeable pores space of mortar mixes.
328 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

tion. At higher substitutions there is a steady decline of this param-

Dynamic modulus of elasticity (MPa)


30000
eter. For series A and B, A40 and B40 have lesser bulk density than
A0 and B0, for series C and D, 40% sand substituted mixes have 25000
equal or higher density than their control mortars. On complete
substitution, the density of mortar mixes has reduced by 18 to 20000
20% for the different mix series. With reduction in density, dead A
15000
load coming on the structures will be lesser as seen by the utilisa- B
tion of fly ash as fine aggregate in mortars [35]. 10000 C
Apparent density (does not include volume taken up by perme- D
able voids) increases with increase in marble substitution. The 5000
extent of rise of apparent density when 20% sand was substituted
by marble powder is between 3% and 6% for all the mixes. It has 0
0 20 40 60 80 100
been reported that for a given volume of cement, volume of the
hydration product increases with degree of hydration and reduc- Percentage substituion of sand by marble powder
tion in water cement ratio [46]. Along with reduced water cement
Fig. 16. Variation of dynamic modulus of elasticity of mortar mixes.
ratio at 20% substitution and marble powder’s capacity of acceler-
ating the hydration process, has led to the increase in apparent
density. It is understood that failure of a cement composite is ini-
tiated by the crack development in the cement matrix [39]. The greater substitutions, there is a steady fall in this parameter with
increase in density of the hydration products have reduced the the minimum value attained for A100, B100, C100 and D100. The
generation, propagation and connections of cracks when loaded. reduction is about 65.5%, 46.7%, 26.5% and 31.4% for the same
This could have imparted greater resistance to compression to mixes when compared to A0, B0, C0 and D0 respectively. Similar
mixes even at greater water cement ratios as seen in Fig. 11. Gal- fall of this parameter was noticed when limestone was used as fine
lucci et al. (2013) have established the relation that greater the aggregate in mortars [28]. This fall was correlated to the variation
apparent density, higher is the degree of hydration or vice versa of porosity of mortars. Because lower the bulk density, lower is the
[47]. Similar modification to mortars density was noticed when Young’s modulus [50].
metakaolin was used in mortar preparations which led to the for-
mation of sodium aluminosilicate hydrate [48]. Khyaliya et al. 3.9. Microstructure
(2017) have also indicated similar increase in apparent density of
mortar matrix on inclusion of marble fine aggregate [13]. From the above results it can be seen that all the four series of
The negative effect of increased water cement ratio is noticed mixes have similar variation in mechanical and physical properties
beyond 60% substitution of river sand which negates the effect of for the same substitution level of river sand by marble powder. At a
accelerated hydration. Though the cement matrix is dense enough, substitution level of 20% of river sand, mortar mixes have better
the presence of excessive permeable voids hastens the crack prop- performance than the control mortar mix, whereas at 40% and
agation and connections of cracks. Hence this might be the reason 60%, the performance was same and worse respectively. Hence
for the fall in strength of these mixes with 60% or greater marble the study regarding the changes in microstructure was limited to
powder incorporation indicated earlier. these four mixes of series A only. The scanning electron micro-
The variation of water absorption and permeable pore space fol- graphs for the mixes A0, A20, A40 and A60 are shown in two mag-
low the same pattern as seen in the changes of hardened bulk den- nification levels. Fig. 17 shows the presence of air voids in mortars
sity. These have been graphically represented in Figs. 14 and 15. At mixes. Due to the spherical nature and size of these voids (200
20% substitution, water absorption is equal or marginally higher mm), they must be due to entrained air. Cohesive mixes (A20) have
than the corresponding control mixes for all series. This is despite more tendency to hold entrained air, and this capacity decreases
the increase in bulk density at the same substitution ratio. Primar- with increase in fine content (A60) [39]. Presence of such air voids
ily this is because of the greater water absorption capacity of mar- in mix A20 might be the reason behind the increased water absorp-
ble powder than river sand or excessive cohesive nature of mortar tion capacity despite the fact that it has lesser water content than
mix. Consequently this has increased the porous volume of this A0 as seen from Figs. 4 and 14. From Fig. 18 it can be seen that mix
mix. This is similar to what was reported on the utilisation of con- A20 clearly is the densest and the area surrounding the sand grains
struction and demolition waste as fine aggregate in mortars [49]. is also homogenous.
At complete substitution the water absorption capacity stands Mass loss pattern (TGA), differential thermogravimetric plots
27%, 28.4%, 28.5 and 27.3% for A100, B100, C100 and D100 which (DTA) and heat flow pattern of the mortar mixes are shown in
is greater by 131.6%, 142.6%, 128.1% and 112.3% when compared Figs. 19–21 respectively and whereas Fig. 22 shows their FTIR spec-
to A0, B0, C0 and D0. tra. From the Fig. 19 it can be seen that there is considerable loss in
mass post 700 °C mark. This is due to the decomposition of dolo-
3.8. Dynamic modulus of elasticity mite mineral present in marble incorporated mortars (A20, A40
and A60) [51]. While in A0 it can be due to carbonation of port-
Similar to compressive strength, dynamic modulus of elasticity landite which has led to the formation of calcite [52]. For clarity
also attains a peak at 20% substitution of river sand by marble pow- purposes the region above 600 °C has been not discussed in the
der as seen in Fig. 16. At this substitution, increase in elasticity DTA plots. From Fig. 20 it can be seen that there are four major
modulus is around 17.1%, 34.6%, 67.6% and 107.1% when compared events occurring at around 100 °C, 250 °C, 400 °C and 460 °C. These
to A0, B0, C0 and D0 mixes respectively. This increase in modulus are due to the dehydration of C-S-H [10], hexagonal hydrates of Al
of elasticity signifies that, when loaded, mortars with 20% marble [53], C-A-S-H [43], and Ca(OH)2 [51] respectively. From the inten-
powder will undergo lesser deformation for the same stress. Con- sity of the trough formed at 100 °C it can be concluded that the
versely it will attract greater stress for the same strain values. amount of C-S-H formed in marble incorporated mortar mixes is
Hence it becomes important to judge the compatibility of these always higher than A0, which substantiates the claim that dolo-
mixes with the masonry blocks and substrates when used as mor- mite is capable of accelerating the hydration of C3S [32]. The event
tars or rendering respectively [33], especially for the mix A20. For taking place at 250 °C in A0 mix which is characteristic of decom-
K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332 329

A0 A20

A40 A60

Fig. 17. Scanning electron micrographs of mixes A0, A20, A40 and A60 showing presence of air voids in marble incorporated mortar mixes.

A0 A20

A40 A60

Fig. 18. Scanning electron micrographs of mixes A0, A20, A40 and A60 showing the nature of interfacial transition zone and density of the microstructure.

position of hexagonal and cubic hydrates of Al, goes missing in teristic dips at around 1430 cm 1 and 877 cm 1 can be associated
A20, A40 and A60 mixes. This is because carbonate rocks are cap- with marble [55] or carbonates [56] arising due to carbonation of
able of retarding the hydration of C3A which in turn favours the portlandite. The dip at 777 cm 1, 646 cm 1 and 692 cm 1 is due
formation of calcium carboaluminates [54]. The formation of this to quartz from sand. The discussion worthy dips at around 1080
compound can be linked to the exothermic bulge occurring around cm 1, 1000 cm 1 and 420 cm 1 can be linked to Al-O [56], Si-O-
400 °C [55] as shown in the heat flow pattern of Fig. 21. Si/Si-O-Al [57] and Al-O [56] bonds respectively. On addition of
The bands occurring at 1600 cm 1 and 3640 in the FTIR plots in marble all these wavenumbers shift appreciably, indicating change
Fig. 22 can be associated to various water molecules. The charac- in microstructure [57]. Most predominant change occurs around
330 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

180
A0
160 A20
A40
140
A60
120

Heat Flow (mW)


100
80

60
40
20
0
-20

0 200 400 600 800 1000


Fig. 19. Mass loss pattern for the mortar mixes A0, A20, A40 and A60.
Temperature (°C)
the band 1000 cm 1 which is 1010 cm 1 for A0 reduces to 1007 Fig. 21. Heat flow pattern of mortar mixes A0, A20, A40 and A60.
cm 1 for A20 and 996 cm 1 and 995 cm 1 for A40 and A60 respec-
tively. This reduction in wavenumbers is an indication of increased
cross linking of Si-O and Al-O bonds to form C-A-S-H which is also with marble powder incorporation, this shoulder becomes a
characterized by the increase in intensity of DTA plot for A20, A40 prominent peak as seen for A60. This peak can be convincingly
and A60 mix at 400 °C. The second most significant change occurs attributed to Al-O and to the formation of calcium mono-
at 420 cm 1 wavenumber. For mix A0, this is only a shoulder, but carboaluminates [56]. Hence with increased formation of C-S-H,

A0 A20
0.000 0.000

-0.001
-0.002
Derivative Weight (%/°C)

Derivative Weight (%/°C)

-0.002
-0.004

-0.003
-0.006

-0.004
-0.008

-0.005

-0.010
0 100 200 300 400 500 600 0 100 200 300 400 500 600
Temperature (°C) Temperature (°C)

0.000 0.000

-0.002
Derivative Weight (%/°C)

Derivative Weight (%/°C)

-0.005

-0.004

-0.010

-0.006
A40
-0.015 A60
-0.008

-0.010 -0.020

0 100 200 300 400 500 600 0 100 200 300 400 500 600

Temperature (°C) Temperature (°C)

Fig. 20. Thermogravimetric analysis of mortar mixes A0, A20, A40 and A60.
K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332 331

A0 A20

1797

646 1999 2516


1883 535 2523

1643 693
692 2855

1624
2925

Arbitary units
Arbitary units

728

3640 459 3640


528 778
777

877
3434 3436
463 1430

878
1074

1079 1436
1007
1010

1000 2000 3000 4000 1000 2000 3000 4000


-1
Wavenumber (cm )
-1
Wavenumber (cm )

A40 A60

462
535
531

461 796
Arbitary units

Arbitary units

2525
727

1818
727

1088
877 995
3434
877
1084
996
1433
1434

1000 2000 3000 4000 1000 2000 3000 4000


-1 -1
Wavenumber (cm ) Wavenumber (cm )

Fig. 22. FTIR spectra of mortar mixes A0, A20, A40 and A60.

better cross linked C-A-S-H network and the formation of calcium  Due to higher specific surface area of marble powder, drying
carboaluminates has increased the compressive resistance of A20 shrinkage of mixes with 20% marble powder is almost same
mix. However due to increased water content (Fig. 4) has resulted as that of control mortars. This is despite the fact that these
in fall in compressive strength of mortar mixes with substitution mixes have lesser water content than conventional cement sand
greater than 40% as seen from Fig. 10. mortars.
 Water absorption of mortars with 20% marble powder have
4. Conclusions marginal variation from control mortars. Porosity values too
indicate similar variation.
From the above study, the conclusions drawn are as follows:
Hence it can be concluded that at a substitution level
 Due to thixotropic property of marble powder, its’ substitution of 20%, marble powder would enable considerable saving
in place of river sand reduces the water requirement of all mix of water and river sand in construction projects. This will also
proportions at a substitution level of 20%. help the process of marble dimension stone manufacturing to be
 With this reduced water content and marble powder’s capabil- cleaner than before by helping it sort out its waste disposal
ity of accelerating the hydration of C3S and formation of calcium problems.
carboaluminates with C3A have led to the formation of a denser
microstructure. This has considerably improved the mechanical
performance of the mortars. Acknowledgments
 Compressive strength of mixes having 60% marble powder in
place of river sand perform on par with the corresponding con- Authors are grateful to Material Research Centre (MRC), Mala-
trol mortars. Also, enhancement of bond and adhesive strengths viya National Institute of Technology, Jaipur and CDOS, Jaipur for
are very much significant due to the inclusion of marble powder their support in conducting X – ray diffraction, FTIR, TGA/DTA
in lean mortar mixes especially. and SEM and XRF analyses respectively.
332 K.I. Syed Ahmed Kabeer, A.K. Vyas / Construction and Building Materials 165 (2018) 321–332

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