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Construction

and Building

Construction and Building Materials 19 (2005) 682–690


MATERIALS
www.elsevier.com/locate/conbuildmat

Influence of coarse aggregate on the permeation,


durability and the microstructure characteristics of ordinary
Portland cement concrete
L. Basheer *, P.A.M. Basheer, A.E. Long
School of Civil Engineering, QueenÕs University Belfast, Belfast BT7 1NN, Northern Ireland, UK

Received 12 February 2005; received in revised form 12 February 2005; accepted 22 February 2005
Available online 26 April 2005

Abstract

Reinforced concrete structures in marine and similar environmental conditions have to withstand severe exposures. Due to this,
the mix design procedures have to be revised to include durability as a primary criterion along with strength and workability. In line
with this need, an investigation was carried out at QueenÕs University Belfast with the financial help of the Department of Environ-
ment, Transport and the Regions, UK. The main objective of the research was to understand the influence of mix parameters on
workability, strength, durability and microstructure and to propose a new mix design procedure within which durability has a higher
priority. The present paper reports part of this study, which investigates the effect of size and grading of the coarse aggregate on the
durability and the microstructure characteristics of concrete. The durability tests carried out included air permeability test, freeze–
thaw/salt scaling resistance test and an accelerated carbonation test. The microstructure study was carried out using a scanning elec-
tron microscope (SEM) and included image analysis of the interfacial transition zone (ITZ) around the coarse aggregate. The results
indicated that as the proportion of larger size aggregate increases in the mix, the local porosity at the ITZ increases and the overall
durability decreases. It has also been found that reducing the average aggregate size in a mix improves the pore structure and en-
hances the durability of the concrete.
 2005 Elsevier Ltd. All rights reserved.

Keywords: Concrete; Durability; Microstructure; SEM; ITZ

1. Introduction concrete permeability is influenced by pore volume, size


and continuity. It is believed that capillary voids larger
Most of the important properties of hardened con- than 50 lm, referred to as macro pores, are detrimental
crete are related to the quantity and characteristics of to strength and impermeability, whereas voids smaller
various types of pores in the cement paste and aggregate than 50 lm, referred to as micro pores, are more related
components of the concrete. For example, the engineer- to drying shrinkage and creep [2].
ing properties of concrete, such as strength, durability, The movement of gases, liquids and ions through
shrinkage and permeability, are directly influenced or concrete is important because of their interactions with
controlled by the number, type and size of pores present concrete constituents and the pore water which can alter
[1]. The total volume of pores, not their size or continu- the integrity of concrete directly and indirectly, leading
ity affect the strength and elasticity of concrete, whereas to the deterioration of structures. In reinforced concrete
this deterioration is mainly due to the corrosion of rein-
*
Corresponding author. Tel.: +28 90974027; fax: +28 90663754. forcement, freeze–thaw attack or chemical attack. In the
E-mail address: l.basher@qub.ac.uk (L. Basheer). recent past the cost of repair of structures due to such

0950-0618/$ - see front matter  2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2005.02.022
L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690 683

deterioration has been high. This has led to efforts by pores [8,13]. Hence, this technique is used in this work
researchers and engineers to understand concrete better for studying the ITZ pore structure.
so that durable concrete can be produced in the future.
Concrete has a highly heterogeneous and complex
structure. At the macroscopic level concrete may be con- 2. Experimental programme
sidered to be a two-phase material, consisting of aggre-
gate particles dispersed in a matrix of cement paste. At 2.1. Variables
the microscopic level, a third phase – the transition zone
– may be identified (2). This transition zone exists as a Table 1 gives the mix variables used in the investiga-
thin shell, called the interfacial transition zone (ITZ), be- tion. To obtain a range of coarse aggregate grading the
tween aggregate particles and hydrated cement paste proportion of 10 and 20 mm aggregate was varied. For
(hcp). It has been established that the ITZ is profoundly the aggregate size effect, 10 and 20 mm single size aggre-
different from the bulk cement paste in terms of mor- gates were used. A constant water–cement ratio of 0.6
phology, composition and density [2–10]. There have and aggregate–cement ratio of 6 was used in all the
been suggestions that the strength of the cement aggre- cases. Mixes with two different fine aggregate-coarse
gate bond may be the limiting factor in the determina- aggregate ratios (FA/CA) were used for both the perme-
tion of the ultimate strength of concrete [11]. ation and durability studies. For the micro structural
Furthermore, as the porosity of the ITZ is higher than study only 0.5 FA/CA was used.
that of bulk paste [6–10], the ITZ has a significant effect
on the permeability and durability of concrete. 2.2. Materials used
This paper reports a study carried out to ascertain the
effect of coarse aggregate grading and size on the perme- Class 42.5 N Portland cement [14], medium graded
ation properties and durability of concrete. The investi- [15] natural sand and crushed basalt coarse aggregate
gation involved a study of the pore structure were used for manufacturing the concrete samples.
characteristics of the ITZ, with the objective of linking The various properties of the aggregates are summarised
the pore structure characteristics to the permeation in Table 2.
properties and the durability of ordinary Portland ce- To control the moisture condition of the aggregate,
ment concretes. all aggregates were oven-dried at a temperature of
40 C. The coarse aggregate was dried for 1 day and
1.1. Characterisation of interfacial transition zone the fine aggregate for 2 days. Before the aggregates were
used to make concrete they were allowed to cool for at
Back scattered electron (BSE) imaging technique can least 1 day. The saturated surface dry 1-hour water
be used to characterise the pore structure of the ITZ. absorption values [16] were also measured. This allowed
Low viscosity epoxy impregnated polished samples of a corrected water quantity to be calculated when batch-
concrete are used for BSE imaging. The underlying prin- ing the materials, to ensure that the aggregate in the con-
ciple is that the contrast of the BSE images depends on crete was in a saturated surface-dry condition.
the mean atomic number of the concrete constituents. In
the BSE images anhydrous phases of the unreacted ce-
ment particles appear bright, the calcium hydroxide
light grey, the other hydration products as various
shades of darker grey with the epoxy impregnated pores Table 2
appearing black [8]. Consequently by processing images Properties of aggregates used
of polished sections it has been possible to determine the Aggregate type 1 h absorption Specific Fineness
distribution of the phases in hydrated cement paste [12]. (%) gravity modulus
Furthermore, these images can also be utilised to ascer- Fine aggregate (sand) 1 2.72 2.6
tain porosity characteristics of the ITZ including the 10 mm crushed basalt 0.5 2.93 5.92
20 mm crushed basalt 0.5 2.88 7.04
porosity gradient [10] and the amount of penetrable

Table 1
Variable used for the investigation
Variable Levels
FA/CA 0.5 0.7
Coarse aggregate 100% 10 mm 67% 10 mm + 33% 20 mm 33% 10 mm + 67% 20 mm 100% 20 mm
grading and notation (10 mm) (10/20 = 2) (10/20 = 0.5) (20 mm)
Note: FA/CA fine aggregate–coarse aggregate ratio.
684 L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690

2.3. Manufacture of test specimens 2.4. Test methods

Six 250 · 250 · 100 mm blocks and three 100 mm 2.4.1. Air permeability test
cubes were cast for each of the variables in Table 1. The air permeability of concrete was measured on the
The blocks were used for the permeation and durability preconditioned blocks using the Autoclam Permeability
studies and the three cubes were used to obtain the com- system [18]. This test has been used in research for more
pressive strength (the slump and cube compressive than a decade and has proved to be very reliable and
strength values are given in Table 3). One sample from easy to use. Details of the test can be obtained in [18].
each mix was used for the micro structural study. The test provides a relative measure of the air perme-
For each mix the required quantities were batched by ability of concrete in Ln(Bar)/min.
mass. These quantities were then mixed together using a
pan mixer in accordance with BS 1881: Part 125: 1986 2.4.2. Salt scaling test
[17]. For both blocks and cubes the concrete was cast The freeze–thaw/salt scaling test was carried out
in two layers. A vibrating table was used to compact according to the RILEM test procedure [19]. The spec-
the concrete. Full compaction was considered to have imens for the test were 100 mm diameter cores taken
been achieved when air bubbles stopped appearing on from the slabs used for the Autoclam air permeability
the concrete surface. After vibrating, the concrete sur- test. The cores were dried for 2 weeks in a fan-assisted
face was finished smooth using a metal float and then cabinet maintained at 40 C and 20% relative humidity.
covered with a polythene sheet to prevent evaporation The curved surfaces of these cores were then coated with
of water from the concrete. an epoxy emulsion. These cores were then kept in a 3%
Approximately, 6 h after the concrete had been cast sodium chloride solution for 7 days, with the test surface
the moulds were covered with a damp hessian. The (mould finished face) touching the solution. The face of
moulds were stripped next day and the hardened con- the cores opposite to the test surface was then coated
crete samples were placed in a constant temperature with the epoxy emulsion. The samples were then trans-
(±20 C) water bath for 3 days. The specimens were then ferred to test cells again with the test surface in contact
transferred into a storage laboratory kept at a constant with the 3% salt solution. The cells were then placed in
temperature of 18 C (±2 C) and a relative humidity of an automatic environmental chamber and subjected to
60% (± 5%). When the blocks were 14 days old they test cycles as shown in Fig. 1. At the end of every two
were placed in a drying cabinet at a temperature of cycles, the specimens were taken out of the chamber
40 C and a relative humidity of 20%. This was done and the loose particles removed by means of an ultra-
to remove moisture from the surface of the concrete in sonic bath. The loose particles collected were dried at
order to eliminate the effect of moisture on the perme- 100 C for 24 h and then weighed. These measurements
ation results. After 14 days of drying the specimens were were continued for 28 cycles.
ready for testing. For this they were transferred to a test-
ing laboratory (kept at a constant temperature of 20 C 2.4.3. Accelerated carbonation test
(±0.5 C) and relative humidity of 50% (± 5%)) and The carbonation resistance of different mixes was
tested on the following day. The cubes were cured and determined by carrying out an accelerated carbonation
conditioned in the same way as the slabs in order to en- test on 100 mm cores removed from the blocks used
sure that the compressive strength and other parameters for the permeability tests. The cores used for the test
were measured using similar concrete. The cubes were were dried in a fan-assisted cabinet for 2 weeks at
then crushed to determine the concrete compressive 40 C and 20% relative humidity. These were then
strength. coated with epoxy emulsion on the curved surface and
the trowel-finished face. When the epoxy was cured,

Table 3
Slump and 28-day compressive strength the study
No: CA-G FA/CA Slump (mm) Strength (N/mm2)
+20.00 C
1 10 mm 0.5 35 46.9
2 10/20 = 2.0 56 44.1 Time
3 10/20 = 0.5 79 44.2 0.00 C (Hours)
4 20 mm 103 42.9
5 10 mm 0.7 18 50.1 -20.00C
6 10/20 = 2.0 28 45.2
4.0 3.0 4.0 1.0
7 10/20 = 2.0 23 45.4 Temperature
8 20 mm 61 44.9 (0 C)

Note: CA-G coarse aggregate grading. Fig. 1. Freeze–thaw cycle used for RILEM salt scaling test.
L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690 685

the cores were placed in an electronically controlled car-


bonation chamber in an environment of 5 ± 0.1% car-
bon dioxide at 20 ± 0.5 C and 65 ± 1% relative
humidity. At the end of 3 weeks, the samples were taken
out and split longitudinally. The freshly broken surface
was sprayed with a phenolphthalein indicator solution.
After 24 h the depth of the pink coloration was mea-
sured to the nearest millimetre at six different locations.
An average of these values was used for comparing dif-
ferent mixes.

2.4.4. Electron microscopic study of the ITZ


Cores of 50 mm diameter were cut from the blocks
used for the permeation studies. The cores were then
cut along their diameter and a slice of size
25 mm · 25 mm · 2 mm was removed from the mould-
finished face of each core. The slices were then wrapped
in thin polythene sheets to prevent any carbonation tak-
ing place. These thin slices were dried under vacuum and
then impregnated with an ultra low viscosity epoxy.
After the epoxy had cured the specimens were polished
with diamond grit of progressively finer sizes down to
0.25 lm. The polished samples were then coated with
carbon to 10 nm thickness.
The carbon-coated samples were placed under a scan-
ning electron microscope (SEM) and 20 backscatter
images from around the coarse aggregate present in Fig. 2. (a) Segmentation using histogram. (b) Typical porosity
the slice were collected at random. The image magnifica- distribuation curve.
tion used was 400 times and the electron beam was kept
at a distance of 15 mm away from the top of the speci-
men in all cases. Each image consisted of a small part
of aggregate on the left hand side of the picture and 3. Results and discussion
the rest was the matrix of cement paste and mortar
(Fig. 2(a)). The overall size of each image was 3.1. Slump and compressive strength
336 · 262 lm.
The porosity gradient was determined using an image The slump and 28-day compressive strength results
analysis computer software programme – NIH Image. In of each mix are presented in Table 3. An increase in
order to do this, thresholding of the grey scale to identify slump and marginal decrease in cube compressive
pores from the rest was essential. This was done by trial strength can be noted with an increase in the proportion
and error and by carrying out a sensitivity analysis. Once of 20 mm aggregate in the mix. The reduction in water
the threshold grey scale was decided, the software en- demand with an increase in the size of coarse aggregate
abled the determination of porosity in a strip of 10 lm is well documented [2]. In this experimental programme
thickness away from the face of the aggregate (Fig. when the proportion of 20 mm aggregate increased for a
2(a)). This strip was moved on an incremental basis by given water–cement ratio, the reduction in water de-
10 lm width away from the face of the coarse aggregate mand led to the increase in slump. However, as the
and each time the porosity of the 10 lm thick strip was water–cement ratio was not changed, the strength did
determined as a percentage of the total area of the strip. not vary significantly.
Once the strip reached the end of the image, the analysis
was repeated on other images collected from the same 3.2. Air permeability
sample. Therefore, for each 10 lm increment strip away
from the coarse aggregate, there were 20 porosity values Tables 4 and 5 give the results of the air permeability
and an average of these values was reported as the poros- test as AP index [18]. When the effect of coarse aggregate
ity of this 10 lm thick strip of concrete. The average grading is considered, it can be seen that as the propor-
porosity values were then plotted against the distance tion of 20 mm aggregate increases in the concrete air
from the face of the aggregate to determine the charac- permeability increases, indicating a reduction in durabil-
teristics of the interfacial zone (Fig. 2(b)). ity [20]. This is seen for both FA/CA ratios. In Table 5,
686 L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690

Table 4
The effect of aggregate grading on air permeability, salt scaling resistance and carbonation resistance
Coarse aggregate grading FA/CA AP index (Ln(mBar)/min) Cumulative scaling wt (g) Depth of carbonation (mm)
10/20 2 0.5 0.114 148.6 12.7
10/20 0.5 0.139 406.9 13.1
20 mm 0.181 642.3 13.7
10/20 2 0.7 0.06 67.02 12.8
10/20 0.5 0.105 53.05 11.3
20 mm 0.115 86.05 12.4

Table 5
The effect of aggregate size on air permeability, salt scaling resistance and carbonation resistance
Coarse aggregate size (mm) FA/CA AP index (Ln(mBar)/min) Cumulative scaling wt (g) Depth of carbonation (mm)
10 0.5 0.11 46.2 11.1
20 0.181 642.3 13.7
10 0.7 0.076 78.05 11.2
20 0.115 86.05 12.4

the effect of increasing the size of coarse aggregate from increase in FA/CA, which would suggest that when the
10 to 20 mm is to increase the air permeability. There are FA/CA increased, there was an associated decrease in
two possible reasons for these results. When the size of water–cement ratio. This might have been the result of
coarse aggregate increases, there is a reduction in the increased absorption of mix water by sand over and
tortuosity of the flow path, which tends to increase the above that was accounted in mix proportioning. Never-
permeability. The second reason is that when larger size theless, it can be concluded that the reduction in effective
coarse aggregates are used, the possibility of the bleed water–cement ratio associated with the increase in fine
water getting collected below the coarse aggregate in- aggregate content is responsible for the reduction in
creases, which leads to an increase in local water–cement air permeability.
ratio and hence the porosity. An increase in porosity Fig. 3 shows the effect of average aggregate size on
around the aggregate would increase the permeability the air permeability. (The average aggregate size was ob-
of the concrete. However, Table 6 indicates that only tained from the sieve analysis data, using standard pro-
moderate variations in air permeability occurred and cedures). As the average aggregate size in the mix
all the samples used for this study fall in the region of increases the air permeability index increases. A straight
medium risk concretes in terms of durability [20]. line, with a regression coefficient of 0.87, can represent
It can also be seen from Tables 4 and 5 that, as the this increase. The combined effect of aggregate size, its
fine aggregate–coarse aggregate ratio was increased relative proportion in a mix and the quantity of fine
from 0.5 to 0.7, the air permeability of the concrete de- aggregate in the mix on air permeability was obtained
creased. This is quite unexpected because when the FA/ by plotting air permeability against the average size of
CA increases, the increase in sand volume for a given aggregate in Fig. 3. The figure would suggest that the
aggregate–cement ratio would increase the area of inter- permeability (and hence the durability) of concrete
facial transition zone, which in turn reduce the tortuos- could be improved by reducing the average size of the
ity of the flow path. This means that the air permeability combined fine and coarse aggregates.
should have increased. In Table 3, there is a reduction in
slump and an increase in compressive strength with the
0.2
AP Index x 102 Ln(Bar)/min

y = 0.0627x - 0.0191
0.18 2
0.16 R = 0.871
Table 6 0.14
Risk rating of durability based on Autoclam air permeability index 0.12
(20) 0.1
0.08
Air permeability index (Ln(mBar)/min) 0.06
0.04
Range Rating 0.02
0
<0.1 Low
0 0.5 1 1.5 2 2.5 3 3.5
0.1–0.5 Medium
Average aggregate size (mm)
0.5–0.9 High
>0.9 Very high Fig. 3. Effect of average aggregate size on air permeablity index.
L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690 687

coarse aggregate mixes are compared for both the FA/


n1 n1 CA ratios. However, the effect of an increase in fine
aggregate–coarse aggregate ratio from 0.5 to 0.7 is to
n2

porosity %
porosity %

improve the salt scaling resistance of the concrete. As


in the case of air permeability, it is possible to conclude
that an increase in the proportion of smaller size frac-
n n
tions of aggregate in a mix would improve its salt scaling
resistance when the water–cement ratio is kept constant.
ITZ1 ITZ2 ITZ2
However, it has to be pointed out that the effect of the
(a) Distance (micron) (b) Distance (micron) average aggregate size is not as significant a factor as
Fig. 4. Two different types of porosity gradients. the water–cement ratio of a mix. In a previous study,
a lower water cement ratio (0.45) concrete withstood
100 cycles of freezing and thawing [21] compared to
3.3. Salt scaling 0.6 water–cement ratio concrete which only withstood
about 28 cycles.
The salt scaling test gave results similar to those of
the air permeability test (Tables 4 and 5). As the propor-
tion of the 20 mm aggregate increases in the mix the 3.4. Carbonation
cumulative salt scaling also increases, indicating a de-
crease in durability (Table 4). A similar trend can also In Table 4, there was no consistent effect of coarse
be seen in Table 5 when the results of 10 and 20 mm aggregate grading and the FA/CA on the depth of

Fig. 5. (a) Aggregate grading and porosity. (b) Aggregate grading and ITZ thickness. (c) Aggregate grading and total porosity percentage.
688 L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690

carbonation. Russell and co-workers [22] showed that – region of peak porosity (n1) which is about 40 lm
the depth of carbonation is primarily dependent on the thick (ITZ1),
water–cement ratio. For the mixes in Table 4, the – a transient porosity region (n2) which is about 160
water–cement ratio was kept constant. Therefore, lm thick (ITZ2),
the depth of carbonation remained almost the same – the bulk porosity region (n).
for all the mixes. However, Table 5 shows that the depth
of carbonation increases when the aggregate size is in- The area under the curve in the peak porosity region
creased. This is similar to the results reported by Basheer is termed as A1 and that in the transient porosity region
et al. [23]. The increase in the size and porosity of the is termed as A2. These values give a combined effect of
ITZ around the coarse aggregate due to the increase in the percentage porosity and the ITZ. In some cases n2
size of the coarse aggregate might have contributed to and the corresponding ITZ1 and A1 values are not pres-
this increase in depth of carbonation. ent (Fig. 4(b)). Although for microstructure studies in
the literature, other researchers have reported the thick-
3.5. ITZ properties ness of the ITZ as 10–50 lm [8,15,16], a more open ap-
proach was used for analysing the results in this paper.
The percentage porosity distributions at the ITZ, This was to avoid losing any valuable information from
obtained from SEM analysis, were used for a compar- the results.
ative study of the ITZ in samples from each mix. In Fig. 5(a)–(c) present the ITZ data versus aggregate
general, the distribution of porosity obtained across grading for mixes of FA/CA ratio 0.5. Results indicate
the ITZ can be divided in to three sections (Fig. 4(a) that as the proportion of 20 mm aggregate increases
and (b)): so does the porosity values (n1, n2 and n) (Fig. 5(a)).

Fig. 6. (a) Aggregate size and porosity. (b) Aggregate size and ITZ thickness. (c) Aggregate size and total porosity.
L. Basheer et al. / Construction and Building Materials 19 (2005) 682–690 689

This effect is more apparent at the ITZ region and is (ii) Unlike other published work on the effect of fine
only marginal for the bulk porosity. These result corre- aggregate content on the air permeability of con-
late well with the previous three test results given in Sec- crete, when the fine aggregate content increased
tions 3.2–3.4. the air permeability decreased. The increase in tor-
When the ITZ thicknesses are compared for these tousity is considered to have contributed to this
mixes (Fig. 5(b)), it can be seen that as the proportion effect.
of 20 mm aggregate increased in the mix, the ITZ thick- (iii) The salt scaling resistance followed a trend similar
ness also increased. This is more evident in ITZ2 than in to that of the air permeability reported in (i) and
ITZ1. Results from this study and a parallel study with (ii). The effect of aggregate grading and FA/CA
different water–cement ratios and aggregate–cement ra- on depth of carbonation was insignificant. How-
tios [24] indicate that the ITZ2 value is an important ever, the increase in size of aggregate led to an
parameter, which has to be considered during the anal- increase in the depth of carbonation.
ysis of ITZ results obtained from SEM analysis. (iv) The micro structural analysis at the ITZ clearly
From Fig. 5(c) it can be seen that the total porosity indicates that the coarser the aggregate the more
percentage, both A1 and A2, increased as the propor- porous it is at the ITZ. This is in line with the
tion of 20 mm aggregate increased in the mix. Therefore, results given by permeability and durability
it can be concluded that when the proportion of course studies.
aggregate is increased, there will be an associated in- (v) Therefore, in order to design durable concretes
crease in interfacial transition zone porosity volume. using oPc, it is preferable to use smaller size aggre-
Fig. 6(a)–(c) show the effect of aggregate size on per- gate and a low average aggregate size for the com-
centage porosity values and ITZ thicknesses. As ob- bined fine and coarse aggregate.
tained for the permeation and durability results,
reported in Sections 3.2–3.4, increasing the coarse aggre-
gate size in the mix resulted in an increase in the percent-
age porosity values (Fig. 6(a)) and the ITZ thicknesses Acknowledgements
(Fig. 6(b)). These results and the results given in the
above paragraphs indicate that the microstructure study The funding to carryout this project was provided by
using SEM and image analysis give a clear picture of the the Department of Environment, Transport and the Re-
pore structure distribution at the aggregate interface, gions, UK. The facilities to carryout this research was
which reflects the air permeability and durability of provided by the school of Civil Engineering and the
the concretes. This is apart from the fact that these Electron microscopic unit at QueenÕs University Belfast.
images only give a two dimensional picture of the pore Both these are gratefully acknowledged.
structure. Also, there could be error introduced in the
SEM analysis because of the fact that it is not known
at what angle to the coarse aggregate the concrete was References
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