Construction and Building Materials 73 (2014) 636–644

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Construction and Building Materials

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

Use of nano-structured waste materials for improving mechanical,

physical and structural properties of cement mortar
K. Al-Jabri a, H. Shoukry b,⇑
a
Department of Civil and Architectural Engineering, College of Engineering, Sultan Qaboos University, P.O. Box 33, Al-Khoudh, Post Code 123, Oman
b
Department of Physics, College of Science, King Khalid University, Abha, Saudi Arabia

h i g h l i g h t s

 The production of nano-structured industrial waste minerals by ball milling has been investigated.
 The ball milling is beneficial for particle size reduction of waste minerals from micro to nano level.
 The ball milling result in significant modification in particles morphologies.
 The nanostructured minerals improve the mechanical, physical and structural properties of mortar.

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

Article history: This work investigates the high-energy ball-milling process in order to develop ultra fine nanostructured
Received 8 September 2014 mineral admixtures. Three types of waste byproduct minerals including; spent catalyst (S.C), copper slag
Received in revised form 26 September (BFS) and cement kiln dust (CKD) were milled for 2 and 4 h in high energy planetary ball mill and then
2014
calcined at 750 °C. The prepared materials were characterized for their particle size/morphology by field
Accepted 3 October 2014
Available online 25 October 2014
emission scanning electron microscope (FESEM). X-ray diffraction (XRD) was used for crystallinity stud-
ies and phase analysis. Upon milling, nanostructured particles were obtained with dimensions less than
100 nm. The milling process led to modification of particles morphology and surface texture. XRD pat-
Keywords:
Ball milling
terns indicated that nanostructured materials are found to be more amorphous as compared with the
Surface area fresh (as received) materials. The aim of this study was also directed to investigate the effect of the pre-
Cement mortar pared nanostructured materials on compressive strength and capillary water absorption (sorptivity) of
Compressive strength mortars. For this purpose, blended mortar samples were prepared with partial replacement of cement
Water absorption by different amounts 5%, 10%, 15% and 20% of nanostructured S.C, BFS and CKD. The compressive strength
Microstructure and sorptivity tests were performed at 28 days of curing; the phase composition/decomposition was
studied by (XRD) and microstructure was investigated by (FESEM). Results showed that compressive
strength of nanostructured blended mortar is greater than that of plain mortar, an enhancement of about
33% was observed. The capillary water absorption generally decreases with increasing replacements of
cement by nanostructured materials. A decrease of about 44% was observed at 20% of nanostructured
CKD. The microstructure of blended mortar appeared quite dense and compact with great modifica-
tion/improving for interfacial transition zone (ITZ) between cement paste and aggregate.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction
In the construction industry, cement an energy intensive mate-
rial, can partially be replaced with mineral admixtures as supple-
mentary material in producing cement and concrete composites
for conserving cement, utilizing waste materials, saving the envi-
ronment, reducing CO2 emission and improving their performance.
The properties of cement mortars and concrete in fresh state (flow
⇑ Corresponding author.
E-mail address: hamadashoukry@yahoo.com (H. Shoukry).
properties and workability) are, for instance, governed by the par-
ticle size distribution (PSD), but also their properties in hardened
state, such as strength and durability, are affected by the mix grad-
ing and resulting particle packing [1]. One way to further improve
the packing is to increase the solid size range, e.g. by including par-
ticles with sizes below 300 nm.
Various methods have been implemented to improve cement
paste and concrete properties in the past. The addition of supple-
mentary materials into cement and concrete has been considered
by various researchers all over the world for improving the
strength and durability of cement paste, mortar and concrete.
These include various supplementary cementing materials, includ-

http://dx.doi.org/10.1016/j.conbuildmat.2014.10.004
0950-0618/Ó 2014 Elsevier Ltd. All rights reserved.
 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644
Table 1
Chemical composition of raw materials (mass%).
Oxide composition (wt%) BFS S.C
SiO2 33.05 39.21
Al2O3 2.79 37.68
Fe2O3 53.45 0.66
CaO 6.06 0.05
MgO 1.46 0.26
SO3 1.84 – 1.65
L.O.I. 0 21.43
Na2O 0.28 0.43
K2O 0.61 0.06
CuO 0.46
ing natural pozzolans as well as artificial ones such as fly ash and
silica fumes and other industrial by-products such as copper slag,
cement kiln dust and pulverized blast furnace slag [2]. These sup-
plementary materials are also known as pozzolans, as they create
the pozzolanic effect by chemically converting calcium hydroxide
(CH) liberated during the hydration of cement into calcium silicate
hydrate (C-S-H) gel which is the major strength contribution com-
ponent among the hydration products. The use of mineral addi-
tions in cement-based materials has grown in recent years, due
to sustainability and environmental issues or due to the technical
advantages gained from the final product [3,4]. When used as a
partial replacement of cement, suitable additions can improve
the performance of materials through modifications in the fresh
and hardened states, physical and chemical properties, as well as
the hydration and microstructure.
Therefore, research on the use of nano-sized particles produced
from mineral admixtures, mineral additives, and industrial by-
products in cement, cement mortars, and concrete has gained spe-
cial attention in recent years in order to achieve the substantial
advantages associated with the use of nanotechnology in the con-
struction industry [5–14]. Recent research studies proved that
nano-engineering of cement-based materials offer tremendous
potential for the development of new cement additives such as
novel superplasticizers, nano-particles, and nano reinforcements
which can have significant effect in enhancing the mechanical
properties and durability of concrete [10]. This can be achieved
by enhancing the distribution of hydration products within the
cement matrix through a physical mechanism causing the hydra-
tion products to diffuse and envelope the nanoparticles which
act as nuclei leading to formation of a more compact matrix with
smaller crystals of calcium hydroxide (CH) [15–17]. Also, nanopar-
ticles can reduce significantly the porosity of the cement/concrete
matrix by acting as a filler to fill up voids causing densifying the
microstructures of interfacial transition zone (ITZ) [18,19].
In this study an attempt has been made to produce ultrafine
nano-structured pozzolans by thermo-mechanical activation of
CKD BFS
Fig. 1. Photo of the prepared/milled materials.
637
the industrial waste byproduct minerals (spent catalyst, copper
slag and cement kiln dust). The effect of the prepared nano-struc-
CKD tured minerals on mechanical strength, capillary water absorption
15.84 and microstructure of hardened cement mortars was investigated.
3.57
2.76 2. Experimental
63.76
1.93 2.1. Materials
6.38 The materials used in this study are:
0.33
2.99 Copper slag (BFS)
–
Copper slag is a by-product obtained during the production of copper metal,
which can be used as pozzolana in the production of cementing materials.
Copper slag used in this work was brought from Oman Mining Company, which
produces an annual average of 60,000 tons.
Spent catalyst (SC)
The spent catalyst used in this study is one of the waste catalysts produced in
oil refineries in Oman (Sohar).
Cement kiln dust (CKD)
CKD is produced as a solid waste from the pre-heater by-pass systems during
the manufacture of Portland cement clinker. Chemical analyses of S.C, BFS and
CKD are presented in Table 1.
2.2. Method
2.2.1. Thermo-mechanical activation
The ‘‘top-down’’ approach [10] was adopted to prepare the by-product materi-
als to the nanoscale level. In this approach, the larger structures are reduced in size
to the nanoscale while maintaining their original properties without atomic level
control or deconstructed from larger structures into their smaller composite parts.
In order to produce nanoparticles, the starting/fresh raw materials were milled with
high power planetary ball mill (FRITSCH Pulverisette 5). The duration of milling
process was 2 and 4 h. The following milling conditions were maintained: the input
quantity of material represents 75% of the grinding jar size 250 ml, and balls type is
Zirconium, the diameter of each ball is 10 mm, the number of balls was 9 and the
rotation speed of the planet carrier was 300 rev/min.
Calcination: After milling, the output material was burned for 2 h at 750 °C for
thermal activation. Fig. 1 presents a photo of the prepared materials.
2.2.2. Preparation of blended mortar
 The blended cement mortar samples were prepared by partial replacement of
cement with different ratios of nanostructured (S.C – BFS – CKD) ranging from
0% up to 20%. Samples were prepared with the standard water of consistency.
 Mix proportions, by weight, for mortars were 1 (binder): 3 (sand), the binder
content consists of cement and the additives (nanostructured minerals).
 The ingredients were homogenized on an electric mixer to assure complete
homogeneity.
 The samples were cast as cubes 7  7  7 cm for compressive strength test.
 The molds filled with cement were vibrated for 1 min to remove entrapped air
bubbles.
 The samples were kept in molds for 24 h, and then demolded and cured in
water for 28 days.
S.C
638 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644

Test reduced to a large extent with the appearance of nano-structured

particles with dimension less than 100 nm. Fig. 3c shows the ultra-
fine nature of the milled S.C. and satisfies the reduction of particle
Paraffin size to the nano level.

Seat
Water
a

Fig. 2. Experimental set up of capillary water absorption test.

3. Testing and analysis

3.1. Compressive strength

The prepared samples were subjected to compressive strength

tests using 600 KN compressive machine (DARTEC) according to
ASTM C109 [20]. The loading rate on the sample was 0.2 KN/s. Three
samples per batch were tested and the average strength is reported.

3.2. Capillary water absorption (sorptivity)

10 µm

The experimental set up of capillary water absorption test is

presented in Fig. 2. In order to perform the test, the specimens
were dried in oven at about 105 °C until constant mass was
obtained. The sides of the specimen were coated with paraffin to b
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 level on the pan was maintained
about 5 mm above the base of the specimen during 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 cap-
illary absorption coefficient (k) was calculated by using the for-
p
mula: k = W/(A t) where W = amount of water absorbed in g,
A = cross sectional area in (cm2) contact with water and t = time
in seconds [21].

3.3. Scanning electron microscopy (SEM)

The field emission scanning electron microscope (Jeol JSM 7600

F) was used to identify the changes occurred in the microstructure 1 µm

of the formed and/or decomposed phases. The resolution of SEM

was 1 nm.
c
3.4. X-ray diffraction spectroscopy (XRD)

Nickel- filtered Cu ka radiation at 40 kV and 40 mA was used

throughout a Philips PW3050/60 diffractometer provided with a
proportional counter. A scanning speed of 2h/min, and a chart
speed of 10 mm/min, was used in all cases.

4. Results and discussion

4.1. Particle size and morphology

Fig. 3 shows the morphology and size of the ball milled spent
catalyst as compared with the starting fresh material. The grains
of the as received spent catalyst showed relatively large homoge-
neity in particle size with an average diameter less than 100 lm 100 nm

and characterized by spherical morphology as depicted from

Fig. 3a. After 2 h of milling the spherical structure of fresh S.C. (a): Fresh S.C, (b): After 2 hrs milling
was partially destroyed and the average particle size is reduced.
(c): After 4 hrs milling
Particles with dimensions less that 0.5 lm had been identified
Fig. 3b. Increasing the milling time to 4 h resulted in complete dis- Fig. 3. SEM photomicrographs of the starting/fresh and ball milled spent catalyst
tortion of the spherical morphology; however the particle size was (S.C).
 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644 639

It was observed also that the SEM analysis was not capable of
detecting a single particle even at higher magnifications while
agglomerates of particles were detected. This is because of the
a
inter-particle fusion caused due to the high surface energy resulted
from the mechanical activation/ball milling process.
Fig. 4a shows the SEM micrograph of the as received copper
slag. As can be seen, the particles have heterogeneous morpholo-
gies and appear like fractured pieces with distinct and sharp edges.
The average grain size is in the range of 200 lm. SEM micrograph

100 µm

1 µm

b
b

1 µm
100 nm

c
c

1 µm
100 nm

(a): Fresh BFS, (b): After 2 hrs milling (a): Fresh CKD, (b): After 2 hrs milling
(c): After 4 hrs milling (c): After 4 hrs milling
Fig. 4. SEM photomicrographs of the starting/fresh and ball milled copper slag Fig. 5. SEM photomicrographs of the starting/fresh and milled cement kiln dust
(BFS). (CKD).
640 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644
of the particles milled for 2 h is shown in Fig. 4b. It indicates the
ultrafine characteristics of the ball milled particles and suggests
that the milling process leads to modification of particles morphol-
ogy where the particles appear finer with ill-defined edges which
suggest some amorphous characteristics. Increasing the milling
time actually resulted in decreasing the particle size and increasing
the homogeneity.
The nano-structured slag particles were achieved due to the ball
mill material as seen from Fig. 4b and c. Semi spherical particles
were identified. Also the texture of slag has changed from glassy
smooth to irregular and rough surfaces. The outer glassy finish of
the fresh slag may have been eroded during ball milling and the
inner crystalline core may have been exposed after ball milling
for 4 h. The increased surface roughness supports the higher sur-
face energy of ball milled particles. The increased surface rough-
ness gives the particles great importance when used as partial
replacement of cement in mortar and concrete industry. Since,
the rough particles will achieve good bonding within the cement
matrix; this in turn will contribute to the enhancement in mechan-
ical strength and result in improving the microstructure.
Fig. 5 shows the morphology and size of the ball milled CKD as
compared with the starting fresh material. It can be seen from
Intensity, CPS
(a): S.C
Fig. 6. XRD patterns of the starting/fresh and ball milled minerals.
Fig. 5 that the grain size of the as received CKD is in the range of
10 lm. The grains appeared as a collection/agglomeration of parti-
cles with non uniform shapes. After milling the particles had dis-
persed and instead more fine particles with great modification in
morphology have been determined. Semi spherical clusters were
identified with dimension less than 400 nm. Increasing the milling
time to 4 h resulted in minimizing the particle to a large extent
with the appearance of nano-structured particles with dimension
in range of 100 nm. At larger magnification it was observed that
even after milling for 4 h, the particles of CKD were crystalline; this
is shown in Fig. 4c and is further confirmed by XRD analysis.
4.2. Crystallinity and phase analysis (XRD analysis)
The mineralogical phase composition of the spent catalyst, cop-
per slag and cement kiln dust were determined using powder X-
ray diffractometry (XRD). Fig. 6 shows the XRD patterns of these
minerals after thermo-mechanical activation (milling for 4 h fol-
lowed by calcination at 750 °C) as compared with the as received
(fresh) samples.
The XRD pattern of S.C presented in Fig. 6a showed a broad dif-
fuse halo at 2h angle of about 23° which confirms the presence of
2 Theta, °
(b): BFS (c): CKD
 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644
amorphous content. The broad diffraction peak at 2h of 23 is typi-
cal silica characteristic and is attributed to the absence of an
ordered crystalline structure [22]. The observed sharp peaks repre-
senting the few crystalline mineral phases present in the material
and correspond to a hydrogen aluminum silicate like faujasite,
quartz, and kaolinite. BFS was found to be mainly composed of vit-
rified (amorphous) alumina-silicate in addition to a small amount
of crystalline minerals, such as quartz, mullite, mica etc. after
thermo-mechanical activation, significant peak broadening was
occurred. The peak broadening was caused by the structural disor-
der introduced during milling and indicates the higher degree of
amorphisation. BFS was totally converted to amorphous material
with the disappearance of the crystalline phases. The X-ray diffrac-
togram of CKD indicating that this mineral is a crystalline material
even after thermo-mechanical activation (see Fig. 6c).
XRD tests were performed to verify that the particle size reduc-
tion alone was not the sole factor in determining if thermo-
mechanical activation has been occurred. The amount of crystal-
line and amorphous phases in the materials might also change
due to the milling process. The results showed that for both (S.C
and CKD), the baseline of the XRD curves was approximately the
same, but the intensity of peaks in the XRD curves was varied
due to the milling process. The decreased crystalline phases of
the tested materials could be considered as an indication for the
increased reactivity. It was observed that the crystalline peaks of
all milled materials were lowered when compared to the as
received materials. It can be concluded that the materials having
the lowest crystalline peaks are the most highly reactive and these
materials can be applied as partial replacement of cement to
improve the mechanical strength of mortar. Since these minerals
contain amorphous active silica and alumina, so they are able to
promote the hydration of cement and participate in pozzolanic
reaction i.e. chemically convert the lime (calcium hydroxide) liber-
ated during cement hydration into calcium silicate hydrate (CSH)
which is the strength responsible phase.
4.3. Specific surface area (SSA)
The specific surface area of the as received and milled materials
as a function of milling time is shown in Fig. 7. As expected, SSA
increases with milling time for the three studied waste materials.
S.C showed the greatest enhancement of SSA. After 4 h of milling,
the rates of increase in SSA for S.C, BFS and CKD (as compared with
the as received materials) were about 425%, 419% and 397% respec-
tively. The significant increase in SSA is attributed to the reduction
of grain size due to milling process.
22000
20000 S.C BFS CKD
18000
16000
SSA (m2/kg)
14000
12000
10000
8000
6000
4000
2000
0 2
Milling time (hours)
Fig. 7. Variations of specific surface area for S.C, BFS and CKD as a function of the
milling time.
641
Increasing surface area of particles will result in increasing the
number of surface atoms of particles, which in turn form unsatu-
rated bonds so that are unstable and tend to react faster i.e. they
are highly active. The extreme fineness and the huge surface area
of the nanostructured S.C, BFS and CKD make them very effective
pozzolanic materials and their application in cement and concrete
structures will enhance the mechanical strength and improve the
microstructure.
4.4. Compressive strength
Fig. 8 shows the variation of compressive strength of cement
mortar blended with different amounts of nano structured (S.C –
BFS – CKD) at 28 days of curing.
It is evident that, for the mortar blended with nanostructured
(S.C and BFS), the compressive strength increases with increasing
nano structured materials replacement ratio up to 15% by about
20% and 14% respectively, this is a significant enhancement in
the compressive strength. The reasons for the increase in compres-
sive strength may be due to the high amorphous silica content,
ultra fineness and specific surface area of the nanostructured (S.C
and BFS). Basically, the nanostructured materials enhance the
strength of hardened cement mortar by two mechanisms. The first
mechanism is the packing effect as filler into interstitial spaces
inside the skeleton of hardened microstructure of mortar and thus
increasing its density as well as the strength. The second mecha-
nism is the pozzolanic effect. The thermo-mechanical treatment
of S.C and BFS produced anhydrous alumino-silicate (Al2SiO5)
which is mainly amorphous material and behaves as a highly reac-
tive artificial pozzolan. The reaction of alumino-silicate with free
lime liberated during cement hydration was led to additional bond
strength and solid volume; resulting in higher strength of hard-
ened cement pastes. The pozzolanic reaction between the calcium
S.C. BFS CKD
40
38
36
34
32
30
28
26
Compressive strength, MPa
24
22
20
0 5 10 15 20
4
Replacement ratio (%)
Fig. 8. Compressive strength of nanostructured blended mortar at 28 days of
curing.
642 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644

2 limestone of the CKD, when the CKD is used as a partial substitute

-1/2

S.C BFS CKD of cement, can be both physical and chemical [23].
Capillary absorption coefficient mg.cm .sec

1.9
Calcium carbonate influences the hydration of C3S. Limestone
-2

1.8
1.7
1.6
1.5
1.4
1.3
1.2
1.1
1 to AFm is delayed or prevented due to the reaction between C3A
0% 5% 10%
Replacement ratio ( % )
Fig. 9. Capillary water absorption of plain and nano structured blended mortar
with different replacement ratios at 28 days of curing.
hydroxide and amorphous silica is capable to form supplementary
calcium-silicate-hydrate similar in composition and structure to
those obtained from Portland cement hydration. Nanostructured
materials can raise the hydrate reaction of cement and produce
more hydration products, which can be observed from the SEM
pictures.
Obviously, increasing the replacement ratio over 15% results in
decreasing the compressive strength to values which are still larger
than plain mortar (in case of S.C) and less than the plain mortar (in
case of BFS).
In case of nano structured CKD, It is clear that the compressive
strength increases with increasing replacement ratio up to 10%. An
enhancement of about 33% relative to plain mortar was observed.
CKD can consist of up to 50% calcium carbonate/limestone (CaCO3),
up to 30% quartz and clays and dehydrated clays. The effects of the
accelerates and enhances the rate of formation of C-S-H and CH.
Probably it offers nucleation sites for growth. Calcium carbonate,
also, can form a complex, calcium carbosilicate hydrate, with the
hydrated products of C3S. During cement hydration, C3A and cal-
cium sulfate react to form AFt (Aluminate–Ferrite-Trisubstituted
or Ettringite). Sulfate depletion typically occurs before the C3A
consumption is complete, resulting in the conversion of AFt to
AFm (Aluminate–Ferrite-Monosubstituted, Monosulfoaluminate,
or Monosulfate). The presence of calcium carbonate, however,
alters these reactions. First, AFt formation is accelerated in the
presence of calcium carbonate [24]. Second, the conversion of AFt
15% 20%
and calcium carbonate to form calciumcarboaluminate.
The formation of calciumcarboaluminate occurs as some of the
sulfates are replaced by carbonate ions during C3A hydration. As a
result, the limestone or CKD can be used for partial substitution of
the gypsum to control the early hydration of C3A.
The quartz (contained in CKD) is inert. The partial replacement
of OPC with CKD may have an impact on cement properties due to
the presence of unreactive raw materials within CKD. Quartz has
physical effects on CKD-PC blends due to nucleation and filler
effects.
The slow decrease of compressive strength with increasing
replacements; may be due to agglomeration of nanostructured
particles around cement grains which lead to retard cement hydra-
tion. Also, it may be due to the defects generated in dispersion of
nano particles that causes weak zones.
4.5. Capillary water absorption (sorptivity)
The effect of nanostructured (S.C – BFS – CKD) on the capillary
water absorption of cement mortar as a function of the replace-
ment ratio is shown in Fig. 9. As seen, the water absorption coeffi-

a b
Cement paste
Cement paste
CH crystal
Sand

Sand

c d

(a): Plain (b): Mortar – 15% S.C (c): Mortar – 15% BFS (d): Mortar – 10% CKD

Fig. 10. SEM micrographs for plain and nanostructured modified mortar.
 K. Al-Jabri, H. Shoukry / Construction and Building Materials 73 (2014) 636–644 643

cient decreases with increasing the amount of nanostructured
materials. A decrease of about 28%, 39% and 44% was observed at
20% replacements of nanostructured S.C, BFS and CKD respectively,
this is attributed to the improvement of microstructure. Due to its
ultra fine size, nano particles fill the voids between cement grains
and in the interface between aggregate and cement paste; this
resulted in a compact structure and led to the reduction of water
mobility inside 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. Densifi-
cation of cement matrix results in the immobilization of water
inside the bulk paste [25]. The durability of cement and concrete
structures is closely related to the water absorption so the reduc-
tion of water absorption will extend life time of cement based
products and hence durability [26].
4.6. Microstructure characteristics
Fig. 10 Shows the SEM micrographs of both plain and nano-
structured blended mortar at 28 days of curing. SEM analysis was
performed on the mixes with promising mechanical performance.
The microstructure of the plain mortar displayed a micro gap
between the cement paste and aggregate which is due to the col-
lection of CH crystals in the interfacial transition zone. This in turn
result in a weak bonding and reduces the mechanical strength of
cement mortar.
Replacement of Portland cement by ultrafine nanostructured
particles was found to influence hydration behavior and led to dif-
ferences in the microstructure of the hardened mortars. The micro-
structure of the hardened cement mortar containing
nanostructured S.C, BFS and CKD appeared quite dense and com-
pact with less voids. Furthermore, large crystals of CH are disap-
peared. It may be assumed that, the strengthening effect of nano
particles would be further enhanced in mortar because the nano
particles improve not only the cement paste but also the interfacial
transition zone between cement paste and aggregate, which result
in a good bonding and this will enhance the mechanical perfor-
mance of nanostructured blended cement mortar [27].
The nano particles have considerably modified the interfacial
transition zone and increased the bond between the cement paste
and aggregate due to the physical packing effect. Also the pozzola-
nic activity of the nanostructured waste minerals resulted in the
creation of additional calcium silicate hydrate which gets depos-
ited in interfacial transition zone.
4.7. X-ray diffraction
Fig. 11 shows the XRD patterns obtained for the plain and nano-
structured blended mortar after 28 days of curing. Obviously, the
main compounds detected from XRD diffractograms are calcium sil-
icate hydrate (C-S-H), calcium hydroxide (CH) and calcium sulfoalu-
minate/Ettringite (E) along with Quartz (Q). The intensities of the
peaks representing the hydration products (CSH and CH) in the
nano CKD blended mortar are higher than those of plain mortar;
this indicates that the nano CKD particles resulted in the accelera-
tion of hydration process and produced more hydrates at the same
time of hydration. Due to the high active silica content of both (S.C
and BFS); these materials resulted in the consumption of CH phase
by pozzolanic reaction. The reduction of CH by reaction with the
pozzolana can result in greatly enhanced durability and strength.

Mortar - 10% Nano CKD CSH

5. Conclusion

CH Q CH
Q The main conclusions that were drawn from the current study
can be summarized as follow:
CH
E E
 The high energy planetary ball milling is a beneficial tool for
particle size reduction of spent catalyst, copper slag and cement
5 10 15 20 25 30 35 40 45 50 kiln dust particles from micro to nano level.
Mortar - 15% Nano BFS
 The ball milling technique leads to a considerable modification
in particles morphologies.
 The replacement of cement by the nanostructured S.C, BFS and
CKD can be considered as helpful in enhancing the compressive
strength of cement mortar and reducing the capillary water
absorption.
 Replacement of cement with 20% nanostructured CKD led to a
Intensity

5 10 15

Mortar -15% Nano S.C

20 25 30 35 40 45 50
decrease of capillary water absorption by about 44% at 28 days
of hydration.
 The nanostructured S.C, BFS and CKD modify the interfacial
transition zone in blended cement mortar and provide a denser,
compact and homogeneous structure.

Acknowledgements
5 10 15 20 25 30 35 40 45 50

Plain mortar

The research team gratefully acknowledges the financial sup-

port provided by Oman Refineries and Petroleum Industries Com-
pany (Orpic) under Sultan Qaboos University Grant No. CR/ENG/
CIVL/09/01. Also, we appreciate the technical support provided
by the staff at SQU.

5 10 15 20 25 30 35 40 45 50 References
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