Construction and Building Materials 35 (2012) 900905

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Construction and Building Materials

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Behavior of blended cement mortars containing nano-metakaolin at

elevated temperatures
M.S. Morsy , Y.A. Al-Salloum, H. Abbas, S.H. Alsayed
Specialty Units for Safety & Preservation of Structures, Department of Civil Engineering, College of Engineering, King Saud University, P.O. Box 800, Riyadh 11421, Saudi Arabia

h i g h l i g h t s
" Studied effects of high temperature on behavior of nano-metakaolin cement mortars.
" There was an initial increase in compressive and exural strengths at 250 C.
" Compressive & exural strengths decrease appreciably at temperatures above 250 C.
" Replacement of cement by 5% nano-metakaolin at 25 C leads to optimal mortar.
" Replacement of cement by 15% nano-metakaolin at above 250 C gives good results.

a r t i c l e

i n f o

Article history:
Received 3 March 2012
Received in revised form 23 April 2012
Accepted 29 April 2012
Available online 15 June 2012
Keywords:
Elevated temperature
Nano-metakaolin
Mortar
Microstructure
Mechanical properties
Thermal analysis

a b s t r a c t
The effects of high temperatures up to 800 C on the mechanical properties and microstructure of nanometakaolin cement mortars were investigated in this study. The blended cement used in this investigation is ordinary Portland cement (OPC) containing nano-metakaolin (NMK). The nano-metakaolin was
prepared by thermal activation of nano kaolin clay at 750 C for 2 h. The mortar was prepared using
blended cement: sand ratio of 1:3 and water/binder ratio of 0.6. The cement mortar pastes were cured
under water for 28 days; then dried at 105 5 C for 24 h and then exposed to 250, 450, 600 and
800 C for 2 h. The compressive and exural strengths were measured for blended cement mortar and
compared with the strength of pure OPC mortar. It was found that after an initial increase in compressive
strength at 250 C for the mortar specimens, the strength decreased considerably at higher temperatures.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
Concrete is well known for its capacity to endure high temperatures and res owing to its low thermal conductivity and high
specic heat [1]. However, it does not mean that re, or high temperatures, do not affect concrete at all. High temperature may result in color changes along with signicantly affecting the
concretes compressive strength, modulus of elasticity, concrete
density and its appearance [25]. One of the most important physical deterioration processes that inuence the durability of concrete structures is high temperature. Nevertheless, it is possible
to minimize the harmful effects of high temperatures on concrete
by taking preventive measures, such as choosing the appropriate
materials. Material properties, such as properties of aggregate,
cement paste and aggregatecement paste bond, and thermal

Corresponding author.
E-mail address: msmorsy@yahoo.com (M.S. Morsy).
0950-0618/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.04.099

compatibility between aggregate and cement paste, greatly affect

the high-temperature behavior of concrete [610].
Therefore, many researchers have recently become increasingly
interested in the possibility of developing concrete that has better
re resistance which can be improved in various ways as discussed. The replacement of cement with pozzolanic materials such
as slag, silica fume or y ash, for example, is a very efcient measure [1117]. The addition of polypropylene bers to concrete mix
is also found to be useful [1820].
The benecial effect of mineral admixtures, such as y ash, silica fume, silica our, metakaolin and ground granulated blast-furnace slag, with respect to high-temperature resistance arises from
the stabilization of Ca(OH)2 released during cement hydration by
means of pozzolanic reaction. The detrimental effects of Ca(OH)2
are that, the micro-cracks appear rst in the areas of Ca(OH)2 concentration at about 300 C [5], due to the decomposition of calcium
hydroxide into lime and water vapor above 350 C. Decomposition
of calcium hydroxide is not critical in terms of strength loss during
heating. However, it may lead to serious damage due to lime

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M.S. Morsy et al. / Construction and Building Materials 35 (2012) 900905

expansion during the cooling period [21]. Such damage can also be
observed during re extinguishing process, where CaO reacts with
water and turns to Ca(OH)2 with a signicant expansion.
When nano particles are used as supplementary cementitious
material (SCM) in concrete, various improvements can be attained,
thereby leading to improved permeability and strength. The nano
particles act as nuclei of hydration, possess pozzolanic behavior
[22], and can ll the voids in the cement matrix [2325]. Pozzolans
react chemically with calcium hydroxide liberated during cement
hydration to form cementitious compounds [26]. The large surface
area of nano particles and their abundance due to their small size
can facilitate the chemical reactions necessary to produce a dense
cement matrix with more calcium silicate hydrate (CSH) and less
calcium hydroxide contents. This, in turn, will enhance the overall
concrete performance. Nano particles are, in general, smaller than
the commonly used SCMs, making them more reactive and effective. Different forms of nano-silica (NS) and nano clays (NC) in cement paste have been shown to increase compressive strength,
reduce permeability, and develop a denser microstructure [27].
Nano particles can also strengthen the interfacial transition zone
between the cement paste and the aggregate, which would lead
to improved strength and permeability. For nano particles to be a
substitute for other SCMs of larger particle size, equal or better performance at lower or equal cost is needed.
The object of this work is to provide experimental data on the
residual mechanical and physical properties of blended cement
mortar containing NMK as a pozzolanic material when exposed
to heat. These properties are very important for a safe design of
concrete and in the repair of concrete structures when exposed
to elevated temperature.

Fig. 1. TEM micrograph of NMK.

2. Experimental
2.1. Materials
The ordinary Portland cement (OPC), ASTM C-150 Type I [28] used in this investigation was supplied by Yamama Cement Company, Saudi Arabia.
The Blaine surface area of nano kaolin was 48 m2/g and average dimensions
100  50  10 nm and was supplied by the Middle East Mining Investments Company (MEMCO), Cairo, Egypt. The morphology of nano kaolin is shown in Fig. 1.
The raw nano kaolin consists of kaolinite, illite and quartz as major mineral phases,
whereas NMK contains only illite and quartz. The heat treatment of raw kaolinite at
750 C resulted in the disappearance of its crystalline structure and the development of an amorphous structure as shown in Fig. 2. The oxide composition of nano
kaolin and OPC are summarized in Table 1. Commercial local red sand was used as a
ne aggregate in the mortar.
Fig. 2. XRD patterns of kaolin and metakaolin.
2.2. Mortar Preparation and Identication
In this investigation OPC was partially substituted by NMK by weight as illustrated in Table 2. The blended cement mixes were prepared by mixing OPC and
NMK in the dry state for successive periods of 5 min until homogeneity was
achieved. The mortar was prepared using blended cement: sand ratio of 1:3 and
water/binder ratio of 0.6.
The mortar pastes were molded into 5 cm cubes for compressive and
4  4  16 cm prisms for exural strengths tests. The molds were vibrated for
one minute to remove any air bubbles. The samples were kept in molds at 100% relative humidity for 24 h, and then cured in water for 28 days. The hardened cement
mortar specimens were removed from water before testing. The compressive and
exural tests were performed on wetted control and blended specimens. The hardened cement paste was dried at a temperature of 105 5 C for 24 h in an oven to
remove the free water. Then, they were kept for 2 h at temperatures 250, 450, 600,
and 800 C. Each temperature was maintained for 2 h to achieve the thermal steady
state. The specimens were allowed to cool gradually inside the furnace to room
temperature. The compressive strength was performed on wetted and heated specimens. The crushed samples (wetted and heated) resulting from compressive
strength tests were grinded for thermal analyses, SEM and X-ray diffraction studies.
The evaporable water of the hydrated crushed samples was removed using the
method described elsewhere [29].
Differential Thermal Analyses run were conducted using a Shimadzu DTA-50
thermal analyzer at a heating rate of 20 C/min. The sample chamber was purged
with nitrogen at a ow rate of 30 ml/min. The crystalline phases present in the
hydration products were identied using the X-ray diffraction technique. Nickle-l-

Table 1
Chemical composition of materials in percent by weight.
Oxide composition

OPC (%)

Nano Kaolin (%)

CaO
SiO2
Al2O2
Fe2O3
MgO
SO3
Na2O
K2O
TiO2
Total
Ignition loss

63.85
19.83
5.29
3.53
0.52
2.43
0.21
0.07

95.73
4. 27

0.01
48.00
36.50
0.20
0.02

0.03
0.07
1.30
86.13
13.87

tered Cu-Ka radiation at 40 kV and 20 mA were used throughout in a Philips PW

1390 diffractometer. Scanning speed of 2/min. was used. The scanning electron
microscope JWEL JSM 6360A was used for identication of the changes occurred
in the microstructure of the formed and/or decomposed phases.

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Table 2
The dry mix composition of blended cement in percent by weight.
Mix

OPC (%)

NMK (%)

M1
M2
M3
M4

100
95
90
85

0
5
10
15

3. Results and discussion

The compressive and exural strengths of blended NMK cement
mortar hydrated for 28 days under water are shown in Fig. 3. It is
clear that, the compressive and exural strengths increase with
increasing replacements up-to 5% and then decrease with its increase up-to 15% by weight. Obviously, the replacement of OPC
by NMK enhances the compressive and exural strengths up to
15% by weight. At 5% NMK replacement the increase in the compressive and exural strengths was 1.23 and 1.08 folds than the
control sample respectively. Basically NMK enhances the compressive and exural strengths of hardened cement mortar by two
mechanisms. The rst mechanism is the physical ller of NMK particles in interstitial spaces inside the skeleton of hardened structure of cement mortar, thereby increasing its density as well as
its strength. The second mechanism is the pozzolanic reaction, between NMK and the free CH liberated during OPC hydration, which
produces additional CSH. The reduction in the compressive and
exural strengths at higher NMK replacements may be due to
the decrease of C3S and b-C2S phases in blended cement. Also, at
higher ratio replacements the NMK agglomerates around the OPC
grains and hinder the hydration process. Therefore, the amount
of hydration product is decreased; leading to the development of
fewer points of contact which act as binding centers between cement grains.
Fig. 4 illustrates the development of compressive strength for
control and blended cement mortars exposed to 250, 450, 600
and 800 C for 2 h. It is evident that, the compressive strength increases with temperature up to 250 C then decreases as the temperature increases up to 800 C. The gain in compressive strength
at 250 C is 28.4%, 5.2%, 33.7%, and 36.6% while the corresponding
loss in compressive strength at 800 C is 57.0%, 61.5%, 58.1%, and
46.5% for mixes M1, M2, M3 and M4, respectively. Moreover the increase of compressive strength of blended cement mortar M2 is
limited in comparison to its control sample and the other

Fig. 3. Compressive and exural strength of NMK-cement mortar versus NMK

proportion.

investigated samples (M3 and M4). The blended cement mortar

containing 5% NMK (M2) achieved the maximum gain in compressive and exural strengths than its control sample in comparison to
other blended mixes at ambient environment (Fig. 3). When a denser structure is exposed to elevated temperatures the dehydration
process of the formed hydrate is associated with driving out of free
water and the remaining fraction of water leads to formation and
development of micro-cracks. However, the compressive strengths
of blended cement mortars, M3 and M4 exhibited slow decrease
than those of M1 and M2 specimens as the exposure temperature
increased up to 800 C. Evidently, the increase in compressive
strength up to 250 C may be due to the additional hydration of
unhydrated cement grains as a result of steam effect under the
condition of the so-called internal autoclaving effect. The increase
in compressive strength of blended cement mortars may be due to
the pozzolanic
reaction of
amorphous aluminosilicate
(Al2O3
2SiO2) present in NMK with CH librated during OPC hydration to form an additional amount of CSH that has low Ca/Si ratio
with high strength [30] and calcium aluminates hydrate (CAH)
phases that deposit in the pore system. Furthermore, the additional
hydration products bridge the pore system leading to a decrease of
the thermal stresses generated around the pores. Cement matrix
with higher contents of gel-like hydration products and lower
Ca(OH)2 crystal contents has improved re resistance. This phenomenon, leads to low increase in strength and decreases porosity
[31]. Also, the decrease in compressive strength with increase in
temperature above 250 C may be due to the dehydration of calcium hydroxide at about 500 C producing CaO and H2O. Strength
losses over 600 C, are mainly caused by calcium carbonate dissociation and subsequent CO2 escape from CaCO3. Strength losses of
M4 blended cement mortar are less signicant than that of its control sample, in comparison to M1, M2 and M3 cement mortar.
Fig. 5 shows variation in exural strength for control and
blended cement mortars exposed to 250, 450, 600 and 800 C for
2 h. It is evident that, the exural strengths of blended cement
mortars increase with temperature up to 250 C, then decrease
up to 800 C. The gain in exural strength of blended mortar at
250 C is 3.4%, 13.9%, and 27% for mixes M2, M3 and M4, respectively. However, the increase in exural strength up to 250 C
may be due to the increased content of hydration products, which
play the dominant role, especially for concrete at the age of
28 days. This process exhibits similar behavior of strength at certain curing treatments (so-called steam curing). Also, due to physical ller of NMK which act as ber in cement structure.
Furthermore, the decrease in exural strength with increase in
temperature from 250 C to 800 C is due to the formation of
micro-cracks. Also, the reduction in exural strength can be

Fig. 4. Compressive strength of NMK-cement mortar versus temperature.

M.S. Morsy et al. / Construction and Building Materials 35 (2012) 900905

903

Fig. 5. Flexural strength of NMK-cement mortar versus temperature.

Fig. 7. DTA thermograms of hydrated cement mortars and NMK-cement mortars:

(a) control cement mortar M1 and (b) blended cement mortar (M4).

Fig. 6. XRD patterns of hydrated cement mortars and NMK-cement mortars: (a)
control cement mortar (M1) and (b) blended cement mortar (M4).

attributed to the driving out of free water and a fraction of hydration water of cement mortar due to high temperatures. Dehydration of concrete causes a decrease in its strength, elastic

modulus, coefcient of thermal expansion and thermal conductivity [32]. Moreover, the replacement of OPC by 10 and 15% NMK in
cement mortar resulted in marginal decrease and/or nearly stable
exural strength up to 450 C followed by a sharp decrease. In cement mortar containing 10% and 15% NMK, the exposure up to
450 C led to further hydrothermal reaction of unhydrated cement
grains as well as pozzolanic reaction of NMK with calcium hydroxide being released during the hydration process. Basically, the decrease in exural strength due to increase of temperature from 450
to 550 C is due to dehyroxylation of Ca(OH)2. The increased microcracking is the result of high thermal stresses, which are generated
due to the induced temperature gradients up to 800 C.
The XRD diffractograms obtained for the hydrated cement mortar samples before and after exposure to elevated temperatures are
shown in Fig. 6. The XRD patterns of control cement mortar sample
are illustrated in Fig. 6a. The main phases identied in hydrated cement mortar are CSH gel, unhydrated C3S and b-C2S, calcium
hydroxide and calcium carbonate. It was found that the amounts
of CSH and CH increased with heating at 250 C. This is because
further hydration of unhydrated cements grains. Evidently, the
crystalline phase of CH (portlandite) decreased as the temperature
increased up to 800 C. This is due to thermal decomposition of calcium hydroxide phase at 570 C. The effect of replacement of OPC
by 15% NMK is shown in Fig. 6b. The calcium hydroxide phase decreases as the exposure temperature increases, while the weak
peaks of CAH and calcium aluminates sulfate hydrate (CASH) in
blended cement mortars increase. Moreover, it can be concluded

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M.S. Morsy et al. / Construction and Building Materials 35 (2012) 900905

Fig. 8. SEM micrographs of control and blended cement mortars subjected to elevated temperatures, (a) control mortar hydrated at 25 C, (b) blended mortar containing 15%
NMK hydrated at 25 C, (c) control mortar thermally treated at 250 C, (d) blended mortar containing 15% NMK thermally treated at 250 C, (e) control mortar thermally
treated at 800 C, and (f) blended mortar containing 15% NMK thermally treated at 800 C.

from these diagrams that, after duration of 2 h, CSH, CH and calcium carbonate all remained persistent at 250 C; both CH and calcium carbonate decomposed but CH decomposed at a slower rate
than calcium carbonate, whereas CSH was persistent at 800 C.
The variations of the DTA thermograms of control cement mortar, (M1), and blended cement mortar, (M4) at ambient temperature and exposed to 250 and 800 C are shown in Fig. 7.
Evidently, there are almost four endothermic peaks. The rst peak
located at about 100110 C, is mainly due to the decomposition of
the nearly amorphous calcium silicate hydrates as well as the calcium sulpho-aluminate hydrates. The second endothermic peak
observed at about 160 C represents the decomposition of the crystalline part of CSH. The third endothermic peak at about 470 C is
due to the dissociation of of Ca(OH)2. The fourth endothermic peak
was observed at around 580 C which represents the transformation of quartz. As the exposure temperature increases the peak area
of calcium hydroxide increases up to 250 C and shifts towards
lower temperature at 800 C as shown in Fig. 7a. This is due to
the formation of ill-crystals of Ca(OH)2. Also, it is clear that the
thermograms of the blended cement mortars made of mix M4 that
thermally treated at 250 C shows a sharp CH endotherm and shifts
to a higher temperature. This is due to the formation of well-crystals of Ca(OH)2. Moreover the thermal treatment at 800 C exhibits
a very weak CH endothermic peak as shown in Fig. 7b. It is clear

that the calcium hydroxide peak area decreases as treatment temperature increases. Evidently, this is due to further reaction between NMK and CaO at high temperature up to 800 C.
The scanning electron micrograph of control mortar (M1) and
blended cement mortar containing 15% NMK (M4) and thermally
treated at 25, 250 and 800 C are shown in Fig. 8. Evidently, the
microstructure of the control mortar at 25 C displays the existence
of microcrystalline and nearly amorphous, CSH; in addition to large
crystals of calcium hydroxide as shown in Fig. 8a. Furthermore, the
micrograph of blended cement mortar containing 15% NMK displayed the presence of a nearly amorphous CSH and dense microstructure as shown in Fig. 8b. It was clear that, the microstructure
of OPC-NMK mortar, thermally treated at 250 C, was perfectly stable for thermal treatment and illustrates a dense structure of hydrated products as shown in Fig. 8d. This can be clearly
understood from the microstructure of the hardened blended cement mortar (M4) after thermal treatment at 250 C which displayed the existence of CSH and calcium hydroxide (CH).
Therefore, the replacement of OPC by 15% of NMK resulted in an
improvement of the thermal stability of the hardened blended cement mortar made of mix M4 as indicated from the SEM micrograph shown in Fig. 8d. Thermal treatment of mix M1 at 800 C
displays decomposition of the hydration products with the formation of wide micro-cracks as shown in Fig. 8e. Furthermore, the

M.S. Morsy et al. / Construction and Building Materials 35 (2012) 900905

cement paste was separated from the aggregate thereby creating

gaps. Moreover, the thermal treatment of blended mortar M4
exhibited all hydrated phases including CSH and CH appearing as
amorphous structures losing their characteristic crystalline structure due to less formation of narrow micro-cracks as shown in
Fig. 8f. Poor microstructure is associated with generation of undesirable conguration of CSH crystals, and increased cracking at
high temperature. Generally, the CSH crystals grow long, thin/narrow and occupy less space in the matrix at high temperatures,
thereby resulting in decreased densication of the microstructure
[33]. The increased micro- cracking is the result of high thermal
stresses that are generated due to the induced temperature
gradients.
4. Conclusions
In this study, the effect of experimental parameters, namely
heating degree and NMK, on the compressive and exural
strengths is investigated experimentally; the research results include the following:
1. The replacement of OPC by 5% NMK in cement mortar hydrated
at ambient temperature increases the compressive and exural
strengths of cement mortar.
2. It is found experimentally that the higher the compressive and
exural strengths results were obtained from the specimens
containing 15% NMK, as compared with other replacement percentages considered in this study for all thermal treatment,
with increase of temperature from 250 to 800 C.
3. The test results showed that the compressive and exural
strengths increases up to 250 C and then decreases as the
exposure temperature increases up to 800 C. The reduction in
compressive and exural strengths may be due to the occurrence of micro- and macro-cracks in mortars because of high
temperatures.
4. The blended cement mortar M4 can be applied as a re resistance binding material.
5. The SEM micrograph of control mortar thermally treated at
800 C possesses a formation and growth of micro-cracks than
blended cement mortar containing 15% NMK.
6. Thermal treatment of blended cement mortar containing 15%
NMK at 250 C indicate a formation of well crystalline CH.

Acknowledgments
The authors extend their appreciation to the Deanship of Scientic Research at King Saud University for funding the work through
the research group project No. RGP-VPP-064. Thanks are also extended to the MMB Chair for Research and Studies in Strengthening and Rehabilitation of Structures, at the Department of Civil
Engineering, King Saud University for providing technical support.
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