Materials and Structures

Influence of hydrophilic nanoclay addition on microstructure, mechanical and

workability-related properties of cement mortar
--Manuscript Draft--

Manuscript Number: MAAS-D-14-00379
Full Title: Influence of hydrophilic nanoclay addition on microstructure, mechanical and
workability-related properties of cement mortar
Article Type: Original Research
Keywords: Nanoclay; cement mortar; mechanical properties; workability; water absorption;
microstructures
Abstract: This paper investigates the impact of partial substitution of cement particles with
hydrophilic nanoclay platelets on the mechanical properties, workability, consistency,
water absorption and microstructure of cement mortar. Cement mortar mixtures with
various replacement ratios, 0.5%, 1%, and 2% of nanoclay by weight of cement, were
prepared and tested according to the standards. The results show that adding small
quantities of nanoclay could improve the compressive, flexural, and tensile strengths of
cement mortar. The best enhancement occurred in the case of cement mortar
reinforced with 2% of nanoclay. 7%, 5%, and 7% enhancement in compressive
strength, flexural strength, and tensile strength, respectively, were observed after 28-
days curing. It was also noted that adding nanoclay into cement mortar leads to
increase the amount of water needed to reach the normal consistency, elongate its
initial and final setting time, increase its water absorption, but reduce its capillary water
absorption coefficient and significantly lower flowability of the pastes. Scanning
electron microscopy analysis showed that the nanoclay particles jointed with ettringite
needles and calcium hydroxide crystals and closed the voids between them.
Powered by Editorial Manager and ProduXion Manager from Aries Systems Corporation
1
Influence of hydrophilic nanoclay addition on
microstructure, mechanical and workability-
related properties of cement mortar


Mohammad R. Irshidat
1*
and Mohammed H. Al-Saleh
2


1 Department of Civil Engineering, Jordan University of Science and Technology,
Irbid Jordan
2 Department of Chemical Engineering, Jordan University of Science and
Technology, Irbid Jordan


*Corresponding Author:
Phone: 00962-2-7201000 ext. 22126
Fax: 00962-2-7201074
e-mail: mrirshidat@just.edu.jo
Civil Engineering Department
Jordan University of Science and Technology

P.O. Box 3030, Irbid 22110, Jordan







Manuscript
Click here to download Manuscript: Manuscript-Irshidat.docx
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
2


Abstract
This paper investigates the impact of partial substitution of cement particles with hydrophilic
nanoclay platelets on the mechanical properties, workability, consistency, water absorption and
microstructure of cement mortar. Cement mortar mixtures with various replacement ratios, 0.5%,
1%, and 2% of nanoclay by weight of cement, were prepared and tested according to the standards.
The results show that adding small quantities of nanoclay could improve the compressive, flexural,
and tensile strengths of cement mortar. The best enhancement occurred in the case of cement
mortar reinforced with 2% of nanoclay. 7%, 5%, and 7% enhancement in compressive strength,
flexural strength, and tensile strength, respectively, were observed after 28-days curing. It was also
noted that adding nanoclay into cement mortar leads to increase the amount of water needed to
reach the normal consistency, elongate its initial and final setting time, increase its water
absorption, but reduce its capillary water absorption coefficient and significantly lower flowability
of the pastes. Scanning electron microscopy analysis showed that the nanoclay particles jointed
with ettringite needles and calcium hydroxide crystals and closed the voids between them.

Keywords
Nanoclay; cement mortar; mechanical properties; workability; water absorption;
microstructures





1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
3
Introduction
Various material additives such as fly ash, silica fume, and macro and micro
fibers have been traditionally used in cementitious materials for a long period of
time. The use of such additives has become common practice in modern concrete
technology not only for their environmental and economic benefits, but also for
their significantly improvement in the strengths and durability of cement-based
materials [113]. On the other hand, nanomaterials have outstanding mechanical
properties and unique geometrical characteristics entitled them to be promising
substitute to the traditional supplementary cementitious materials to improve the
mechanical properties and then the durability of cement mortar and concrete. The
small size of nanomaterials makes them distributed on a much finer scale than
other materials and filled the nano-sized voids between the ingredients of cement
mortar. Accordingly, micro-cracks are expected to be interrupted much more
quickly during propagation in a nano reinforced cementitious materials which
leads to enhance their mechanical properties and then workability-related
properties such as workability, consistency and water absorption.
A significant number of works dealing with the use of nanomaterials to improve
the behavior of cement based materials have been accomplished. Much of the
work had been with nano-silica [1424] and nano-titanium oxide [18, 25]. There
are a few studies on incorporating nano-iron (nano-Fe
2
O
3
) [17], nano-alumina
(nano-Al
2
O
3
) [26], and nanoclay [1, 3, 2729]. The results of work conducted to
investigate the effect of adding nano silica on the behavior of cementitious
materials revealed that using nano silica leads to improve the workability and
strength of concrete [17, 19, 22], increase the resistance of concrete to water
penetration [15], accelerate the hydration of C3S and an ash-cement mortar [14,
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
4
20], improve the microstructure and promote pozzolanic reactions [16], and
accelerate the hydration of cement [24]. Studies on using other nano materials
with cement based materials showed that nano titanium can improve compressive
and flexural strengths of concrete as well as increase its abrasion resistance [18,
25], nano Fe2O3 can provide concrete with self-sensing capabilities as well as
improve its compressive and flexural strengths [17], and nano Al2O3 can increase
the modulus of elasticity of concrete [26]. The results of research performed to
investigate the effect of adding nanoclay into cementitious materials revealed that
using nanoclay leads to improve the mechanical properties, chloride penetration
resistance, self-compacting and to reduce the permeability of concrete [1, 3, 27
29]. Other studies showed that non-modified nano sized clays can act as
nucleation agents for CSH which leads to modify the structure of CSH [5, 6].
It is widely accepted that the properties of nanocomposites; including nano
cementitious materials; are affected by two major factors: the dispersion of
nanofiller within the matrix and the strength of bond between the matrix and the
nanofiller [30, 31]. Based on the literatures, most of nanomaterials used in this
field are either hydrophobic; needs a surfactant to be well dispersed in water; or
organo-modified materials. The present research is aimed to investigate the
influence of adding hydrophilic; directly dispersed in water; nanoclay named nano
montmorillonite on mechanical properties, workability, consistency, water
absorption and microstructure of cement mortar. The mechanical properties were
characterized by compressive, tensile, and flexural strengths. These strengths were
measured at both 7 and 28 days. The mortar was reinforced with nanoclay at
concentrations of 0%, 0.5%, 1%, and 2% by weight of cement. A scanning
electron microscopy (SEM) imaging and Energy dispersive X-ray (EDX) were
used to analyze the effect of nanoclay addition on the microstructure of the
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
5
cement mortar.
Experimental Details
Materials and mixture proportions
Portland cement, silica sand, tap water, and nanoclay were used to prepare the
cement mortar used in this study. The Portland cement was commercially
available Type II obtained from Alrajihi Cement Company, Jordan conforming to
ASTM C150 standard. The chemical composition and physical properties of the
cement is shown in Table 1. Locally available natural silica sand with physical
properties shown in Table 2 was used. The nanoclay was hydrophilic
Montmorillonite; (Nanocor Inc, USA) and was used as received without any
treatment. Montmorillonites are high purity aluminosilicate minerals sometimes
referred to as phyllosilicates. Montmorillonites have a sheet-type or platey
structure. Although their dimensions in the length and width directions can be
measured in hundreds of nanometers, the minerals thickness is only one
nanometer. As a result individual sheets have aspect ratios (L/w) varying from
200-1000, with a majority of platelets in the 200-400 range after purification. The
theoretical formula for montmorillonite is:
( )

( )

)()

.
The physical properties of nanoclay used are summarized in Table 3. This type of
nanoclay can be dispersed in water with no chemical treatment needed which
makes it easy to use in mortar preparation and then in concrete applications. A
total of four batches of cement mortar were prepared. The first batch was prepared
as control sample of plain cement mortar (water, sand and cement). In the other
three batches, different dose levels (0.5%, 1%, and 2% by weight of cement) of
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
6
nanoclay were selected to partially substitute cement particles. The four batches
were labeled as NC-0.0 for control sample, NC-0.5, NC-1.0, and NC-2.0 for other
samples with 0.5%, 1%, and 2% nanoclay replacement, respectively. All batches
were prepared using a binder-sand ratio of 1:3 and water-binder (w-b) ratio of
0.55.
Nanoclay dispersion and mortar preparation
The nanoclay used in this study was first dispersed within tap water using an
ultrasonic Sonicator. The nanoclay was sonicated for 15 minutes to assure that
good dispersion occurred. The tap water was used to prepare the control sample
whereas the dispersed solution was used to prepare the nanocomposite mortar
according to ASTM C305 standard [32].
Testing procedures
Mechanical Strengths
After mixing, the mortar mix was cast in steel molds; briquette for tensile
strength, 5 cm cubes for compressive strength, and cm prisms for
flexural strength tests. All samples were demolded after 24 h and then cured in
lime saturated water for 7 and 28 days. The compressive strength test was
conducted according to the ASTM C109 standard [33]. ASTM C348 standard [34]
was followed to perform flexural strength test. The tensile strength test was
performed according to ASTM C190 standard. Six specimens of each formulation
at each age were tested and the average values were then obtained.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
7
Standard consistency, setting time, and workability
The required water to binder (w-b) ratio of standard consistency were determined
according to ASTM C187 standard [35] whereas the initial and final setting time
of cement pastes were determined according to ASTM C191 standard [36].
Workability of the pastes was determined using flow table test in conformity with
the procedure described in ASTM C230 standard [37].
Capillary water absorption test
In order to explain the effect of the porous microstructure of nanoclay reinforced
cement mortar on its behavior, capillary water absorption test was performed
according to BS EN 1015-18. The water absorption coefficient due to capillary
action of hardened mortar reinforced with different doses of nanoclay were
measured and compared. Five prismatic (40x40x160 mm) specimens for each
batch were casted then wet cured for 28 days. At the completion of the curing
period, the long faces of the test specimens were coated with paraffin wax. The
test specimens were then dried by keeping them in an oven at 60
o
C up to constant
mass and were then broken into half. The cut surface of the specimens was
submerged in water at a depth of 5-10 mm. The weight change of the specimens
in time was monitored and recorded. Finally, the capillary water absorption
coefficient was calculated.
Water absorption
Water absorption of hardened nanoclay cement mortar was measured in this
study. Six specimens of each batch were casted then wet cured for 28 days. At the
end of curing period, the specimens were dried to constant mass. Each specimen
was then weighed and immediately immersed in water for different period of
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
8
times. On removal from the water, the surface of the specimens was wiped and
weighed again. The water absorption was calculated from the increase in mass as
a percentage of the dry specimens mass.
Scanning electron microscopy (SEM) imaging
An environmental scanning electron microscope (ESEM, Quanta 450 FEG) was
used to characterize the influence of nanoclay addition on the microstructure of
cement mortar.
Results
Mechanical strengths
Experimental results of 7-day and 28-day compressive strength of cement mortars
reinforced with various concentrations of nanoclay are shown in Fig.1 and
tabulated along with the percent of enhacment in Table 4. It is evident that an
enhacment in the compressive strength of cement mortar could be achived by
repalacing small amount of cement particles with nanoclay materials. The
enhancement in compressive strength increases with increasing the nanoclay
replacement level from 0% up to 2% . It is also noticed that the improvement in
compressive strength exhibit almost same trend for both 7 and 28 days. The
improvement in compressive strengths reveals that the nanoclay not only acts as
filler material but also acts as a binder where the nanoclay particles are distributed
around and jointed with the ettringite needles and CH crystals as shown later in
SEM imaging section.
The measured 7-day and 28-day flexural strength of cement mortars reinforced
with various concentrations of nanoclay are depicted in Fig.2. The enhancement
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
9
in flexural strengths are listed in Table 4. It is noted that replacing cement
particles with small amount of nanoclay (0.5% by weight of cement) does not
cause any significant enhancement in flexural strength of the mortar especially
after 7 days. However, incraesing the replacement ratio up to 2% marginally
enhanced the flexural strength after 28 days by almost 5% of the control specimen
strength. This enhancement is less than the enhancement in compressive strength
for the same replacement level at the same age.
Fig.3 shows the 7-day and 28-day tensile strength of cement mortars with and
without nanoclay repalcement and Table 4 summaries the enhancement in tensile
strength due to the addition of nanoclay. The results show that the tensile strength
of cement mortar can be enhanced by replacing cement particles with small
amount of nanoclay. The enhancement follows same trend for both 7 and 28-day
strengths. It can be also noted that the tensile strength of cement mortar reinforced
with nanoclay increases as the percentage replacement of cement with nanoclay
increases.The enhancements in tensile strength were probably because of good
bonding between the nanoclay platelets and the cement matrix. The SEM imaging
(discussed next) show that the platelets of nanoclay act as a fiber between
hydration products which leads to resist crack propagation at micro scale and
delay the failure. The improvement in tensile and flexural strengths for cement
mortar when added nanoclay is crucial for structural applications in which higher
strength in needed.
Standard consistency, setting time, and workability
The required w-b ratio of standard consistency is represented in Fig.4. It is clear
that the water demand increases with increasing nanoclay replacement level.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
10
Cement pastes containing nanoclay need higher amount of water to form hydrated
products due to the high fineness and surface area of nanoclay particles.
The influence of nanoclay addition on the initial and final setting time is shown in
Fig.5. It is clear that the initial setting time was clearly elongated were as the final
setting time was slightly elongated due to nanoclay addition. This behavior may
be attributed to the excess amount of water needed for mixing process in case of
nanoclay presence. It was also noted that the difference between the initial and the
final setting time decreased with increasing the nanoclay content.
The effect of nanoclay with different replacement levels on the flow of fresh
cement pastes at a w-b ratio of 0.55 was measured. The results are plotted in
Fig.6. The results show that increasing the replacement level of nanoclay led to
significantly lower flowability of the pastes. Considerable quantity of mixed water
absorbed by nanoclay particles apparently results in decrease in flowability. It
seems that less workability of the pastes containing higher nanoclay quantity is
probably responsible about some of the enhancement in mechanical strength of
the mortars.
Capillary water absorption
The capillary water absorption test results are shown in Fig.7. The results show
that adding 0.5% of nanoclay did not affect the capillarity of the mortar whereas
adding 1% and 2% of nanoclay decrease the coefficient of water absorption
coefficient by 12.5%. It is interesting to compare the results with the mechanical
strengths of the mortar. Among all the mixtures containing nanoclay, the highest
increase in compressive, tensile and flexural strengths (7%, 7%, and 5%;
respectively) was observed at the dose of 2%; where the largest reduction in the
coefficient of capillary water absorption was achieved.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
11
Water absorption
The water absorption of nanoclay cement mortar is plotted in Fig.8. The results
show that adding 0.5% of nanoclay caused a reduction in the water absorption of
the mortar whereas adding 1% and 2% of nanoclay unexpectedly caused an
increase in the water absorption. Comparing the results with capillary water
absorption coefficients, it can be noticed that the increase in water absorption of
the mortar when 1% and 2% of nanoclay were added was associated with the
reduction in capillary water absorption coefficient when same amount of nanoclay
was used. The variations of water absorption with age showed that the water
absorption for all mixtures increases with increasing ages of curing.
Scanning electron microscopy (SEM) imaging
The influence of adding nanoclay on the microstructure of cement mortar was
investigated using SEM images and EDX analyses. The microstructure tests were
performed on the control and 2% nanoclay substituted cement mortar samples that
yielded the highest compressive, flexural, and tensile strengths in the mechanical
tests. Fig. 9 shows the SEM micrographs of cement mortars reinforced with 0%
and 2% of nanoclay particles, respectively, at magnification factor of 10000. The
SEM micrograph of plain cement mortar at 10000x magnification factor (Fig. 9a)
shows hydrated products like calcium silicate hydrate (CSH) gel, calcium
hydroxide (CH) crystals, and ettringite needles. With 2% of nanoclay addition
into the mortar, more amorphous C-S-H gel is observed as shown in Fig.9b. By
comparing the microstructure of plain cement mortar to the microstructure of 2%
nanoclay reinforced cement mortar at higher magnification factor (20000x) as
shown in Fig.10, the most distinguishing feature between them is the presence of
plate-like component which probably belong to the nanoclay platelets in the latter.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
12
According to EDX analysis, the composition in the areas where the plates were
fully developed is shown in Fig.11b. These results indicate that such plates could
be nanoclay platelets. The EDX analysis in Fig11 shows that the Ca and Si ratios
appear as 16% and 8% for control mortar, and 13% and 10% for 2% nanoclay
reinforced cement mortar, respectively. The increase in the ratio of Si indicates
that more amorphous C-S-H gel was formulated. It is clear that the nanoclay
platelets are distributed around and jointed with the ettringite needles and CH
crystals. The previous situation could be the reason beyond the improvement in
mechanical strengths of cement mortar. The good dispersion of the nanoclay plays
a major role on better distribution of the particles within the paste and then more
enhancements on the properties. On the other hand, when nanoclay particles are
dispersed in the cement mortar, the products of the hydration process will cluster
around the nano particles and grow to form uniformly distributed conglomeration.
Conclusion
This study investigates the effect of cement particles partially substituted with
hydrophilic nanoclay on mechanical properties, workability, consistency, water
absorption and microstructure of cement mortar. The following conclusions can
be drawn:
1. Adding small amount of nanoclay to the cement mortar could improve its
compressive, tensile and flexural strengths. For cement mortar reinforced
with 2% of nanoclay after 28 days, enhancements up to 7%, 5%, and 7%
in compressive strength, flexural strength, and tensile strength,
respectively, were obtained. It was also noticed that the enhancement in
mortar strengths increases with increasing the substitution percentage from
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
13
0.5% to 2% by weight of cement. The enhancement was also followed
same trend but at different scale for both 7-days and 28-days strengths.
2. Increasing the replacement level of nanoclay led to increase the amount of
water needed to reach the standard consistency of cement mortar but
significantly lower flowability of the pastes.
3. Adding nanoclay into cement mortar leads to clear elongation in its initial
setting time whereas the final setting time was slightly elongated.
4. The increase in water absorption of cement mortar when 1% and 2% of
nanoclay were added was associated with the reduction in capillary water
absorption coefficient when same amount of nanoclay was used. The
variations of water absorption with age showed that the water absorption
for all mixtures increases with increasing ages of curing.
5. Partial replacement of cement by nanoclay has led to the modification of
the microstructure of the mortars to some extent. The SEM images show
the clustering of nanoclay particles around the ettringite needles and CH
crystals which fill the voids between them. The results reflect the
importance of the dispersion of the nanoclay particles in cement mortar
components. Good dispersion means that the particles can reach and fill
the small voids and make the mortar denser and stronger.
Acknowledgment
The work presented in this article was funded by the Deanship of Research at Jordan University of
Science and Technology, Jordan. The authors would also like to thank the Nanotechnology Center
at Jordan University of Science and Technology where the SEM imaging was conducted.

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
14
References
1. Antoni M, Rossen J, Martirena F, Scrivener K (2012) Cement substitution by a combination of
metakaolin and limestone. Cem Concr Res 42:15791589.
2. Fischer G, Li VC (2007) Effect of fiber reinforcement on the response of structural members.
Eng Fract Mech 74:258272.
3. Kuo W-Y, Huang J-S, Lin C-H (2006) Effects of organo-modified montmorillonite on strengths
and permeability of cement mortars. Cem Concr Res 36:886895.
4. Li VC, Maalej M (1996) Toughening in cement based composites. Part II: Fiber reinforced
cementitious composites. Cem Concr Compos 18:239249.
5. Lindgreen H, Skibsted J, Kryer H, Jakobsen HJ (2003) Hydration of Portland cement in the
presence of clay minerals studied by 29Si and 27Al MAS NMR spectroscopy. Adv Cem Res
15:103112. doi: 10.1680/adcr.2003.15.3.103
6. Lindgreen H, Geiker MR, Kryer H, et al. (2008) Microstructure engineering of Portland
cement pastes and mortars through addition of ultrafine layer silicates. Cem Concr Compos
30:686699. doi: 10.1016/j.cemconcomp.2008.05.003
7. Ostertag CP, Yi CK, Vondran G (2001) Tensile strength enhancement in interground fiber
cement composites. Cem Concr Compos 23:419425.
8. Richardson IG (1999) The nature of CSH in hardened cements. Cem Concr Res 29:11311147.
9. Richardson IG (2004) Tobermorite/jennite- and tobermorite/calcium hydroxide-based models
for the structure of C-S-H: applicability to hardened pastes of tricalcium silicate, -dicalcium
silicate, Portland cement, and blends of Portland cement with blast-furnace slag, metakaolin, or
silica fume. Cem Concr Res 34:17331777. doi: 10.1016/j.cemconres.2004.05.034
10. Savastano Jr H, Warden PG, Coutts RSP (2005) Microstructure and mechanical properties of
waste fibrecement composites. Cem Concr Compos 27:583592.
11. Scrivener KL, Kirkpatrick RJ (2008) Innovation in use and research on cementitious material.
Cem Concr Res 38:128136. doi: 10.1016/j.cemconres.2007.09.025
12. Scrivener KL, Fllmann T, Gallucci E, et al. (2004) Quantitative study of Portland cement
hydration by X-ray diffraction/Rietveld analysis and independent methods. Cem Concr Res
34:15411547.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
15
13. Wang C, Li K-Z, Li H-J, et al. (2008) Effect of carbon fiber dispersion on the mechanical
properties of carbon fiber-reinforced cement-based composites. Mater Sci Eng A 487:5257. doi:
10.1016/j.msea.2007.09.073
14. Bjrnstrm J, Martinelli A, Matic A, et al. (2004) Accelerating effects of colloidal nano-silica
for beneficial calciumsilicatehydrate formation in cement. Chem Phys Lett 392:242248.
15. Ji T (2005) Preliminary study on the water permeability and microstructure of concrete
incorporating nano-SiO< sub> 2</sub>. Cem Concr Res 35:19431947.
16. Jo B-W, Kim C-H, Tae G, Park J-B (2007) Characteristics of cement mortar with nano-SiO<
sub> 2</sub> particles. Constr Build Mater 21:13511355.
17. Li H, Xiao H, Ou J (2004) A study on mechanical and pressure-sensitive properties of cement
mortar with nanophase materials. Cem Concr Res 34:435438.
18. Li H, Zhang M, Ou J (2006) Abrasion resistance of concrete containing nano-particles for
pavement. Wear 260:12621266. doi: 10.1016/j.wear.2005.08.006
19. Qing Y, Zenan Z, Deyu K, Rongshen C (2007) Influence of nano-SiO< sub> 2</sub> addition
on properties of hardened cement paste as compared with silica fume. Constr Build Mater 21:539
545.
20. Lin KL, Chang WC, Lin DF, et al. (2008) Effects of nano-SiO< sub> 2</sub> and different
ash particle sizes on sludge ashcement mortar. J Environ Manage 88:708714.
21. Lin DF, Lin KL, Chang WC, et al. (2008) Improvements of nano-SiO< sub> 2</sub> on
sludge/fly ash mortar. Waste Manag 28:10811087.
22. Sobolev K, Flores I, Torres-Martinez LM, et al. (2009) Engineering of SiO2 nanoparticles for
optimal performance in nano cement-based materials. Nanotechnol. Constr. 3. Springer, pp 139
148
23. Qing YE, Zenan Z, Li S, Rongshen C (2006) A comparative study on the pozzolanic activity
between nano-SiO2 and silica fume. J Wuhan Univ Technol-Mater Sci Ed 21:153157.
24. Madani H, Bagheri A, Parhizkar T (2012) The pozzolanic reactivity of monodispersed
nanosilica hydrosols and their influence on the hydration characteristics of Portland cement. Cem
Concr Res 42:15631570.
25. Li H, Zhang M, Ou J (2007) Flexural fatigue performance of concrete containing nano-
particles for pavement. Int J Fatigue 29:12921301.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
16
26. Li Z, Wang H, He S, et al. (2006) Investigations on the preparation and mechanical properties
of the nano-alumina reinforced cement composite. Mater Lett 60:356359. doi:
10.1016/j.matlet.2005.08.061
27. Chang T-P, Shih J-Y, Yang K-M, Hsiao T-C (2007) Material properties of Portland cement
paste with nano-montmorillonite. J Mater Sci 42:74787487.
28. Morsy MS, Aglan HA, Abd El Razek MM (2009) Nanostructured zonolitecementitious
surface compounds for thermal insulation. Constr Build Mater 23:515521.
29. He X, Shi X (2008) Chloride permeability and microstructure of Portland cement mortars
incorporating nanomaterials. Transp Res Rec J Transp Res Board 2070:1321.
30. Al-Saleh MH, Sundararaj U (2011) Review of the mechanical properties of carbon
nanofiber/polymer composites. Compos Part Appl Sci Manuf 42:21262142. doi:
10.1016/j.compositesa.2011.08.005
31. Tyson B, Abu Al-Rub R, Yazdanbakhsh A, Grasley Z (2011) Carbon Nanotubes and Carbon
Nanofibers for Enhancing the Mechanical Properties of Nanocomposite Cementitious Materials. J
Mater Civ Eng 23:10281035. doi: 10.1061/(ASCE)MT.1943-5533.0000266
32. C01 Committee (2013) Practice for Mechanical Mixing of Hydraulic Cement Pastes and
Mortars of Plastic Consistency. ASTM International
33. C01 Committee (2013) Test Method for Compressive Strength of Hydraulic Cement Mortars
(Using 2-in. or [50-mm] Cube Specimens). ASTM International
34. C01 Committee (2008) Test Method for Flexural Strength of Hydraulic-Cement Mortars.
ASTM International
35. C01 Committee (2011) Test Method for Amount of Water Required for Normal Consistency
of Hydraulic Cement Paste. ASTM International
36. C01 Committee (2013) Test Methods for Time of Setting of Hydraulic Cement by Vicat
Needle. ASTM International
37. C01 Committee (2013) Specification for Flow Table for Use in Tests of Hydraulic Cement.
ASTM International



1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
17
Figures caption list:
Fig1 Compressive strength of cement mortar
Fig2 Flexural strength of cement mortar
Fig3 Tensile strength of cement mortar
Fig4 Required w-b ratio for standard consistency
Fig5 Initial and final setting time of cement mortar
Fig6 Flowability of the pastes with different nanoclay replacement levels
Fig7 Capillary water absorption coefficient of cement mortar with different
nanoclay replacement levels
Fig8 Water absorption of cement mortar with different nanoclay replacement
levels
Fig9 SEM micrographs of cement mortar at 10000 magnification factor (a)
control specimen (b) 2% nanoclay replacement
Fig10 SEM micrographs of cement mortar at 20000 magnification factor (a)
control specimen (b) 2% nanoclay replacement
Fig11 EDX results for control and2% nanoclay reinforced mortar













1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
18
Table 1: Chemical compositions and physical properties of cement
Compound %
CaO 56.02
SiO
2
24.59
Al
2
O
3
5.87
Fe
2
O
3
4.67
MgO 2.87
SO
3
2.49
Na
2
O 0.55
K
2
O 0.58
Loss on ignition 0.8
Property Value
Specific gravity 3.15
Blaine fineness (m
2
/kg) 400
Color Gray














1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
19


Table 2: Physical properties of silica sand
Property Value
Maximum particle size 1.18 mm
Absorption 1.5 %
Fineness modulus 1.72
Specific gravity 2.6



Table 3: Physical Properties of Nanoclay used in the study
Property
Color Off white
CEC (meq/100g) 10% 120
Aspect Ratio 300-500
Specific Gravity 2.6
Maximum Moisture (%) 12
pH (5% dispersion) 9-10










1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
20
Table 4: Enhancement in compressive, flexural, and tensile strengths of cement
mortar
Enhancement in compressive strength
Mi
x
No.
7-day 28-day

Compressiv
e strength
(MPa)
Enhancemen
t (%)
Standard
deviatio
n
Compressiv
e strength
(MPa)
Enhancemen
t (%)
Standard
deviatio
n
C-
0.0
26.40 1.15 37.58 0.37
C-
0.5
27.30 3 0.14 38.36 2 3.11
C-
1.0
NA NA NA 38.54 3 1.3
C-
2.0
28.70

9 1.32 40.35 7 0.68
Enhancement in flexural strength
Mi
x
No.
7-day 28-day
C-
0.0
6.34
0.36
7.42
0.24
C-
0.5
6.36
0.2 0.22
7.60
2 0.31
C-
1.0
NA
NA NA
7.64
3 0.15
C-
2.0
6.59

4 0.02
7.80
5 0.17
Enhancement in tensile strength
Mi
x
No.
7-day 28-day
C-
0.0
2.87
0.34
3.22
0.09
C-
0.5
2.93
2 0.25
3.33
3 0.2
C-
1.0
NA
NA NA
3.37
5 0.11
C-
2.0
3.08

7 0.17
3.46
7 0.17

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65

Fig1 Compressive strength of cement mortar


Fig2 Flexural strength of cement mortar

20
25
30
35
40
45
0 0.5 1 1.5 2 2.5
C
o
m
p
r
e
s
s
i
v
e

s
t
r
e
n
g
t
h

(
M
P
a
)

Nanoclay replacement (%)
7-day
28-day
5
5.5
6
6.5
7
7.5
8
8.5
0 0.5 1 1.5 2 2.5
F
l
e
x
u
r
a
l

s
t
r
e
n
g
t
h

(
M
P
a
)

Nanoclay replacement (%)
7-day
28-day
Figs.1-8
Click here to download attachment to manuscript: Figs. 1-8.docx
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65



Fig3 Tensile strength of cement mortar







2
2.2
2.4
2.6
2.8
3
3.2
3.4
3.6
3.8
0 0.5 1 1.5 2 2.5
T
e
n
s
i
l
e

s
t
r
e
n
g
t
h

(
M
P
a
)

Nanoclay replacement (%)
7-day
28-day
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65

Fig4 Required w-b ratio for standard consistency



Fig5 Initial and final setting time of cement mortar

0
0.1
0.2
0.3
0.4
0 0.5 1 2
w
/
b

r
a
t
i
o

Nanoclay content (%)
0
50
100
150
200
250
300
0 0.5 1 1.5 2 2.5
S
e
t
t
i
n
g

t
i
m
e

(
m
i
n
)

Nanoclay contents %
Initial set. time
Final set. Time
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65

Fig6 Flowability of the pastes with different nanoclay replacement levels



Fig7 Capillary water absorption coefficient of cement mortar with different nanoclay
replacement levels


0
20
40
60
80
100
0 0.5 1 2
S
p
r
e
a
d

(
m
m
)

Nanoclay content (%)
0
0.01
0.02
0.03
0.04
0.05
0 0.5 1 2
C
a
p
i
l
l
r
y

a
b
s
o
r
p
t
i
o
n

c
o
e
f
f
i
c
i
e
n
t

(
k
g
/
m
2
.
m
i
n
0
.
5
)

Nanoclay content (%)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65

Fig8 Water absorption of cement mortar with different nanoclay replacement levels

8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
0 10 20 30 40 50 60 70
W
a
t
e
r

a
b
s
o
r
p
t
i
o
n

%

Age (days)
0%
0.50%
1%
2%
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
Fig.9a
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
Fig.9b
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
Fig.10a
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
Fig.10b
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
Fig.11a
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
Fig.11b
Click here to download high resolution image
Click here to view linked References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49