Construction

and Building

Construction and Building Materials 21 (2007) 15341541

MATERIALS
www.elsevier.com/locate/conbuildmat

Eect of y ash neness on microstructure of blended cement paste

Prinya Chindaprasirt a, Chai Jaturapitakkul b, Theerawat Sinsiri c,*

a
Department of Civil Engineering, Faculty of Engineering, Khon Kaen University, Khon Kaen 4002, Thailand
b
Department of Civil Engineering, Faculty of Engineering, King Mongkuts University of Technology Thonburi, Bangkok 10140, Thailand
c
School of Civil Engineering, Institute of Engineering, Suranaree University of Technologi, Nakorn Ratchasima 30000, Thailand

Received 1 May 2005; received in revised form 20 November 2005; accepted 5 December 2005
Available online 6 October 2006

Abstract

This research demonstrates the eect of y ash neness on pore size and microstructure of hardened blended cement pastes. Two sizes
of y ash, original y ash and classied y ash were used to replace Portland cement type I paste. Test results indicated that the pore sizes
of hardened blended cement paste were signicantly aected by the rate of replacement and the neness of y ash. The replacement of
cement by original y ash decreased the pore sizes of blended cement paste and the incorporation of classied y ash resulted in a further
decrease in the pore sizes of blended cement paste. The X-ray diraction (XRD) results showed that the blended cement paste with clas-
sied y ash was more eective at reducing the intensity of Ca(OH)2 than that with the original y ash. The scanning electron microscope
(SEM) results revealed that the hardened blended cement paste containing ner y ash produced a denser structure than the one con-
taining coarser y ash.
2006 Elsevier Ltd. All rights reserved.

Keywords: Fineness; Fly ash; Pore size; Microstructure; Blended cement paste

1. Introduction eective means for improving the properties of concrete.

Concrete is a composite material which has a complex
microstructure and exhibits a wide range of scale lengths
from nanometers to millimeters [1]. Aggregates are the big-
gest materials in concrete and have particle size in millime-
ters. At the micrometer scale, the cement paste is a
composite of unhydrated residues of cement grains and
hydration products (CSH, Ca(OH)2, and capillary pore).
Hydrated cement paste contains large capillary pores with
diameters between 5010,000 nm, medium capillary pores
with diameters of 1050 nm and gel pores with diameter
of less than 10 nm [2]. It is well known that the service life
of a concrete structure is strongly dependent on its material
transport properties, which are controlled by the micro-
structure characteristics of concrete. It is generally recog-
nized that the incorporation of pozzolanic materials as a
partial replacement for Portland cement in concrete is an
*
Corresponding author. Tel.: +66 4422 4420 1; fax: +66 4422 4220.
E-mail address: sinsiri@sut.ac.th (T. Sinsiri).
Pozzolanic materials react with calcium hydroxide during
hydration reaction and forms calcium silicate hydrate. This
can reduce the size of the pores of crystalline hydration
products, make the microstructure of concrete more uni-
form and improve the impermeability and durability of
concrete. These improvements can lead to an increase in
the service life of a concrete structure.
Fly ash is a waste product from the combustion of pul-
verized coal in electricity power plants. It is estimated that
more than 3.5 million tons of y ash has been produced
annually in Thailand since 2001, however, only half has
been utilized. The utilization of y ash is still limited due
to lack of understanding of the characteristics of y ash
itself and the properties of concrete containing y ash.
Many researchers have already reported on the inuence
of y ash on the properties of concrete such as compressive
strength, sulfate resistance, durability and so on. However,
few researches were found, which deal with the neness of
y ash on pore structure and microstructure of blended
cement paste. An understanding of the inuence of neness

0950-0618/$ - see front matter 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2005.12.024
 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541 1535

of y ash on pore structure and microstructure of cement 100

paste could lead to an increase in the use of y ash in con- 90
crete. In this paper, pore structure and microstructure of y Portland Cement Type I
80
ash cement pastes with dierent y ash nenesses are Original Fly Ash (OFA)

Cumulative Passing (%)

70 Classified Fly Ash (CFA)
investigated.
60
2. Experimental program 50

40
2.1. Material properties
30
Fly ash from Mae Moh power plant in the north of 20
Thailand, Portland cement type I (PC) and tap water were 10
used in this study. The chemical composition of Portland
0
cement type I (PC), original and classied y ashes (OFA 0.1 1 10 100 1000
and CFA) are given in Table 1. The total amount of the Particle Size (micron)
major components SiO2, Al2O3, and Fe2O3 in OFA and
Fig. 1. Particle size distribution of PC type I and y ashes.
CFA are 81.54% and 79.44%, respectively. They can be
classied as class F y ash in accordance with ASTM C
618. It should be noted that there is no signicant dierence the ne y ash (about 8590%) was higher than that of
in the chemical composition of OFA and CFA. Two y ash the coarser y ash (about 7075%). This result agreed with
sizes of OFA with median particle size of 19.1 lm and CFA Berry et al. [4], who showed that the glassy phase was
with median particle size of 6.4 lm were used to replace found to increase in the ne y ash as compared to the ori-
Portland cement. Physical properties of PC, OFA, and ginal y ash.
CFA are shown in Table 2 and particle size distributions
are shown in Fig. 1. Particle shapes of PC, OFA, and 2.2. Mix proportion
CFA by SEM are shown in Fig. 2.
The X-ray diraction patterns (XRD) of OFA and CFA Fly ashes were used to replace Portland cement at the
are shown in Fig. 3. There is little dierence between the rate of 0, 20, and 40% by weight of binder. The water to
XRD patterns of OFA and CFA. It is known that y ashes binder ratio (W/B) was constantly 0.35 throughout the
consists of a glassy matrix with crystalline phases like investigation. The pastes were mixed in a mechanical mixer
quartz, mullite, hematite, anhydrite, lime, and so on. In and were cast in 50 mm cube molds and compacted by
the Mae Moh y ash, quartz is commonly found as the tamping rod, and were sealed by plastic to prevent water
crystalline compound in OFA and CFA. In addition, traces loss. 24 h after casting, specimen were removed from the
of hematite and mullite are also noticeable. Chindaprasirt molds and cured in saturated lime water.
et al. [3] studied the glassy phase content of the Mae
Moh y ash and found that the glassy phase content of 2.3. Mercury intrusion porosimetry

Table 1 Measurement on pore size distribution of paste was car-

Chemical composition of PC type I and y ashes ried out using mercury intrusion porosimeter (MIP) with a
Chemical Portland cement Original Classied pressure range from 0 to 33,000 psi (228 MPa), capable of
composition (%) type I y ash y ash measuring pore size diameter down to 5.7 nm. By carefully
SiO2 20.90 45.69 44.72 breaking the hardened blended cement paste cubes with a
Al2O3 4.76 24.59 23.69 chisel, the representative samples of 36 mm pieces weigh-
Fe2O3 3.41 11.26 11.03
ing between 1 and 1.5 g were taken from the middle of the
CaO 65.41 12.15 12.67
MgO 1.25 2.87 2.63 specimen. The samples were frozen at 195 C by immer-
SO3 2.71 1.57 1.28 sion in liquid nitrogen for 5 min and evacuated at a pres-
Na2O 0.24 0.07 0.07 sure of 0.5 Pa at 40 C for 48 h [57]. Mercury
K2O 0.35 2.66 2.87 porosimetry is expressed by the Washburn equation [8].
LOI 0.96 1.23 1.42
A constant contact angle of 140 and a constant surface

Table 2
Physical properties of PC type I and y ashes
Sample Median particle size (lm) Retained on a sieve No. 325 (%) Specic gravity Blaine neness (m2/kg)
Portland cement type I 14.1 4.8 3.15 360
Original y ash 19.1 31.0 2.33 300
Classied y ash 6.4 0 2.54 510
1536 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541

Fig. 2. SEM of PC type I and y ashes (a) PC type I (b) Original y and (c) Classied y ash.

90 days. At specied ages of 28, 60 and 90 days, samples

from the crushed paste cubes and freeze-dried samples were
tested for degrees of hydration, as prepared in the MIP
examination. The dried sample pastes were ground using
a ball mill and sieved through a sieve No. 100 (opening
150 lm). The powder sample weighing about 1 g was used
CFA to determine the amount of Ca(OH)2 in the XRD analysis
(Bruker D5005).

OFA 2.5. Scanning electron microscope (SEM)

Paste cubes at the required ages of 7, 28 and 90 days

were broken from the center into small fragments. Hydra-
5 10 20 30 40 50 60 70 tion of the paste was stopped by freezing and drying, as
2-Theta prepared in the MIP examination. The fracture surface
Fig. 3. X-ray diraction patterns of original and classied y ashes.
was observed by using SEM (JOEL JSM-6400). All sam-
ples were also coated with gold before using SEM analysis.

tension of mercury of 480 dynes/cm were used for pore size
calculation by,
D 1=P 4c cos u
where D is the pore diameter (lm), P is the applied pressure
(MPa), c is the surface tension (dynes/cm), and u is the
contact angle (degree).
2.4. X-ray diraction (XRD)
The hydration of cement pastes containing y ashes,
with an increased intensity of Ca(OH)2, were investigated
by XRD analysis. All samples were cured for 28, 60 and
3. Results and discussion
3.1. Eect of y ash neness on pore size distribution of
1
blended cement paste
Relationships between pore diameter and incremental
pore volumes of OFA paste at 28 and 90 days are shown
in Figs. 4 and 5. Figs. 6 and 7 show the relationships between
pore diameter and incremental pore volumes of CFA paste
at 28 and 90 days. At 28 days, the rst peak of capillary
pores of CFA20 and CFA40 pastes were located at
50.4 nm with the incremental pore volume of 0.0266 ml/g
and 44.7 nm with incremental pore volume of 0.0195 ml/g,
 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541 1537

0.035 0.035

Incremental Pore Volume (mL/g)

Incremental Pore Volume (mL/g)

(54.5 nm, 0.026 m L/g) W/B = 0.35 W/B = 0.35

0.03 28 Days Cured 0.03 90 Day s Cured
(15.3 nm, 0.0154 m L/g )
(55.2 nm, 0.022 m L/g)
PC ( 25. 8 nm, 0.0215 m L/g ) PC
0.025 (29.1 nm,0.018 mL/g) 0.025
OFA20 CFA20
( 29. 0 nm, 0.0204 m L/g ) CFA40
OFA40
0.02 0.02
(55.1 nm, 0.019 m L/g) ( 15. 3 nm, 0.0114 m L/g )

0.015 0.015 ( 36. 0 nm, 0.01 mL/g : OPC )

0.01 0.01

0.005 0.005

0 0
1 10 100 1000 10000 100000 1 10 100 1000 10000 100000
Pore Diameter (nm) Pore Diameter (nm)

Fig. 4. Relationship between pore diameter and incremental pore volume Fig. 7. Relationship between pore diameter and incremental pore volume
of OFA paste at 28 days. of CFA paste at 90 days.

respectively (Fig. 6). These values were lower than those of

OFA20 and OFA40 pastes which were 54.5 nm at 0.026 ml/
0.035 g at the rst peak and 55.1 nm at 0.019 ml/g at the second
peak, respectively, with the same replacement (Fig. 4). These
Incremental Pore Volume (mL/g)

W/B = 0.35
0.03 90 Days Cured results suggest that classied y ash is more eective for
( 15. 3 nm, 0.022 m L/g ) decreasing capillary pores than original y ash.
0.025 PC
OFA20 In Fig. 7, there are three visible peaks of incremental
( 35. 9 nm, 0.018 m L/g )
0.02
OFA40 pore volume; two peaks in the range of capillary pore
( 15. 3 nm, 0.01 mL/g ) and one in the range of gel pore. The peak of pore diameter
0.015 (36.0 nm, 0.01 mL/g : PC) of CFA20 paste decreased from 50.4 nm with 0.0266 mL/g
(at 28 days, as shown in Fig. 6) to 29.00 nm with
0.01 0.0204 mL/g for the rst peak and 15.3 nm with
( 36. 0 nm, 0.009 m L/g : OFA20 )
0.0114 mL/g for the second peak at 90 days. The peaks
0.005
( 15.3 nm, 0.006 mL/g ) of pore diameter of CFA20 and CFA40 pastes were smaller
0 than those of OFA20 and OFA40 pastes. These results sug-
1 10 100 1000 10000 100000 gest that the higher the neness of y ash, the more eec-
Pore Diameter (nm) tive for reducing the pore diameter of the paste. The
Fig. 5. Relationship between pore diameter and incremental pore volume results also show that blended cement paste containing
of OFA paste at 90 days. y ash has a smaller pore size than PC paste. The pore size
decreased with an increase in y ash replacement. Similar
results were also reported else where [911].
As demonstrated, the incorporation of classied y ash
0.035 in cement paste resulted in lower pore size compared with
the use of original y ash. This is due to the gradual lling
Incremental Pore Volume (mL/g)

W/C = 0.35
0.03 (50.4 nm, 0.0266 m L/g ) 28 Days Cured of large pores from factors such as hydration reaction,
(55.2 nm, 0.022 m L/g )
nucleation eect, packing eect, and pozzolanic reaction
0.025 PC
CFA20 of y ash particles. The hydration reaction occurs from
CFA40 the chemical constituents in cement and water while the
0.02
(44.7 nm, 0.0195 m L/g ) pozzolanic reaction occurs from the reaction of Ca(OH)2
0.015 with SiO2 and Al2O3 from y ash. The smaller spherical
particle of y ash could be easily dispersed into the blended
0.01 (15.3 nm, 0.0127 m L/g ) cement paste and made the cement paste matrix more
0.005 homogeneous. The packing of the ne, solid and spheri-
cally shaped y ash particles that were not completely
0
10
reacted, lled the voids and allowed denser packing within
1 100 1000 10000 100000
the particle of materials and matrix phase [12,13]. The
Pore Diameter (nm) nucleation eect, when the smaller particles were dispersed
Fig. 6. Relationship between pore diameter and incremental pore volume into blended cement paste, accelerated the reactions and
of CFA paste at 28 days. formed a smaller product of the cementing paste [14,15].
1538 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541

3.2. XRD analysis

20CFA Paste
Fig. 8 shows the XRD patterns of PC, 20OFA and CH CH
20CFA pastes at 28 days while the XRD patterns of PC, CH CH CH
40OFA and 40CFA pastes at the same age are shown in
Fig. 9. It is easily noticed that CH or Ca(OH)2 is one of
the hydration products during the hydration reaction. 20OFA Paste
The intensity peaks of Ca(OH)2 appeared at 2h of 18.07,
28.75, 34.13, 47.12, and 50.85 degree. From the results of
Figs. 8 and 9, the intensity peaks of Ca(OH)2 in the
PC Paste
XRD patterns of the blended cement paste with y ashes
were almost similar to that of PC paste. At early ages (28
days), this result supported the hypothesis that the hydra-
5 10 20 30 40 50 60 70
tion reaction was a dominant phase while the reactivity
of y ash was minimal [1619]. 2-Theta
The XRD patterns of PC, OFA, and CFA pastes at 60 Fig. 10. XRD patterns of PC, 20OFA and 20CFA pastes at 60 days.
and 90 days are shown in Figs. 1013. The results show
that the intensity peaks of Ca(OH)2 in the XRD patterns
decreased when y ashes were incorporated into the
blended cement paste. In particular, the classied y ash 40CFA Paste
was more eective for decreasing the intensity peak of CH CH
Ca(OH)2 than the original one, especially at 90 days. It is CH CH CH

40OFA Paste
CH
20CFA Paste
CH
CH CH
CH
PC Paste

20OFA Paste
5 10 20 30 40 50 60 70
2-Theta

PC Paste Fig. 11. XRD patterns of PC, 40OFA and 40CFA pastes at 60 days.

5 10 20 30 40 50 60 70
2-Theta
20CFA Paste
Fig. 8. XRD patterns of PC, 20OFA and 20CFA pastes at 28 days. CH CH
CH CH CH

20OFA Paste
CH 40CFA Paste

CH CH CH
CH
PC Paste

40OFA Paste
5 10 20 30 40 50 60 70
2-Theta
PC Paste Fig. 12. XRD patterns of PC, 20OFA and 20CFA pastes at 90 days.

5 10 20 30 40 50 60 70
well known that Ca(OH)2 consumption in a blended
cement paste is related to the degree of pozzolanic reaction.
2-Theta
Factors aecting the pozzolanic reactivity are neness and
Fig. 9. XRD patterns of PC, 40OFA and 40CFA pastes at 28 days. the glassy phase content of the y ash. Fly ash with a high
 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541 1539

[21], and Harris et al. [22]. It was also noticeable that

Ca(OH)2 decreased signicantly with the increase in y
40CFA Paste ash content (40% replacement). This phenomenon was con-
CH
CH
CH
CH sidered to be the result of two factors: the large quantity of
CH y ash used to replace cement resulted in an adequate level
of reaction, and high neness of y ash allowed pozzolanic
reaction to react faster.
40OFA Paste

3.3. SEM observations

PC Paste The microstructure morphology of fractured surface

5 10 20 30 40 50 60
2-Theta
Fig. 13. XRD patterns of PC, 40OFA and 40CFA pastes at 90 days.
percentage of glassy phase tends to be more reactive than
those with a less percentage of glassy phase [20]. This indi-
cated that the classied y ash, which had a smaller size
and higher glassy content, had a larger surface area to pro-
vide the silica and alumina compounds for higher pozzola-
nic activity than the original y ash. The compounds
reacted and consumed Ca(OH)2, resulting in a decrease
in Ca(OH)2 content. The ner y ash had a more glassy
content resulting in a higher consumption of Ca(OH)2.
These results conform to Berry et al. [4], Sybertz and Wiens
pastes at 7, 28 and 90 days are shown in Figs. 1417. At
7 days, the microstructures of OFA20 and OFA40 pastes
70
(Figs. 14a and 15a) were porous and had many voids. It
can be seen that the hydration products on the y ash sur-
face hardly proceeded, some of the surfaces of y ash par-
ticles were found to be coated with layers of small amounts
of hydration products. Some of the ettringite needles,
which grow in vacant areas in paste, were occurring. Signif-
icantly, the pozzolanic reaction of y ash in concrete
started after one or more weeks [12,19,21]. In this period,
two mechanisms of hydration and nucleation occupied
simultaneously [2325].
Considering OFA20 and OFA40 pastes at 28 days
(Fig. 14b and Fig. 15b), y ash particles were observed
in three forms: particles with a dissolved surface, smooth
surface, and a covering layer made of hydration product
and pozzolanic reaction. In the rst form, it appeared that

Fig. 14. Fractured surface of OFA20 paste by SEM.

Fig. 15. Fractured surface of OFA40 paste by SEM.

1540 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541
Fig. 16. Fractured surface of CFA20 paste by SEM.
Fig. 17. Fractured surface of CFA40 paste by SEM.
some y ash particles had signs of etching on their sur-
face, indicating precipitation in the pozzolanic reaction
[19,23,25]. The second form showed some y ash particles
were still smooth, suggesting that they were unreacted or
acted as an inert material with the ability to increase the
packing eect and served as a precipitation nucleus for
hydration compounds. In the third form, hydration and
pozzolanic products around the y ash particles were
observed.
At 90 days (Fig. 14c and Fig. 15c), etched y ash parti-
cles and hydrated rims with broken y ash surfaces were
quite common. A lot of y ash particles were substituted
by hydrates, when the y ashes were activated by Ca(OH)2.
The pozzolanic reaction of y ash speeded up at the later
ages and the consumed content of CSH increased. The
surface of y ash particles covered by CSH were caused
by the reaction of y ash and Ca(OH)2 and other hydration
products [23,25,26]. As the process continued, the layer on
the y ash and cement grain thickened. The hydration
products growing from the cement grains and y ash par-
ticles are to be connected, although some particles still
remain unreacted and acted as lling eects [27,28].
For classied y ash pastes, as shown in Figs. 16 and 17,
the results are similar to that obtained from original y ash
pastes. More empty pores were evident in the pastes at 7
and 28 days (Figs. 16 and 17a,b). Another nding was that
a lot of y ash particles still had smooth surfaces at these
ages. As previously explained, they were still unreacted at
the early age and acted as a ller material, serving as a pre-
cipitation nucleus for Ca(OH)2 and CSH gel and lling
the voids between particles of y ash and cement grain.
The ner y ashes reduced the pore sizes and provided
higher numbers of nucleation sites for the hydration prod-
ucts than those of original y ash. At 90 days (Fig. 16c and
Fig. 17c), the pastes had a denser structure. The change in
pore size of pastes with age was a result of the growth of
hydration and pozzolanic products. At this age, the pozzo-
lanic reaction on some y ash particles was discernible
from the broken surface of y ash particle. It was seen that
the observed particles had a smooth surface even though
they were embedded in the paste for a long time. It was evi-
dent that although the matrix had not been fully developed
it still underwent the product of either pozzolanic reaction
or hydration. From these results, it is concluded that the
blended cement paste containing ner y ash produces a
denser structure than that of the paste with the coarser
y ash.
4. Conclusions
Based on the results obtained, the following conclusions
can be drawn.
1. The blended cement paste containing original y ash
generally exhibited a lower pore size than that of Port-
land cement type I paste.
 P. Chindaprasirt et al. / Construction and Building Materials 21 (2007) 15341541
2. The blended cement paste containing classied y ash
resulted in a lower pore size than that of the one with
original y ash.
3. The intensity peak of Ca(OH)2 of blended cement paste
containing y ash decreased with an increase in y ash
content and neness.
4. The hydration reaction, pozzolanic reaction, packing
eect, and nucleation eect were enhanced by the incor-
poration of ner y ash. As a result the paste becomes
more homogenous, denser in structure and lower
Ca(OH)2 than the paste with the coarser y ash.
Acknowledgements
The authors gratefully acknowledge the nancial sup-
ports from the Thailand Research Fund (TRF) who spon-
sored the research under the Royal Golden Jubilee Ph.D.
program and the Ministry of Education of Thailand under
the Ministry Sta Development Project. We also thank the
Department of Civil Engineering, King Mongkuts Univer-
sity of Technology Thonburi and Suranaree University of
Technology for providing facilities and equipments.
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