Construction and Building Materials 112 (2016) 276–283

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Construction and Building Materials

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

Enhanced physical, mechanical and microstructural properties of

lightweight vermiculite cement composites modified with nano
metakaolin
H. Shoukry a,⇑, M.F. Kotkata b, S.A. Abo-EL-Enein c, M.S. Morsy a, S.S. Shebl a
a
Housing & Building National Research Center, HBRC, Cairo, Egypt
b
Semiconductors Technology Lab, Faculty of Science, Ain Shams University, Cairo 11566, Egypt
c
Chemistry Department, Faculty of Science, Ain Shams University, Cairo, Egypt

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Lightweight cement composite with

unique physical and mechanical
properties is proposed.

Effect of nano metakaolin on physical,
mechanical and microstructural
properties has been studied.

Nano metakaolin has enhanced the
compressive and flexural strengths by
about 57 and 59%, respectively.

Considerable improvement in the
microstructure has been achieved.

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

Article history: This article presents a study on the influence of nano metakaolin (NMK) on physical, mechanical and
Received 11 January 2016 microstructural properties of high volume vermiculite blended white Portland cement (WPC). WPC
Received in revised form 16 February 2016 was replaced with 70 vol% expanded vermiculite (EVM), NMK were incorporated at a rate of 2, 4, 6, 8
Accepted 26 February 2016
and 10% as partial replacement by weight of EVM. The density, thermal conductivity, compressive
Available online 2 March 2016
strength, flexural strength, and capillary water absorption of the blended mixes were determined in
accordance with ASTM standards at 28 days of curing. Differential scanning calorimeter (DSC) was used
Keywords:
to study the phase transitions. The microstructure characteristics of the hardened samples were investi-
Cement replacement
Nano metakaolin
gated by scanning electron microscope (SEM). The experimental results revealed a significant enhance-
Vermiculite ment in both compressive and flexural strength, enhancements of about 57 and 59%, respectively were
Compressive strength obtained at 10% NMK replacement. The capillary water absorption generally decreases with increasing
Flexural strength replacements of EVM by NMK. A considerable decrease of about 74% was observed at 10% NMK. No sig-
Capillary water absorption nificant effect of the NMK content on density and thermal conductivity. NMK led to noticeable improve-
Microstructure ment in the microstructure characteristics of the hardened blends.
Ó 2016 Elsevier Ltd. All rights reserved.

⇑ Corresponding author.
E-mail address: hamadashoukry@yahoo.com (H. Shoukry).

http://dx.doi.org/10.1016/j.conbuildmat.2016.02.209
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283
1. Introduction
Lightweight aggregates are those minerals, natural rock mate-
rials, products, and by-products of manufacturing processes used
as bulk fillers in lightweight structural cement and concrete, con-
crete masonry units, precast concrete structural products, road-
surfacing materials, plaster aggregates, and insulating fill. Other
uses include Architectural wall covers, suspended ceilings, light-
weight structural fill, soil conditioners, and other agricultural
uses [1]. The lightweight aggregates can be classified into organic
and inorganic cellular materials. Examples of organic cellular
materials are expanded polystyrene foam (EPS), extruded poly-
styrene foam (XPS) and polyurethane foam. The inorganic cellular
materials are produced from natural and artificial sources such as
expanded perlite, expanded clay, vermiculite, ceramic micro-
sphere, glass hollow sphere, etc. [2], These materials are charac-
terized by high porosity and contain a high volume of voids so
their densities and thermal conductivities are very low [3]. While
lightweight cement pastes and mortars present superior proper-
ties such as, thermal insulation [4–6], fire/high temperature resis-
tance and so protection [7], sound insulation [8,9], they are
brittle, suffer from cracks and low tensile strength, and exhibit
low tensile strains prior to failure [10]. Incorporation of perlite
and vermiculite (VM) as fillers into mortar decreases mechanical
properties of mortar, due to lack of cohesion. Also, perlite and
vermiculite are responsible for voids and high capillarity, water
demand and shrinkage [11]. Combined effect of silica fume (SF)
and expanded vermiculite on properties of lightweight mortars
at ambient and elevated temperatures has been investigated; SF
enhanced the mechanical properties of mortar incorporating high
volume VM furthermore, increased durability against elevated
temperature has been achieved [12]. Recently, due to their
unique physical and chemical characteristics, nano materials
(NMs) have been strongly used for improving the properties of
plain cement, however; studies about the influence of NMs on
the properties of cement incorporating high volume replacements
are limited. Previous studies indicated that, incorporating 2 mass,
% nano silica (NS) into high volume fly ash-blended cement con-
taining 68 mass, % FA has increased the strength at 28 days by
about 56% [13]. The replacement of White Portland Cement
(WPC) by 2 mass, % nano clay in 30% WPC and 70% perlite
blended mix has improved the indirect tensile strength of the
hardened pastes by 25% compared to the cement without nano
clay at 28 days of hydration [14]. Nano metakaolin (NMK) was
found to be very effective for compensating the loss in flexural
strength of WPC incorporating 70% expanded perlite [3]. The
focus of this study will be on the effect of NMK on physical,
mechanical and microstructural properties of high volume vermi-
culite blended WPC, replacing 70% of cement. The motivations for
choosing the vermiculite can be summarized as follows: Vermi-
culite is a naturally occurring hydrous phyllosilicate (sheet sili-
cates) mineral. When heated to elevated temperatures up to
600–1000 °C, it expands as much as 8–20 times with respect to
their original size providing Accordion-like shape granules [15].
Particles of expanded vermiculite are viewed as thin plates sepa-
rated by air gaps, i.e. highly porous, lightweight, and have quite
low densities and thermal conductivities. Considering the
expanded vermiculites high porosities and low densities, they
are adequate as lightweight aggregates for developing light-
weight cement-based materials with improved thermal resis-
tance for energy efficient building envelopes [12,16]. There are
many studies on lightweight aggregates such as pumice, perlite,
expanded clay, expanded polystyrene and their usages in light-
weight composites. However, studies about the use of EVM are
limited.
277
2. Experimental procedure
2.1. Materials
The materials used in this study were white Portland cement (WPC) (type I),
nano kaolin clay (NK) and vermiculite. Nano kaolin was supplied by Middle East
Mining Investments Company (MEMCO), Egypt; the vermiculite was supplied by
the Egyptian company for manufacturing perlite & vermiculite (E.C.P.V).
Nano Metakaolin (NMK) was obtained by thermal activation (calcination) of NK
at 750 °C for 2 h. Calcination was conducted in alumina crucible with Length:
100 mm; Width: 40 mm and Height: 18 mm. Expanded vermiculite (EVM) was
obtained by heating raw vermiculite rapidly in a muffle furnace at 600 °C for 3 min.
The oxide compositions of WPC, NMK and EVM were determined by X-ray flu-
orescence (XRF) as shown in Table 1. The mineralogical analyses of NMK and EVM
were performed by X-ray diffractometer and given in Fig. 1. The scanning electron
microscope (SEM) was used to investigate the micro morphologies of NMK and
EVM and introduced in Fig. 2. The physical properties of EVM are summarized in
Table 2.
NMK has plate like structure and characterized by large length to thickness
aspect ratio; it is especially favourable in matrix reinforcement, and the platelet
thickness is only 1–20 nm, although its dimensions in length and width can be mea-
sured in hundreds of nanometers, with a majority of platelets in 200–500 nm range
after purification.
The EVM looks like flakes, the flakes have separated from each other, providing
highly porous exfoliated structure as a result of flash heating (shock thermal treat-
ment). The rapid heating of raw VM resulted in the transformation of the interlayer
water into steam, the pressure of the steam forces the silicate layers to separate
forming packets, which are several orders thicker than the fundamental layers so
that the particles exhibit ‘‘accordion” type morphology.
2.2. Samples preparation
Table 3 illustrates the mix design of the high volume vermiculite blended
cement composites modified with NMK particles. WPC was partially replaced with
70 vol% EVM. EVM was then substituted by various amounts of NMK at a rate of 0, 2,
4, 6, 8 and 10 mass, %. The dry WPC and EVM were mixed at a speed of 50 rpm using
an electric mixer for 2 min to obtain a homogenous mix. The NMK particles were
first dispersed in the mixing water (without surfactant) using high intensity ultra-
sonic bath (frequency: 20 kHz) for 15 min to assure a good dispersion and to avoid
agglomeration then, added to make the freshly blended cement mortars.
The blended cement mortars were prepared using the water of standard consis-
tency in order to maintain a constant degree of workability between different sam-
ples. Three groups of samples were cast for testing as shown in Fig. 3, the first group
was cast as cubes 5  5  5 cm3 for density, capillary water absorption and com-
pressive strength tests, the second group was cast as prisms 4  4  16 cm3 for flex-
ural strength test and the third group was disks (5 cm Dia. & 2 cm height) for
thermal conductivity test. The fresh mortars were kept in moulds for 24 h, and then
de-moulded and allowed to cure under water for 27 d.
2.3. Testing
2.3.1. Compressive strength
This test was performed using control compression machine (DARTEC) accord-
ing to ASTM C 109 with a constant loading rate of 0.75 kN/s. Every result of the
compressive strength was reported as the average value of measurements carried
out on 5 test cubes.
2.3.2. Flexural strength
The flexural strength test was performed on 4  4  16 cm3 prisms using 600
KN machine (DARTEC) in accordance with ASTM C348-08. Three samples per batch
were tested, and the average strength was reported.
2.3.3. Capillary water absorption
In this test the specimens were dried in an oven drier at about 60 ± 5 °C until
constant mass was obtained. The sides of the specimen were coated with paraffin
to achieve unidirectional flow. The specimens were exposed to water on one face
by placing it on slightly raised seat (about 5 mm) on a pan filled with water. The
water on the pan was maintained about 5 mm above the base of the specimen dur-
ing the test. The weight of the specimen was measured at regular 30 min interval up
to 2.5 h to get the little absorption variation of water. The capillary absorption coef-
p
ficient (k) was calculated by using the formula: k = W/ (A. t) where, W = amount of
water absorbed, A = cross sectional area contact with water and t = time [17].
2.3.4. Bulk density
The average bulk density of three cubic samples with dimensions of 5 cm was
determined in oven-dry condition according to ASTM 6426-82.
278 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283

Table 1
Chemical compositions of starting raw materials (mass, %).

Oxide, % SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2O K2O TiO2 L.O.I.
WPC 20.92 3.69 0.19 68.32 0.57 2.67 0.12 0.02 – 3.5
NMK 54.24 31.99 0.18 0.32 0.03 0.039 0.14 0.04 – 13
EVM 40.34 16.88 10.9 3.59 15.39 – 0.13 2.3 1.36 9.1

400 300
P

K + I+ Q
NMK EVM
350
250
300
K: kaolinite 200 P: phlogopite
250 I: illite P H: hydrobiotite

Intensity
K+Q
Intensity

Q: quartz V: vermiculite
200 150 Q
H
K

150
100 V
H Q
100 V P
H
50
50

0 0
5 10 15 20 25 30 35 40 45 50 5 10 15 20 25 30 35 40 45 50
2θ (degree) 2θ (degree)

Fig. 1. X-ray diffraction patterns of NMK and EVM.

Fig. 2. SEM micrographs of (a) NMK and (b) EVM.

Table 2 Surface
Physical properties of EVM granules.

Color Golden-yellow
Shape Accordion-like granule
Specific Gravity 0.58
Grain Size 0–4 mm
Specific surface area 4.5 m2/g
Specific Heat 950–1050 J/kg k
Thermal Conductivity At (24 °C) 0.06–0.065 W/m K

Table 3
Mix design of the developed composites (mass expressed per 1 m3).

Mix code NMK, % Constituents (kg)

WPC EVM NMK Water
M0 0 650 274 0 353 Fig. 3. Photo of the prepared test samples as per ASTM standards.
M1 2 650 268.52 5.48 355
M2 4 650 263.04 10.96 358
M3 6 650 257.56 16.44 359 2.3.5. Thermal conductivity
M4 8 650 252.08 21.92 362 The thermal conductivity test was performed by using guarded heat flow meter
M5 10 650 246.60 27.4 365 apparatus (FOX-50) in accordance with ASTM C 518. Since moisture content affects
the thermal conductivity, all the specimens were tested in an oven-dry condition.
 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283 279

2.3.6. Differential scanning calaorimetry (DSC) 1.3

The phase composition/decomposition analysis was studied by using (schi- Flexural Strength
madzu DSC-50) thermal analyzer. Inert atmosphere with N2 flow of 30 mL/min, Poly. (Flexural Strength)
heating rate of 10 °C/min, analysis range of 30–600 °C. 1.2

Flexural strength (MPa)

2.3.7. Scanning electron microscopy (SEM) 1.1
R² = 0.9911
The analytical scanning electron microscope, (JSM 6360) equipped with EDAX
unit for phase analysis was used to investigate the microstructure characteristics.
Freshly fractured samples were used for SEM examination. 1

3. Results and discussion 0.9

3.1. Compressive strength 0.8

Fig. 4 shows the variations in the compressive strength of WPC

0.7
incorporating 70% EVM and modified by different NMK ratios at 0 2 4 6 8 10
28 days of curing. As it is clear, NMK enhanced the compressive NMK, Wt%
strength; the highest strength was obtained for the mortars with
the highest NMK ratio. A significant enhancement of about 57% Fig. 5. Variations of flexural strength as a function of NMK content at 28 days of
curing.
was obtained at 10% NMK. The role of NMK in enhancing the com-
pressive strength can be summarized as following: Due to its high
amorphous silica content, NMK participates in the pozzolanic reac-
tion, i.e. reacts with free lime Ca(OH)2 liberated during the hydra-
tion of cement to produce additional calcium silicate hydrate
(CSH), which is essentially responsible for strength in cement-
based materials (this is confirmed by DSC technique as shown in
Fig. 7). Due to its ultrafine size, NMK particles fill the voids among
cement grains and reduce the capillary pores of the internal matrix,
i.e. leads to improve the microstructure of the hardened cement
(this is confirmed by SEM) [18,19]. Generally, the strength of hard-
ened cement samples with high volume replacements is lower
than conventional plain cement without replacements; however,
replacing the EVM with 10 wt% NMK in 30% WPC and 70% EVM
blended mix is found to be very helpful in compensating the loss
in compressive strength that has been produced due to the porous
and soft structure of EVM aggregates. The compressive strength of
the system incorporating 10% NMK at 28 days of hydration is
Fig. 6. Variations of capillary water absorption as a function of NMK content at
16.56 MPa; this is a significant value that might satisfy prescribed 28 days of curing.
mechanical requirements for indoor and outdoor plastering appli-
cations [21].
Temperature (°C)
0
3.2. Flexural strength 30 80 130 180 230 280 330 380 430 480 530 580

M0 M5
Fig. 5 shows the variations in the flexural strength of the devel- -20

oped mortars as a function of NMK % at 28 days of curing. Under

flexural tension, the test samples showed a similar trend to their -40
Heat Flow (μV)

behaviours under compression stress. Flexural strength increases

with the increase of the NMK content and the enhancement ratio -60 CH

M0 : 99.90 j/g

-80 M5 : 66.44 j/g

18
Compressive Strength
Poly. (Compressive Strength)
17
-100
M0 : 101.61j/g
Compressive strength (MPa)

CSH
Endo

16 M5 : 146.53 j/g

-120
15
Fig. 7. DSC thermograms of the 10% NMK-modified mix (M5) as compared with the
14 R² = 0.9853
control mix (M0).

13

12 reached 59% at 10% NMK. Basically, the NMK enhances the flexural
strength by two mechanisms. The first mechanism is the physical
11
filling of the NMK platelets, which act as fibers between hydration
10 products causing 2-dimensional reinforcement, leading to bridging
0 2 4 6 8 10
the microcracks in the matrix, providing tightly bonding and resis-
NMK, Wt%
tance to crack propagation and crack opening [20]. The second
Fig. 4. Variations of compressive strength as a function of NMK content at 28 days mechanism is the pozzolanic effect. As mentioned above, the reac-
of curing. tion of amorphous aluminosilicates (Al2O3.2SiO2) in NMK with the
280 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283
Ca(OH)2 liberated from cement hydration result in creating supple-
mentary C–S–H to form dense and compact hardened cement
paste. The flexural strength of the system incorporating 10% NMK
at 28 days of hydration is 1.25 MPa, which is higher than the stan-
dard minimum value of 0.8 MPa [21].
3.3. Capillary water absorption (Sorptivity)
The effect of NMK on capillary water absorption of the exam-
ined mortars as a function of NMK % is shown in Fig. 6. As seen,
the water absorption coefficient decreases with increasing the
amount of NMK content. The highest value of sorptivity was
obtained for the control mix (without NMK), while the lowest
value is obtained for the mix modified with 10% NMK, a decrease
of about 74 was observed. The significant reduction in sorptivity
is attributed to the increase of the solid volume and the
microstructure improvement. NMK fill the voids between cement
grains and in the interface between EVM aggregate and cement
paste; this resulted in a compact structure leading to the reduction
of water mobility inside the hardened cement paste skeleton. In
addition, the pozzolanic reaction with free calcium hydroxide
(CH) resulted in the creation of more CSH, which fill the internal
capillary pores and make the structure more uniform and dense
as will be seen from SEM micrographs. Densification of cement
matrix results in the immobilization of water inside the bulk paste
[22]. The durability of cement and concrete structures is closely
related to the water absorption so the reduction of water absorp-
tion will extend the lifetime of cement based products and hence
durability [23].
3.4. Bulk density and thermal conductivity
The variations of bulk density and thermal conductivity of the
prepared mortars as a function of NMK content is presented in
the Table 4. As expected, since EVM has a lower density and ther-
mal conductivity than natural sand, so, replacing cement with
70% EVM reduces both bulk density and thermal conductivity.
As compared with the thermal conductivities of the conventional
sand mortars reported in many articles [24–28], the prepared
mortars showed a significant reduction in thermal conductivity.
The low density is due to the presence of a large number of pores
and air voids in the structure as a result of the porous nature of
EVM; this is confirmed by SEM micrographs shown in Fig. 9.
Porosity is the main factor which decreases the thermal conduc-
tivity of cement and concrete structures; the air contained in the
pores contributes significantly to the poor conduction properties
of the material, due to the low thermal conductivity of air [29].
Reducing the thermal conductivity increases the thermal resis-
tance (R-value) provided by the lightweight cementitious com-
posite, significantly contributing to a reduction in heating and
cooling loads in residential and commercial buildings, i.e. achiev-
ing energy saving in building sector. The partial replacement of
EVM with NMK (on a weight basis) has not a considerable effect
on bulk density and thermal conductivity. The very little increase
Table 4
Density and thermal conductivity variations of the prepared mortars.
Mix code NMK ratio, Bulk density, Thermal conductivity,
% kg/m3 W/m K
M0 0 1245 0.380
M1 2 1247 0.382
M2 4 1251 0.383
M3 6 1254 0.383
M4 8 1259 0.384
M5 10 1261 0.389
in thermal conductivity may be attributed to the densification of
internal cement matrix, which leads to increase heat transfer by
conduction.
3.5. Differential scanning calaorimetry (DSC)
Fig. 7. shows the DSC thermograms of the plain (M0) and 10%
NMK-modified WPC incorporating 70 vol% of EVM (M5) hydrated
for 28 days. Evidently; there are almost two main endothermic
peaks. The first endothermic peak located at 88–158 °C is attrib-
uted to the CSH decomposition. The second endothermic peak
observed at 475–533 °C represents the CH decomposition. The
main feature of the thermograms is the decrease of the peak
area characterizing the CH phase and the increase of the CSH
peak area, which confirm the partial transformation of CH into
CSH, this is an indication for the NMK pozzolanic activity. The
additional new CSH provided by pozzolanic reaction will deposit
in the pore system inside cement matrix, improving the
microstructure and enhancing the mechanical strength further-
more, reducing the migration of free water inside cement
skeleton.
3.6. Heat of decomposition (Enthalpy)
Fig. 8. depicts the variations of the heat required for decompo-
sition of the C–S–H and CH phases as a function of NMK %. Clearly;
as the amount of NMK increases, the heat of decomposition of CSH
increases, while that required for decomposition of CH decreases,
which confirm the high degree of hydration in the cement pastes
modified with NMK particles. In addition, the amounts of heat
required for the decomposition of CH decreases as a result of its
consumption by NMK. The decrease of the enthalpy of CH indicates
that, the CH phase liberated during hydration of NMK-modified
cement has an ill crystalline structure (i.e. eroded crystals) this is
caused by the pozzolanic reaction with NMK. The hardened
WPC–NMK paste has a denser structure as compared to the neat
WPC paste since the amorphous hydration products possess higher
strength characteristics as compared to the crystalline hydrates
[30].
3.7. Microstructure characteristics
In order to investigate the role of NMK in enhancing mechanical
strength and reducing the capillary water absorption of the NMK-
modified mortars, SEM analysis was performed on the control mix
100 150
CH CSH
140
90
Decomposition heat for CSH, J/g
Decomposition heat for CH, J/g
R² = 0.9817
130
80
120
70
110
R² = 0.9861
60
100
50 90
0 2 4 6 8 10
NMK, Wt%
Fig. 8. Variations of the decomposition heat for CSH and CH phases at 28 days of
curing as a function of NMK %.
 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283
Cement paste
EVM aggregate
Fig. 9a. SEM micrographs and EDAX patterns for selected areas of the control mix (M0).
(cement replaced with 70 vol% EVM, without NMK) as shown in
Fig. 9a and the mix with the highest mechanical performance
(incorporating 10% NMK on basis of EVM weight) as shown in
Fig. 9b. These micrographs can give visual evidence of the
microstructural characteristics responsible for the enhancement
of the mechanical and physical properties of the NMK modified
mortar. As it is clear from SEM micrographs, EVM aggregates are
embedded in the cement matrix, the images demonstrated good
adhesion/bonding in cement paste. The phases identified for the
control mix cement are the nearly amorphous CSH, the small
hexagonal particles stacked in layers of CH and hexagonal plates
of mono-sulfate hydrate crystals. The microstructure revealed the
non-uniform distribution of the hydration products. Furthermore,
capillary pores were seen near the interfacial transition zone
(ITZ) between the EVM aggregate and cement paste. The
microstructure of the hardened cement paste containing NMK
appeared considerably dense and compact with relatively less cap-
illary pores as compared to the control mix; moreover, large crys-
tals of CH are disappeared. The NMK modified the interfacial
transition zone and increased the bond between the cement paste
and aggregate due to the physical packing effect. Also, the
281
pozzolanic activity of NMK resulted in the production of additional
CSH which gets deposited in the ITZ.
4. Conclusion
Based on the experimental results of this study, the following
conclusions can be drawn:

NMK is very effective in enhancing the mechanical performance
and minimizing the capillary water absorption of high volume
EVM white cement composites, replacing 70 vol% cement.

Partial replacement of EVM by 10% NMK has significantly
enhanced the compressive and flexural strengths by about 57
and 59%, respectively.

NMK has considerably reduced the capillary water absorption
by about 74% at 28 days of hydration.

NMK has led to a great improvement in the microstructure.

The developed lightweight vermiculite cement composites are
characterized by low density and thermal conductivity while
have an enhanced mechanical strength, i.e. are fully recom-
mended for energy efficient building envelopes.
282 H. Shoukry et al. / Construction and Building Materials 112 (2016) 276–283

Fig. 9b. SEM micrographs and EDAX patterns for selected areas of 10% NMK-modified mix (M5).

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