Materials and Structures (2010) 43:665673

DOI 10.1617/s11527-009-9519-6

ORIGINAL ARTICLE

Combined effect of chemical nature and fineness of mineral

powders on Portland cement hydration
E. H. Kadri S. Aggoun G. De Schutter
K. Ezziane

Received: 20 February 2009 / Accepted: 19 June 2009 / Published online: 1 July 2009
RILEM 2009

Abstract This paper focuses on the influence of the

chemical nature and the fineness of the fillers on the
hydration process and on the compressive strength
development. Four different types of fillers are considered in combination with Portland cement: quartzite
filler, alumina filler, limestone filler, and silica fume.
The study deals with blended mortars having a 0.45
water to powder (cement and filler) ratio with a 10%
substitution of cement by filler. Quartzite fillers do not
seem to accelerate the hydration process in a significant
way. No positive effect is noticed on the strength
development either. The presence of a fine inert
alumina powder increases the rate of early hydration
of Portland cement. The greater the fineness, the faster
the rate of hydration heat development. This reactivity
leads to an increase in the compressive strength at early
age for mortar containing the finest alumina powders.
In case of coarse alumina powder, no acceleration
effect is obtained. Finely ground limestone (calcite)

fillers promote heterogeneous nucleation of hydrates

which significantly accelerates hydration. At early age,
this also results in an increased mortar compressive
strength in comparison with the control mortar. From
the obtained results, it is clear that both chemical
natures as well as fineness are important with regard to
the accelerating effect of the hydration process. With
increasing fineness, the accelerating effect increases.
For powders with comparable fineness, it is clear that
limestone powder has a more significant accelerating
effect than silica fume and alumina filler. Quartzite
filler seems to have no significant effect.
Keywords Hydration  Calcite  Alumina 
Quartzite filler  Silica fume  Fineness

1 Introduction
E. H. Kadri (&)  S. Aggoun
Laboratory L2MGC, Universite Cergy Pontoise, Rue
Eragny Neuville sur Oise, 95031 Cergy Pontoise, France
e-mail: el-hadj.kadri@u-cergy.fr
G. De Schutter
Magnel Laboratory for Concrete Research, Department
of Structural Engineering, Ghent University, 9052 Ghent,
Belgium
K. Ezziane
Laboratory of Materials and Environment,
Chlef University, Chlef, Algeria

The incorporation of cementitious materials or mineral powders as an addition to cement or to partially

replace cement is now common use in modern
concrete technology. These fillers can help to achieve
specific concrete properties like self-compactability
[1] to improve mechanical properties and durability,
or just to reduce the production cost. Fine powder
particles may improve workability, and may improve
microstructure and mechanical properties by densely
packing at optimum dosage [2, 3]. The fines may also

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Materials and Structures (2010) 43:665673

have some hydraulic or pozzolanic activity, or may

modify the hydration reaction of cement [3, 4].
This paper focuses on the influence of the chemical
nature and the fineness of the fillers on the hydration
process and on the compressive strength development.
Four different types of fillers are considered in
combination with Portland cement: quartzite filler,
alumina filler, limestone filler, and silica fume. The
study deals with blended mortars having a 0.45 water
to powder (cement and filler) ratio with a 10%
substitution of cement by filler.

2 Experimental programme
2.1 Materials
In this study, several mineral additions of different
mineralogical nature are studied. All mixes are based
on Ordinary Portland Cement (OPC) CEM I 52.5. The

first mineral filler mainly contains crystallized silica,

with a silica content of 98.5%. Three different
finenesses are considered, with a particle size of
2.6 lm (F1), 5.5 lm (F2) and 11 lm (F3). The second
filler mainly contains alumina, with a percentage
higher than 95%. The average particle size of this
alumina filler is 63 lm (A1), 1.5 lm (A2) and 0.8 lm
(A3). The aluminium filler considered in this study has
a crystalline structure. It is Aluminium oxide (Al2O3),
also called corundum or alpha-aluminium oxide. This
has been confirmed by XRD analysis. The third filler
type is silica fume (SF), containing 95% amorphous
silica with an average particle size of 0.15 lm. Finally,
a high purity ([99.9%) calcium carbonate limestone
filler (CC) is considered, artificially obtained through
a reaction between lime and carbon dioxide. This
limestone filler contains ultrafine particles with an
average size of 0.07 lm.
The plain cement for the blended mortars is a French
ordinary Portland cement. Composition and properties
of OPC and mineral filler materials are given in Table 1.

Table 1 Composition and properties of OPC and mineral fillers

SiO2 (%)
Al2O3 (%)

OPC

F1

F2

F3

20.2

98.5

98.5

98.5

0.8

0.8

94.8

4.29

0.85

A1

A2

A3

CC

SF

95

94.8

94.8

0.3

Fe2O3 (%)

2.35

0.1

0.08

0.04

0.6

TiO2 (%)

0.25

0.04

0.04

0.03

MnO

0.02

0.05

0.03

0.03

1.4

2.2

CaO (%)

63.6

MgO (%)

3.88

SO3 (%)

2.8

1.5

K2O (%)

0.69

0.6

0.6

0.55

Na2O (%)

0.14

0.04

0.04

0.03

P2O5 (%)

0.31

L.O.I.

1.1

2.7

Si (%)
CaCO3

99.9

3.2

11

63

Average particle size (lm)

18.5

Surface specific BET (m2/g)

Specific gravity (g/cm3)

3.13

Bogue composition
C3S

66.9

C2S

10.7

C3A

8.4

C4AF

7.60
2

* Blaine value 0.36 m /g

2.6
22
2.65

5.5
10.3
2.65

6.9

9.7

2.65

3.95

1.5

0.8

12.2

13.8

3.95

3.95

0.07
15.2
2.83

0.15
18.2
2.24

Materials and Structures (2010) 43:665673

667

2.2 Mix proportions

In order to obtain blended mortars, normalized sand
CEN EN 196-1 of siliceous origin with a silica
content of more than 98% is used. In order to get a
homogeneous mixture and avoid a flocculation of the
finest particles, a naphthalene sulphonate superplasticizer (40% solids) is introduced, at a dosage of 0.8%
by mass, relative to the powder (cement ? filler)
content. The series of blended mortars are prepared
with a 10% cement replacement by the mineral fillers.
The blended mortar compositions are shown in
Table 2. All mixes have a 0.45 water powder ratio.
The mixing process is as follows. The dry silica
sand and the powder are mixed without water for
1 min. Mixing water is added with one-third of the
superplasticizer, and the mixing is continued for
2.5 min. The remaining superplasticizer is added,
followed by 1 min additional mixing time.

The measurements are made over 6 days, since the

heat increase is observed to be very low at later times.
Using a semi-adiabatic calorimeter the variation of
the temperature of the mortar with time has been
measured immediately after mixing. For each mixture, the heat of hydration is determined based on the
accumulated heat in the calorimeter and the heat
dispersed in the environment. At time t, the hydration
heat Q by gram of powder (cement ? filler) is
obtained by the following formula:
C
1
Q DH
mc
mc

Zt
a DH dt
0

where C is the total thermal capacity of the mortarfilled calorimeter (J/C), mc is the cement or powder
mass (g), Dh is the mortar temperature rise (C),
and a is the total calorimeter thermal loss coefficient
(J/h C).
2.4 Compressive strength

2.3 Hydration tests

The heat of hydration is determined using a semiadiabatic calorimeter (Fig. 1), according to the NF
EN 196-9 standard. The method is based on the
Langavant Calorimeter. This semi-adiabatic method
consists of quantifying the heat generated during
cement hydration using a thermally insulated bottle.
Since the exterior conditions are very influential, the
test is carried out in a climatized room at 20 2C.

The blended mortars are also mechanically tested in

compression. The obtained strength results are the
average of individual test results obtained on three
mortar specimens 40 mm 9 40 mm 9 160 mm. The
variation coefficient is lower than 5%. The specimens
were stored in their moulds for 24 h at a temperature
of 20 1C and at a relative humidity of 55 5%.
After demoulding, they were cured in lime-saturated
water 20 1C until testing.

Table 2 Mortar mix design

Materials (kg/m3)

OPC

Powder

500

Sand

1,350

Water

225

Superplastizer (water ? solids)

Cement

500

F1
F2
F3
A1
A2
A3
CC
SF

F1

F2

F3

A1

A2

A3

CC

SF

450

450

450

450

450

450

450

450

50
50
50
50
50
50
50
50

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Materials and Structures (2010) 43:665673

300

PC

Software

OPC
F1
F2
F3

Calorimeter

Heat of hydration (J/g)

250
200
150
100
50
0

Fig. 1 Experimental setup for hydration test

10

12

14

16

18

Time ( h )

3 Experimental results and discussion

Fig. 2 Evolution of the heat of hydration for the quartzite filler

mortars

3.1 Quartzite filler

Figure 2 shows the heat release curves during the first
20 h for the three blended quartzite filler mortars and
the control OPC mortar. A slight acceleration of the
hydration process can be noticed, although the effect
is not significant. This is in agreement with earlier
results obtained by Poppe [5] and Poppe et al. [6],
indicating that quartzite filler does not seem to
influence the induction period and is not changing
the acceleration period of the hydration process.
Even if the influence of quartzite filler on the
hydration process is not significant, the slight acceleration seems to depend on the fineness, as can be
seen in Fig. 2.
The evolution of the compressive strength between
1 and 120 days is shown in Fig. 3. Using a finer
quartzite filler, a higher compressive strength is
obtained at all ages. However, the strength results
remain below the values obtained for the reference
OPC mortar, except for the finest quartzite filler (F1)
at high age.
3.2 Alumina filler
Figure 4 shows the evolution of the heat of hydration
for the three blended mortars containing alumina filler
and the OPC control mortar over a 20 h period.
After 12 h, the heat released by the (A3) and (A2)
mortars is respectively 80% and 55% higher than the

Compressive strength (MPa)

70

OPC

F3

F2

F1

60
50
40
30
20
10
0
1

3
7
Time ( days )

28

120

Fig. 3 Strength development for the quartzite filler mortars

heat released by the control mortar. The control

mortar releases 25% more heat than the (A1) mortar.
If the heat of hydration would be expressed in Joule
per gram of cement (and not per gram of powder), the
reference curve and the curve for (A1) would
coincide, indicating that the coarser alumina filler
(A1) is not influencing the hydration process of OPC.
It is repeated here that the average particle size of (A1)
is 63 lm, which is significantly higher than the
average particle size of (A2) 1.5 lm and (A3) 0.8 lm.
The evolution of the accumulated heat as a
function of time up to 6 days is shown in Fig. 5. It

Materials and Structures (2010) 43:665673

669
70

350

250

Compressive strength (MPa)

300

Heat of hydration (J/g)

OPC

OPC
A1
A2
A3

200
150
100
50

A2

A1

28

50
40
30
20
10
0
1

120

Time ( days )

0
0

10

12

14

16

18

20

Time ( h )
Fig. 4 Evolution of heat of hydration for the alumina filler
mortars

400
350

Heat of hydration (J/g)

A3

60

300
250
200

OPC
A1
A2
A3

150
100
50
0
0

24

48

72

96

120

144

Fig. 6 Strength development for the alumina filler mortars

However, the fine alumina particles may promote sites

of heterogeneous nucleation to precipitate more or
less crystallized hydrates. This hypothesis needs
further investigation.
In order to know whether the accelerated early
hydration by fine alumina particles may have repercussions on the compressive strength of mortars, the
evolution of strength up to 4 months, as seen in Fig. 6,
is studied. The results confirm the heat evolution data.
After 1 day, the compressive strength of the reference
mortar is lower than that of the mortar with the finest
(A3) alumina. However, after 2 days the strength of
the OPC control mortar becomes higher than that of
all blended alumina compositions.
3.3 Limestone filler

Time ( h )

Fig. 5 Development of total heat of hydration for the alumina

filler mortars

appears that the heat released by the reference mortar

becomes progressively higher than that of the blended
alumina mortars after 48 h.
The addition of fine alumina particles appears to
accelerate the hydration of cement phases within the
first hours, except in case of the coarser (A1). Alumina
is a particularly stable oxide in alkaline solutions since
the solubility product given in textbooks is about
10-31 at pH [ 13. Consequently, the alumina filler is
not chemically active within the hydration reactions.

As can be clearly seen in Fig. 7, limestone filler (CC) is

accelerating the hydration process in a very significant
way. This accelerating effect has also been reported by
other researchers [58]. Concerning the shortening of
the induction period and the acceleration of the
hydration reactions due to the addition of finely
ground limestone filler, different theories have been
formulated [9]. The accelerating effect can mainly be
ascribed to the increased nucleation possibilities of the
finely ground limestone filler, leading to a faster
formation of hydration products of OPC hydration.
This is a pure catalyst effect, without the limestone
filler being chemically active. Even after a long
hydration period, the limestone filler remains in the

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Materials and Structures (2010) 43:665673

the acceleration process has disappeared, and the

strength results remain below those of the reference.

Heat of hydration (J/g)

350
OPC

300

3.4 Silica fume

CC

250

Silica fume is accelerating the hydration process, as

shown in Fig. 9. This effect is also well-known, and
has been reported many times, e.g. [15]. However, it
is to be mentioned that the accelerating effect of
silica fume depends on the water powder ratio and on
the level of cement replacement by silica fume. This
is discussed in more detail in Kadri et al. [3].

200
150
100
50

3.5 Chemical nature versus fineness

0
0

8 10 12
Time ( h )

14 16 18

Fig. 7 Evolution of heat of hydration for the limestone filler

mortar

microstructure in its original form [7, 10], although it

is to be mentioned that a minor part of the limestone
filler could be involved in the formation of carboaluminates [1114].
The accelerating effect of the limestone filler can
also be noticed from the strength development results,
as given in Fig. 8. At early age, the strength of the
limestone filler mortar is higher than the reference
OPC mortar. However, at later ages the advantage of

Besides the chemical nature, also the fineness of the

mineral powders is of great importance when studying the influence on the hydration process. The results
given in previous sections are obtained for different
powders, having different fineness. In order to
eliminate as far as possible the effect of fineness
when comparing the different mineral fillers, the
results for the mortars containing (F1), (A3), (CC)
and (SF) can be summarized as shown in Fig. 10. The
selected powders all have more or less comparable
fineness, as shown by the BET values given in
Table 1.

350

OPC
300

SF

OPC

60

Heat of hydration (J/g)

Compressive strength (MPa)

70

CC

50
40
30

250
200

150
100

20
50

10
0

28

120

10

12

14

16

18

Time ( h )

Time (h)
Fig. 8 Strength development for the limestone filler mortar

Fig. 9 Evolution of heat of hydration for the silica fume

mortar

Materials and Structures (2010) 43:665673

671

350

OPC
SF
F1
CC
A3

Heat of hydration (J/g)

300
250
200
150
100
50
0
0

10

12

14

16

18

Time ( h )
Fig. 10 Heat of hydration with respect to time, for different
blended mortars containing mineral powders of different
chemical nature but with comparable fineness

The accelerating effect of the initial hydration due

to the fine substituted particles progressively decreases
in the following order: limestone filler (CC), alumina
filler (A3), silica fume (SF) and quartzite filler (F1). At
an age of 8 h, the amount of heat released by the
blended calcite (CC) mortar is 10 times higher than the
corresponding amount in the reference and three times
for the silica fume (SF) mortar.

Figure 11 represents the incremental heat evolution curves of the different blended mortars relative
to the OPC control mortar. In the beginning, the four
blended mortars show a positive incremental heat of
hydration, and thus a higher cumulated heat release in
comparison with the OPC control mortar. From 20 h
on for the calcite (CC) mortar and from 72 h on for
the alumina (A3) mortar, the incremental heat
becomes negative, pointing at a lower cumulated
heat development in comparison with the reference
mortar. In the long run, the calcite (CC) and alumina
(A3) mortars release less heat compared to the
control mortar. On the other hand, the two mortars
containing quartzite (F1) and especially silica fume
(SF) produce more heat than the control mortar,
although in case of quartzite (F1) the difference is
rather low.
The evolution of the compressive strength over a
4 month period is shown in Fig. 12. The values
obtained confirm the results of the calorimetric study.
After 1 day, the compressive strength of blended
mortars, especially calcite (CC) and alumina (A3)
mortars is higher than the control mortar. Then after
2 days, the resistance of these mortars decreases
compared with the reference mortar, while after
3 days, the strength increase of the quartzite mortar
develops faster and after 7 days their strength
becomes higher than the reference mortar. This is
in agreement with Duval et al. [2].

Incre mental heat of hydration (J/g)

250

SF
F1
CC
A3

200

150

100

50

24

48

72

-50

Time ( h )
Fig. 11 Incremental heat of hydration for the different
blended mortars, relative to the OPC control mortar

Fig. 12 Strength development for different blended mortars

containing mineral powders of different chemical nature but
with comparable fineness

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4 Discussion
At very early stages, sub-micron particles of inert or
active fillers act as heterogeneous nucleation sites
onto which first hydrates can precipitate. It appears
that the initial hydration rate depends on the fineness
of the filler particles as well as on the chemical
nature. The effect of the enhancement of hydration is
a decrease of the dormant period and an increase of
the strength of blended mortars up to 24 h.
The hydration rate of inert alumina particles is
higher as the fineness increases. Similar results have
been reported by Guteridge et al. [16] who observed
that at an early age, for a cement paste with a 20%
fine rutile powder, the degree of hydration is higher
than for the corresponding Portland cement. Moreover, Detwiler et al. [17] showed that 10% cement
replacement by carbon black powder gives comparable strength as for the plain cement concretes up to
age 7 days. On the contrary, Beedle et al. [4] found
that fine powders, such as titanium dioxide and
graphite, have no substantial effect on the acceleration of hydration by heterogeneous nucleation.
In the same way, submicron particles of limestone
filler develop a faster rate of hydration and serve as
precipitation nuclei of hydration products. Moreover,
the dissolution of active calcite is increased by the
formation of few soluble salts of ettringite and
hydrosilicates, as reported by Khatib et al. [18]. The
early hydration gives an alumino-hydrosilicate gel
doped by calcium and carbonate ions liberated from
the calcite. Hexagonal plates of calcium monocarboaluminate appear only after a few days and have
only a minor contribution to the mechanical strength
development [19]. For a given water powder ratio, the
limestone filler cement contains more portlandite
than the corresponding Portland cement as a result of
a higher rate of tricalcium silicate hydration [20].
For the silica fume, the heterogeneous nucleation
takes place in the initial stage but it is immediately
followed by the early dissolution of amorphous silica.
The dormant period is reduced and the silica fume (SF)
particles actively contribute to the cement hydration
process during the first hours [21]. The pozzolanic
reaction consumes calcium hydroxide and in the early
stages, the decrease of free calcium ions stimulates
the dissolution of cement particles, as reported by
Yajun et al. [22]. Later on, the cement grains are
gradually covered by the silica fume (SF) particles and

Materials and Structures (2010) 43:665673

hydrosilicate gel forming a diffusion barrier which

hinders the contact with the interstitial solution and
slows down the hydration rate [23].
The particles of finely ground quartzite filler (F1)
show no clear accelerating effect. Possibly, some
nucleation effects could occur, however not very
significant. The intensive grinding can probably
contribute to the disorder of the crystal lattice of
quartz which slightly dissolutes in the alkaline
solution and also develops some reaction.
From the obtained results, it is clear that both
chemical nature as well as fineness are important with
regard to the accelerating effect of the hydration
process. With increasing fineness, the accelerating
effect increases. For powders with comparable fineness, it is clear that limestone powder has a more
significant accelerating effect than silica fume and
alumina filler. Quartzite filler seems to have no
significant effect.

5 Conclusions
This paper examines the effect of fine fillers of
different chemical nature and fineness on the initial
hydration of Portland cement and the corresponding
strength development, by experimentally studying
mortars with 10% cement replacement. The following conclusions can be drawn:

Quartzite fillers do not seem to accelerate the

hydration process in a significant way. No positive
effect is noticed on the strength development
either.
The presence of a fine inert alumina powder
increases the rate of early hydration of Portland
cement. The enhancement most probably results
from the multiplication of nuclei sites on which
hydrates could grow. The greater the fineness, the
faster the rate of hydration heat development.
This reactivity leads to an increase in the
compressive strength at early age for mortar
containing the finest alumina powders. In case of
coarse alumina powder, no acceleration effect is
obtained.
Finely ground limestone (calcite) fillers promote
heterogeneous nucleation of hydrates which significantly accelerates hydration. At early age, this
also results in an increased mortar compressive

Materials and Structures (2010) 43:665673

strength in comparison with the control mortar.

At later age, no strength increase is noticed.
From the obtained results, it is clear that both
chemical nature as well as fineness are important
with regard to the accelerating effect of the
hydration process. With increasing fineness, the
accelerating effect increases. For powders with
comparable fineness, it is clear that limestone
powder has a more significant accelerating effect
than silica fume and alumina filler. Quartzite filler
seems to have no significant effect.

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