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Microcracking and strength development of alkali activated slag
concrete
Frank Collins a,*, J.G. Sanjayan b
a
Maunsell Pty Ltd, Level 9, 161 Collins Street, Melbourne, Victoria 3000, Australia
b
Department of Civil Engineering, Monash University, Clayton, Victoria 3800, Australia
Received 23 August 2000; accepted 3 January 2001
Abstract
Alkali activated slag concrete (AASC) is made by activating ground granulated blast furnace slag with alkalis without the use of
any Portland cement. This study investigates the level of microcracking which occurs in AASC when subjected to various types of
curing regimes. The corresponding compressive strength developments of AASC were monitored. The level of microcracking were
measured using three di€erent types of tests: (1) frequency and size of surface cracks using crack-detection microscope (2) water
sorptivity tests measuring absorption of water by capillary attraction and (3) mercury intrusion porosimetry (MIP) tests which
measured the pore size distribution of AASC and AAS pastes (AASPs). The results show that the lack of moist curing of AASC
increased the level of microcracking measured using all three di€erent tests mentioned above. The strength development of AASC is
also signi®cantly reduced by lack of moist curing. Ó 2001 Elsevier Science Ltd. All rights reserved.
Keywords: Strength development; Microcracking; AASC; AASPs
1. Introduction
Alkali activated slag concrete (AASC) is made with
100% ground granulated blast furnace slag activated by
alkalis, instead of the Portland cement in the binder of
concrete. Details of AASC can be found in [33].
AASC shares the same sensitivity to lack of curing
found in concretes made with slag blended cements
(blend of Portland cement and slag). Wainwright [34],
Butler and Ashby [3], and Butler and Ashby [4] found
high sensitivity of slag blended cement concrete to lack
of moist curing and found signi®cantly lower compres-
sive strength than companion samples cured in lime
saturated bath water. Swamy and Bouikni [31] showed
that concrete mixtures containing 65% slag as the ce-
mentitious binder have strength retrogression when air
cured. Nakamura et al. [24] measured up to 30±40%
lower compressive strength of air cured 50% slag blen-
ded cement concrete compared with bath cured con-
crete. However, Wainwright [34] argues that this may be
a size e€ect since the strength loss in larger samples is
not as pronounced. In the case of 40 MPa concrete with
50% slag blended cement as the binder, Sioulas [30]
measured 17% lower compressive strength of sealed
cured cylinders compared with bath cured cylinders.
Furthermore, Sioulas [30] showed the cores taken from
large columns made of blended cement concrete (up to
70% replacement of Portland cement with slag) had up
to 35% less strength than the bath cured cylinder
strength, and had signi®cantly less strength than that of
companion ordinary Portland cement (OPC) concrete
columns.
The strength of AASC is also sensitive to the relative
humidity (RH) of the curing environment. Talling and
Brandstetr [33] report that loss of moisture during dry
air storage reduces strength between 7 and 28 days,
however the magnitude of strength loss and the type of
activator is unreported.
Slag binder that has been activated by NaOH shows
lower strength following exposed curing. Kutti and
Malinowski [18] showed there is considerable decrease
in compressive strength when comparing air-dried
NaOH alkali activated slag mortar (AASM) at 50% RH
and 20°C with bath cured NaOH AASM samples at
20°C. Byfors et al. [5] measured up to 20% lower com-
pressive strength when comparing water cured AASC
Cement & Concrete Composites 23 (2001) 345±352
www.elsevier.com/locate/cemconcomp
*
Corresponding author. Tel.: +61-3-9653-1234; fax: +61-3-9654-
7117.
E-mail address: fgco@maunsell.com.au (F. Collins).
0958-9465/01/$ - see front matter Ó 2001 Elsevier Science Ltd. All rights reserved.
PII: S 0 9 5 8 - 9 4 6 5 ( 0 1 ) 0 0 0 0 3 - 8
with air cured (50% RH) AASC after initial seven days
wet curing. Kukko and Mannonen [17] measured lower
early age compressive strength when comparing samples
cured at 40% RH and 20°C) with samples cured at 95%
RH and 20°C, however, following one year, the com-
pressive strength was almost identical. Kutti et al. [19]
measured 35% lower compressive strength between
NaOH activated AASM cured at 33% RH and 20°C at
36 months and companion samples cured at 94% RH
20°C. However, when exposed at RH of 76% and 86%,
the samples show similar compressive strength to prisms
cured at 94% RH. Hakkinen [13] showed that NaOH
activated AASC cylinders moist cured for seven days
followed by exposure to 40% RH and 20°C were 10.5%
lower in compressive strength at one year compared
with companion samples cured at 70% RH and 20°C.
For sodium silicate AASM, Anderson and Gram [1]
measured lower compressive strength of air cured (80%
RH and 20°) AASM compared with ordinary Portland
cement mortar (OPCM) up to seven days. However,
beyond seven days AASM showed better compressive
strength than OPCM. Following air storage at 95% and
70% RH and 20°C, Talling [32] reports little di€erence in
cylinder strength of sodium silicate activated AASC.
However, when stored at 50% RH and 20°C, strength
development stops after 28 days and the strength at 91
days is 14% lower than companion samples stored at
95% RH.
Hakkinen [13] showed that dry exposed NaOH acti-
vated AASC displays a size e€ect, whereby the strength
of 150-mm diameter cylinders is less a€ected than 100-
mm diameter cylinders by microcracks developed during
drying. However, the strength variations of a sample
thicker than 150 mm following exposed curing is unre-
ported.
This paper describes the e€ect of microcracking on
the strength development of AASC cylinders subjected
to di€erent curing types.
2. Experimental programme
2.1. Constituent materials and concrete and paste mix-
tures
The chemical composition and properties of the slag
is summarised in Table 1. The term water/binder (w=b)
ratio is used instead of the conventional water/cement
ratio to describe the non-Portland cement binder. The
slag is supplied with gypsum (2% SO3) which is blended
with the slag. The dry powdered sodium silicate acti-
vator (composed of 29% Na2O, 28% SiO2, and 43%
H2O) was pre-blended with the slag in the dry form
prior to use for concrete manufacture. The hydrated
lime activator (1% lime in water slurry form) was added
to the mix with the mixing water.
The coarse aggregate consisted of 14 mm maximum
size basalt with a speci®c gravity of 2.95 and 24 h water
absorption of 1.2%. The ®ne aggregate consisted of river
sand with a speci®c gravity of 2.65, 24 h water absorp-
tion of 0.5%, and a ®neness modulus of 2.19.
The concrete mixture proportions are summarised in
Table 2. The materials used for concrete making and the
method of preparing concrete mixes in the laboratory
were in accordance with Australian Standards. Collins
and Sanjayan [8] have previously reported the fresh and
mechanical properties of the concrete mix shown in
Table 2.
Paste mixtures were also made to investigate the pore
size distribution by mercury intrusion porosimetry
(MIP). Mixing of AAS paste (AASP) was conducted in
a 20-l stainless steel mixing bowl. Mixing was by ma-
chine at 98 revolutions per minute in a Kenwood KNM20
planetary mixer. The slag and sodium silicate activator
was pre-blended in the dry form for 2 min. The mixing
water was then added. The hydrated lime was added as a
Table 1
Properties of cementitious materials
Constituent/property Slag
SiO2 (%) 35.04
Al2O3 (%) 13.91
Fe2O3 (%) 0.29
MgO (%) 6.13
CaO (%) 39.43
Na2O (%) 0.34
TiO2 (%) 0.42
K2O (%) 0.39
P2O5 (%) <0.1
MnO (%) 0.43
Total sulphur as SO3 (%) 2.43
Sulphide sulphur as S2À
0.44
Cl (ppm) 80
Fineness (m2
=kg) 460
Loss on ignition (%) 1.45
Table 2
Summary of concrete mixture proportions (kg=m3
)
Constituents AASCa
Slag 360
Free waterb
180
w=b 0.5
Fine aggregate 830
Coarse aggregate 14 mm 1130
Air content % 1.2
a
Slag activated by powdered sodium silicate and lime slurry.
b
Adjustments made for water in aggregates (to saturated surface dry
condition), lime slurry, and sodium silicate.
346 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
1:3 hydrated lime: water slurry. The mixing procedure
was 2-min mixing followed by 2 min of rest, followed by
further mixing for 2 min. The ¯uid pastes were poured
into cylindrical moulds, which had internal dimensions
63 mm diameter  98 mm length. The w=b of AASP
was 0.5. Following demoulding at one day, samples
from each paste type were exposed to 23°C and 50% RH
for 3, 7, 28, and 56 days. At the required time of test, the
samples were crushed to a size adequate to pass a 2.36-
mm sieve.
2.2. Compressive strength tests
Standard cylinders (100 mm diameter and 200 mm
height) were made in accordance with Australian Stan-
dard AS1012, Parts 8 and 9 for compressive strength
testing. Following demoulding, the cylinders were sub-
jected to one of three curing regimes: bath, exposed or
sealed. The de®nitions of the curing regimes are:
1. bath ± immersed in saturated lime water at 23°C;
2. sealed ± specimen is storage in two polythene bags
and a sealed container so that no moisture movement
in or out of the specimen. The specimen temperature
was maintained at 23°C;
3. exposed ± air exposed at 50% RH and 23°C.
The cylinder specimens were tested under compression
in triplicate at 1, 3, 7, 28, 56, 91, 365 days.
Following compressive strength testing of AASC at
365 days, fragments of a size adequate to pass a 2.36-
mm sieve were obtained from the concrete test cylinders
for subsequent MIPs testing.
2.3. Surface crack measurements
For each cylinder, a line parallel to the longitudinal
axis of the cylinder was drawn at the third points around
the circumference. At the central 100 mm length of each
of these three lines, the number of cracks and crack size
was measured. The crack width was measured with a
crack-detection microscope that had a 4-mm range,
0.01-mm divisions, 40Â magni®cation, and built-in light
source.
2.4. MIP tests
The pore size distribution was determined using a
Micromeritics Autopore III 9429 porosimeter which was
capable of pressures from 0 to 414 MPa (60,000 psi). A
hydraulic pump generates the pressure and a contact
sensor measures the mercury volume. All operations are
automated by microprocessor and are conducted within
a fully enclosed pressure chamber. The assumed surface
tension of the triple-distilled mercury was 0.484 N/m at
25°C (ASTM D 440484 1992). The density of the mer-
cury was 13.546 g/ml and the assumed contact angle was
140°.
2.5. Water sorptivity tests
The MIP results only provide data on very small-scale
samples and therefore the extent of microcracking across
a larger cross-sectional area of concrete was examined by
water sorptivity testing. Therefore water sorptivity testing
of the 100-mm diameter test cylinders was conducted to
determine whether microcracking causes signi®cant con-
nected voids, thus leading to reduced compressive
strength of AASC during exposed curing.
Additional cylinders that were exposed to bath, sealed,
and exposed curing for 1, 3, 7, 28, and 56 days were saw
cut into two halves. The purpose of saw cutting is to
eliminate skin e€ects at the top or bottom concrete sur-
face. One half of each cylinder was tested for water
sorptivity, based on the procedure of Bamforth et al. [2].
The water sorptivity test measures capillary e€ects
when one face of the sample is just in contact with water.
The uptake of water, registered as vertical height rise and
weight gain, is determined over a period of time. The
capillary pores in concrete cause absorption of water by
capillary attraction. Hence, a measure of the rate of ab-
sorption provides a useful indication of the pore conti-
nuity of the concrete. The technique of Bamforth et al. [2]
relies on a simple set-up where one face of the sample is
immersed to a depth of 1±2 mm and the weight gain and
height rise of the sample is monitored with time. In un-
saturated concrete, water absorption is linearly related to
the square root of time, with the slope of the line de®ning
sorptivity of the material.
3. Compressive strength development
Compressive strength development of the standard
cylinders subject to bath, sealed, and exposed curing is
shown in Fig. 1. Fig. 1 shows that the strength of sealed
cured cylinders is lower than bath cured; after 365 days
the strength di€erence is 21%. The sealed cured cylinders
show little strength gain between 91 days and 1 yr. Fig. 1
shows 17% strength loss of exposed cylinders between 56
and 365 days. The strength of the exposed cylinders is
54% and 41% less than bath and sealed cylinders
strengths, respectively, at 365 days. Strength retrogres-
sion of AASC cylinders subjected to exposed curing has
not been reported previously in the literature.
4. Surface microcracking
AASC cylinders that were exposed to 23°C and 50%
RH from Day 1 onwards developed visible surface
F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352 347
crazing cracks, or microcracking (Fig. 2). The cause of
microcracking may be due to the very dry condition of
the surface concrete, as evidenced by zero measured
bleed [8], and also restraint of shrinkage-prone AASP by
rigid basalt coarse aggregate. The cylinders that were
cured under sealed and bath conditions showed no vis-
ible surface microcracking.
The crack frequency (number of cracks per sample)
for at 3, 7, 28, and 56 days is summarised in Fig. 3.
The results show that the majority of microcracks
occur within the ®rst three days and are mostly of the
size 0.01 mm. The frequency of the 0.01-mm crack size
reaches a maximum at 7 days followed by crack width
growth. The widths of the microcracks are as high as 0.3
mm.
Hsu et al. [15] showed that microcracks exist at the
interface between coarse aggregate and mortar before
any load is imposed, and the microcracks are caused by
mortar volume changes. AASC shows signi®cantly
greater shrinkage strains than OPCC when subjected to
drying conditions [8] and it is likely that the restraint
provided by the sti€ basalt coarse aggregate and the high
shrinkage of the AASP has lead to microcracking under
drying conditions. Meyers et al. [23] and Ravindrarajah
and Swamy [25] have shown that the microcrack density
increases with the magnitude of drying shrinkage. High
shrinkage of the paste can lead to interconnected mi-
crocracks, as shown by Sicard et al. [29], in the case of
very high strength concrete, due to desiccation. In the
case of repairs to reinforcement corrosion damaged
concrete, Collins and Roper [7] showed that the depth of
the zone of microcracking, observed near the repair
mortar to concrete substrate interface, had a strong
in¯uence on the soundness of the repair. Carrasquillo
et al. [6] asserts that the development of combined mi-
crocracks is an essential step in the progression toward
impending failure.
Following microscopic examination, Malolepszy and
Deja [21] observed negligible microcracks on 7-day
water cured AASM, however, when the same samples
were subsequently exposed to 65% RH and 20°C, mi-
crocracking was observed. Byfors et al. [5] also observed
microcracking on AASC and, following microscopic
examination, concluded that the frequency was greater
following exposed curing and this lead to reduced ¯ex-
ural strength. Cracking is more frequent and intense for
concrete with binders composed of alkali activated slag
than OPC and slag blended cements [11] and with in-
creased activator content [12]. At low aggregate/cement
ratio the microcracks become long and continuous [10].
Kutti and Malinowski [18] and Kutti et al. [19] conclude
that the microcracking is due to the formation of an
unstable (during drying) gel phase within the activated
slag paste. During drying, a number of breaks in the
particle to particle bonds throughout the gel structure
occur thereby forming microcracks in the paste. Ha-
kkinen [14] showed that microcracking is most pro-
nounced within the zone of drying and that 150-mm
diameter cylinders, which have a smaller proportion of
the cross-section a€ected by surface drying and hence
Fig. 2. Microcracks on AASC exposed to 50% RH and 23°C from
Day 1 onwards.
Fig. 3. Microcrack frequency of AASC exposed to 50% RH and 23°C
from Day 1 onwards.
Fig. 1. E€ect of type of curing on compressive strength, AASC,
w=b ˆ 0:5.
348 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
microcracking, show greater compressive strength than
100-mm diameter cylinders.
5. Pore size distribution
It is well established that blended slag cement binders
have a ®ner pore size distribution than OPC binders
[9,22,27,20,26,28,35].
AAS is sensitive to the type of curing. When sub-
jected to air curing, however, alkali activated slag binder
has higher number of pores in the 100±10,000 nm range
than OPC binder [1,10,12,13]. Hakkinen et al. [10]
showed that as hydration proceeds, under drying con-
ditions, activated slag binder has an increasing number
of pores within the 1000±10000 nm range, whereas the
number of pores for OPC binder remains constant. The
cause of increasing porosity within the 1000±10000 nm
range is microcrack development [12,13].
Fig. 4 shows the cumulative pore size distributions
for bath cured AASP with w=b ˆ 0:5. At one day, the
pore size distribution of AASP is coarse. From 1 to 3
days, there is a signi®cant shift towards a ®ner pore size
distribution. The results show increasing pore re®ne-
ment with increasing age.
Fig. 5 shows the cumulative pore size distributions
for sealed cured AASP with w=b 0.5. The pore size
distributions are very similar to the bath cured results
shown in Fig. 4.
The bath and sealed paste samples that were under
test were taken from the centre (interior) of the sample.
However, microcracking was visible on the surface of
the exposed AASP samples and therefore MIPS testing
was also undertaken at the outside and midway between
the centre and outside of the sample. Fig. 6 shows cu-
mulative pore size distribution of exposed AASP at 3, 7,
28, and 56 days.
Fig. 6 shows signi®cantly coarser pore size distribu-
tion at the exterior and interior locations than bath and
sealed cured specimens shown in Figs. 4 and 5, dem-
onstrating the e€ects of lack of curing. The pore size
distribution becomes coarser with distance towards the
exterior of the sample, however the total porosity at 3, 7,
and 28 days is very similar for all sample locations. At
56 days, the exterior pore size distribution is signi®cantly
coarser and the total porosity higher than at the internal
sample location and this is re¯ected by cessation of
growth of compressive strength for concrete tested at the
same age.
Table 3 shows the proportion of pores within the
mesopore, macropore, and voids/microcracks for
AASP, based on the IUPAC [16]. There is a higher
proportion of pores within the voids/microcracks pore
size region up to 28 days. Many of the microcracks that
were identi®ed and discussed above are too large to be
measured by MIPS and hence are not shown in Table 3.
Samples of 365 day AASC from standard cylinders
that were subjected to bath, sealed, and exposed curing
were tested by MIPS and the cumulative pore size dis-
tribution for concrete subjected to each of the curing
types is shown in Fig. 7.
The pore size distributions of bath and sealed cured
AASC are almost identical. This is despite the di€er-
ences that were measured in compressive strength. Ex-
posed AASC has considerably coarser pore size
distribution than both bath and sealed cured AASC.
For the exposed sample taken from the interior of the
cylinder, the total porosity is almost the same as the
bath and sealed cured samples. However, in the case of
the exposed sample taken from the exterior, the total
porosity is 3.67% greater than the sample taken from the
interior of the exposed cylinder. Although there is likely
to be errors introduced by aggregate contamination in
the sample, the e€ect of microcracking on the pore size
distribution is evident in the exposed samples.
Fig. 4. Cumulative pore size distribution of bath cured AASP,
w=b ˆ 0:5.
Fig. 5. Cumulative pore size distribution of sealed cured AASP,
w=b ˆ 0:5.
F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352 349
6. Water sorptivity
Fig. 8 shows that following exposed curing AASC has
increasing water sorptivity at ages beyond 3 days, indi-
cating the existence of a network of interconnected mi-
crocracks within the sample that become progressively
larger and continuous with increasing age. This indicates
that the interconnected network of microcracks is a
likely explanation for lower compressive strength of
AASC following exposed curing.
Fig. 8. E€ect of curing on water sorptivity.
Fig. 6. Cumulative pore size distribution of exposed cured AASP, w=b ˆ 0:5. (a) 3 days, (b) 7 days, (c) 28 days, (d) 56 days.
Fig. 7. Cumulative pore size distribution of bath, sealed, and exposed
curing for 365 days.
Table 3
Pore size proportions for AASP
Age
(days)
% Mesopores
(1.25±25 nm
radius)
% Macropores
(25±5000 nm
radius)
% Voids/microcracks
(5000±50,000 nm
radius)
3 74.0 16.6 9.4
7 76.0 14.9 9.1
28 82.0 10.4 7.6
56 81.3 12.5 6.2
350 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
7. Conclusions
The compressive strength is almost identical when
comparing bath cured AASC cylinders with sealed
cured cylinders for w=b ˆ 0:5. The laboratory exposed
(23°C and 50% RH) cylinders have 41.4% and 53.5%
lower compressive strength at 365 days than sealed
and bath cured cylinders, respectively. Between 28 and
365 days the exposed cured cylinders show 17.2%
strength loss.
Exposed AASC showed visible surface microcracks.
The majority of microcracks occur within the ®rst 3 days
and are mostly of the size 0.01 mm. The frequency of the
0.01-mm crack size reaches a maximum at 7 days fol-
lowed by crack width growth. The widths of micro-
cracks are as high as 0.3 mm.
The e€ect of microcracking on exposed AASC samples
were evident by considerably higher total porosity and
coarser pore size distribution that was measured by MIPS
testing.The pore size distribution of exposed AASP is
more porous than bath and sealed samples, with the po-
rosity increasing with distance towards the exterior of the
sample. Following exposed curing, AASC shows that
visible microcracking on the surface and water sorptivity
testing showed the samples to have high uptake of water
compared with bath and sealed cured companion cylin-
ders. The high uptake of water can be associated with a
continuous microcracking and capillary network, which
has lead to inferior compressive strength. This shows that
should AASC be used for construction it is imperative
that the concrete is well cured.
Acknowledgements
The ®nancial support for this project is jointly pro-
vided by Independent Cement and Lime Pty Ltd., Blue
Circle Southern Cement Ltd. and Australian Steel Mill
Services. The authors thank the sponsors, especially Alan
Dow, Tom Wauer, Katherine Turner, Wayne James, Paul
Ratcli€, John Ashby, and Dr. Ihor Hinczak for the
guidance and support. The enthusiastic participation of
®nal year student Dennis Kueh in this project is very much
appreciated. The e€orts and assistance with the labora-
tory work provided by Je€ Doddrell, Roger Doulis, and
Peter Dunbar are also gratefully acknowledged.
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352 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352

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Microcracking-Activated Slag (C&CC)

  • 1. Microcracking and strength development of alkali activated slag concrete Frank Collins a,*, J.G. Sanjayan b a Maunsell Pty Ltd, Level 9, 161 Collins Street, Melbourne, Victoria 3000, Australia b Department of Civil Engineering, Monash University, Clayton, Victoria 3800, Australia Received 23 August 2000; accepted 3 January 2001 Abstract Alkali activated slag concrete (AASC) is made by activating ground granulated blast furnace slag with alkalis without the use of any Portland cement. This study investigates the level of microcracking which occurs in AASC when subjected to various types of curing regimes. The corresponding compressive strength developments of AASC were monitored. The level of microcracking were measured using three di€erent types of tests: (1) frequency and size of surface cracks using crack-detection microscope (2) water sorptivity tests measuring absorption of water by capillary attraction and (3) mercury intrusion porosimetry (MIP) tests which measured the pore size distribution of AASC and AAS pastes (AASPs). The results show that the lack of moist curing of AASC increased the level of microcracking measured using all three di€erent tests mentioned above. The strength development of AASC is also signi®cantly reduced by lack of moist curing. Ó 2001 Elsevier Science Ltd. All rights reserved. Keywords: Strength development; Microcracking; AASC; AASPs 1. Introduction Alkali activated slag concrete (AASC) is made with 100% ground granulated blast furnace slag activated by alkalis, instead of the Portland cement in the binder of concrete. Details of AASC can be found in [33]. AASC shares the same sensitivity to lack of curing found in concretes made with slag blended cements (blend of Portland cement and slag). Wainwright [34], Butler and Ashby [3], and Butler and Ashby [4] found high sensitivity of slag blended cement concrete to lack of moist curing and found signi®cantly lower compres- sive strength than companion samples cured in lime saturated bath water. Swamy and Bouikni [31] showed that concrete mixtures containing 65% slag as the ce- mentitious binder have strength retrogression when air cured. Nakamura et al. [24] measured up to 30±40% lower compressive strength of air cured 50% slag blen- ded cement concrete compared with bath cured con- crete. However, Wainwright [34] argues that this may be a size e€ect since the strength loss in larger samples is not as pronounced. In the case of 40 MPa concrete with 50% slag blended cement as the binder, Sioulas [30] measured 17% lower compressive strength of sealed cured cylinders compared with bath cured cylinders. Furthermore, Sioulas [30] showed the cores taken from large columns made of blended cement concrete (up to 70% replacement of Portland cement with slag) had up to 35% less strength than the bath cured cylinder strength, and had signi®cantly less strength than that of companion ordinary Portland cement (OPC) concrete columns. The strength of AASC is also sensitive to the relative humidity (RH) of the curing environment. Talling and Brandstetr [33] report that loss of moisture during dry air storage reduces strength between 7 and 28 days, however the magnitude of strength loss and the type of activator is unreported. Slag binder that has been activated by NaOH shows lower strength following exposed curing. Kutti and Malinowski [18] showed there is considerable decrease in compressive strength when comparing air-dried NaOH alkali activated slag mortar (AASM) at 50% RH and 20°C with bath cured NaOH AASM samples at 20°C. Byfors et al. [5] measured up to 20% lower com- pressive strength when comparing water cured AASC Cement & Concrete Composites 23 (2001) 345±352 www.elsevier.com/locate/cemconcomp * Corresponding author. Tel.: +61-3-9653-1234; fax: +61-3-9654- 7117. E-mail address: fgco@maunsell.com.au (F. Collins). 0958-9465/01/$ - see front matter Ó 2001 Elsevier Science Ltd. All rights reserved. PII: S 0 9 5 8 - 9 4 6 5 ( 0 1 ) 0 0 0 0 3 - 8
  • 2. with air cured (50% RH) AASC after initial seven days wet curing. Kukko and Mannonen [17] measured lower early age compressive strength when comparing samples cured at 40% RH and 20°C) with samples cured at 95% RH and 20°C, however, following one year, the com- pressive strength was almost identical. Kutti et al. [19] measured 35% lower compressive strength between NaOH activated AASM cured at 33% RH and 20°C at 36 months and companion samples cured at 94% RH 20°C. However, when exposed at RH of 76% and 86%, the samples show similar compressive strength to prisms cured at 94% RH. Hakkinen [13] showed that NaOH activated AASC cylinders moist cured for seven days followed by exposure to 40% RH and 20°C were 10.5% lower in compressive strength at one year compared with companion samples cured at 70% RH and 20°C. For sodium silicate AASM, Anderson and Gram [1] measured lower compressive strength of air cured (80% RH and 20°) AASM compared with ordinary Portland cement mortar (OPCM) up to seven days. However, beyond seven days AASM showed better compressive strength than OPCM. Following air storage at 95% and 70% RH and 20°C, Talling [32] reports little di€erence in cylinder strength of sodium silicate activated AASC. However, when stored at 50% RH and 20°C, strength development stops after 28 days and the strength at 91 days is 14% lower than companion samples stored at 95% RH. Hakkinen [13] showed that dry exposed NaOH acti- vated AASC displays a size e€ect, whereby the strength of 150-mm diameter cylinders is less a€ected than 100- mm diameter cylinders by microcracks developed during drying. However, the strength variations of a sample thicker than 150 mm following exposed curing is unre- ported. This paper describes the e€ect of microcracking on the strength development of AASC cylinders subjected to di€erent curing types. 2. Experimental programme 2.1. Constituent materials and concrete and paste mix- tures The chemical composition and properties of the slag is summarised in Table 1. The term water/binder (w=b) ratio is used instead of the conventional water/cement ratio to describe the non-Portland cement binder. The slag is supplied with gypsum (2% SO3) which is blended with the slag. The dry powdered sodium silicate acti- vator (composed of 29% Na2O, 28% SiO2, and 43% H2O) was pre-blended with the slag in the dry form prior to use for concrete manufacture. The hydrated lime activator (1% lime in water slurry form) was added to the mix with the mixing water. The coarse aggregate consisted of 14 mm maximum size basalt with a speci®c gravity of 2.95 and 24 h water absorption of 1.2%. The ®ne aggregate consisted of river sand with a speci®c gravity of 2.65, 24 h water absorp- tion of 0.5%, and a ®neness modulus of 2.19. The concrete mixture proportions are summarised in Table 2. The materials used for concrete making and the method of preparing concrete mixes in the laboratory were in accordance with Australian Standards. Collins and Sanjayan [8] have previously reported the fresh and mechanical properties of the concrete mix shown in Table 2. Paste mixtures were also made to investigate the pore size distribution by mercury intrusion porosimetry (MIP). Mixing of AAS paste (AASP) was conducted in a 20-l stainless steel mixing bowl. Mixing was by ma- chine at 98 revolutions per minute in a Kenwood KNM20 planetary mixer. The slag and sodium silicate activator was pre-blended in the dry form for 2 min. The mixing water was then added. The hydrated lime was added as a Table 1 Properties of cementitious materials Constituent/property Slag SiO2 (%) 35.04 Al2O3 (%) 13.91 Fe2O3 (%) 0.29 MgO (%) 6.13 CaO (%) 39.43 Na2O (%) 0.34 TiO2 (%) 0.42 K2O (%) 0.39 P2O5 (%) <0.1 MnO (%) 0.43 Total sulphur as SO3 (%) 2.43 Sulphide sulphur as S2À 0.44 Cl (ppm) 80 Fineness (m2 =kg) 460 Loss on ignition (%) 1.45 Table 2 Summary of concrete mixture proportions (kg=m3 ) Constituents AASCa Slag 360 Free waterb 180 w=b 0.5 Fine aggregate 830 Coarse aggregate 14 mm 1130 Air content % 1.2 a Slag activated by powdered sodium silicate and lime slurry. b Adjustments made for water in aggregates (to saturated surface dry condition), lime slurry, and sodium silicate. 346 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
  • 3. 1:3 hydrated lime: water slurry. The mixing procedure was 2-min mixing followed by 2 min of rest, followed by further mixing for 2 min. The ¯uid pastes were poured into cylindrical moulds, which had internal dimensions 63 mm diameter  98 mm length. The w=b of AASP was 0.5. Following demoulding at one day, samples from each paste type were exposed to 23°C and 50% RH for 3, 7, 28, and 56 days. At the required time of test, the samples were crushed to a size adequate to pass a 2.36- mm sieve. 2.2. Compressive strength tests Standard cylinders (100 mm diameter and 200 mm height) were made in accordance with Australian Stan- dard AS1012, Parts 8 and 9 for compressive strength testing. Following demoulding, the cylinders were sub- jected to one of three curing regimes: bath, exposed or sealed. The de®nitions of the curing regimes are: 1. bath ± immersed in saturated lime water at 23°C; 2. sealed ± specimen is storage in two polythene bags and a sealed container so that no moisture movement in or out of the specimen. The specimen temperature was maintained at 23°C; 3. exposed ± air exposed at 50% RH and 23°C. The cylinder specimens were tested under compression in triplicate at 1, 3, 7, 28, 56, 91, 365 days. Following compressive strength testing of AASC at 365 days, fragments of a size adequate to pass a 2.36- mm sieve were obtained from the concrete test cylinders for subsequent MIPs testing. 2.3. Surface crack measurements For each cylinder, a line parallel to the longitudinal axis of the cylinder was drawn at the third points around the circumference. At the central 100 mm length of each of these three lines, the number of cracks and crack size was measured. The crack width was measured with a crack-detection microscope that had a 4-mm range, 0.01-mm divisions, 40 magni®cation, and built-in light source. 2.4. MIP tests The pore size distribution was determined using a Micromeritics Autopore III 9429 porosimeter which was capable of pressures from 0 to 414 MPa (60,000 psi). A hydraulic pump generates the pressure and a contact sensor measures the mercury volume. All operations are automated by microprocessor and are conducted within a fully enclosed pressure chamber. The assumed surface tension of the triple-distilled mercury was 0.484 N/m at 25°C (ASTM D 440484 1992). The density of the mer- cury was 13.546 g/ml and the assumed contact angle was 140°. 2.5. Water sorptivity tests The MIP results only provide data on very small-scale samples and therefore the extent of microcracking across a larger cross-sectional area of concrete was examined by water sorptivity testing. Therefore water sorptivity testing of the 100-mm diameter test cylinders was conducted to determine whether microcracking causes signi®cant con- nected voids, thus leading to reduced compressive strength of AASC during exposed curing. Additional cylinders that were exposed to bath, sealed, and exposed curing for 1, 3, 7, 28, and 56 days were saw cut into two halves. The purpose of saw cutting is to eliminate skin e€ects at the top or bottom concrete sur- face. One half of each cylinder was tested for water sorptivity, based on the procedure of Bamforth et al. [2]. The water sorptivity test measures capillary e€ects when one face of the sample is just in contact with water. The uptake of water, registered as vertical height rise and weight gain, is determined over a period of time. The capillary pores in concrete cause absorption of water by capillary attraction. Hence, a measure of the rate of ab- sorption provides a useful indication of the pore conti- nuity of the concrete. The technique of Bamforth et al. [2] relies on a simple set-up where one face of the sample is immersed to a depth of 1±2 mm and the weight gain and height rise of the sample is monitored with time. In un- saturated concrete, water absorption is linearly related to the square root of time, with the slope of the line de®ning sorptivity of the material. 3. Compressive strength development Compressive strength development of the standard cylinders subject to bath, sealed, and exposed curing is shown in Fig. 1. Fig. 1 shows that the strength of sealed cured cylinders is lower than bath cured; after 365 days the strength di€erence is 21%. The sealed cured cylinders show little strength gain between 91 days and 1 yr. Fig. 1 shows 17% strength loss of exposed cylinders between 56 and 365 days. The strength of the exposed cylinders is 54% and 41% less than bath and sealed cylinders strengths, respectively, at 365 days. Strength retrogres- sion of AASC cylinders subjected to exposed curing has not been reported previously in the literature. 4. Surface microcracking AASC cylinders that were exposed to 23°C and 50% RH from Day 1 onwards developed visible surface F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352 347
  • 4. crazing cracks, or microcracking (Fig. 2). The cause of microcracking may be due to the very dry condition of the surface concrete, as evidenced by zero measured bleed [8], and also restraint of shrinkage-prone AASP by rigid basalt coarse aggregate. The cylinders that were cured under sealed and bath conditions showed no vis- ible surface microcracking. The crack frequency (number of cracks per sample) for at 3, 7, 28, and 56 days is summarised in Fig. 3. The results show that the majority of microcracks occur within the ®rst three days and are mostly of the size 0.01 mm. The frequency of the 0.01-mm crack size reaches a maximum at 7 days followed by crack width growth. The widths of the microcracks are as high as 0.3 mm. Hsu et al. [15] showed that microcracks exist at the interface between coarse aggregate and mortar before any load is imposed, and the microcracks are caused by mortar volume changes. AASC shows signi®cantly greater shrinkage strains than OPCC when subjected to drying conditions [8] and it is likely that the restraint provided by the sti€ basalt coarse aggregate and the high shrinkage of the AASP has lead to microcracking under drying conditions. Meyers et al. [23] and Ravindrarajah and Swamy [25] have shown that the microcrack density increases with the magnitude of drying shrinkage. High shrinkage of the paste can lead to interconnected mi- crocracks, as shown by Sicard et al. [29], in the case of very high strength concrete, due to desiccation. In the case of repairs to reinforcement corrosion damaged concrete, Collins and Roper [7] showed that the depth of the zone of microcracking, observed near the repair mortar to concrete substrate interface, had a strong in¯uence on the soundness of the repair. Carrasquillo et al. [6] asserts that the development of combined mi- crocracks is an essential step in the progression toward impending failure. Following microscopic examination, Malolepszy and Deja [21] observed negligible microcracks on 7-day water cured AASM, however, when the same samples were subsequently exposed to 65% RH and 20°C, mi- crocracking was observed. Byfors et al. [5] also observed microcracking on AASC and, following microscopic examination, concluded that the frequency was greater following exposed curing and this lead to reduced ¯ex- ural strength. Cracking is more frequent and intense for concrete with binders composed of alkali activated slag than OPC and slag blended cements [11] and with in- creased activator content [12]. At low aggregate/cement ratio the microcracks become long and continuous [10]. Kutti and Malinowski [18] and Kutti et al. [19] conclude that the microcracking is due to the formation of an unstable (during drying) gel phase within the activated slag paste. During drying, a number of breaks in the particle to particle bonds throughout the gel structure occur thereby forming microcracks in the paste. Ha- kkinen [14] showed that microcracking is most pro- nounced within the zone of drying and that 150-mm diameter cylinders, which have a smaller proportion of the cross-section a€ected by surface drying and hence Fig. 2. Microcracks on AASC exposed to 50% RH and 23°C from Day 1 onwards. Fig. 3. Microcrack frequency of AASC exposed to 50% RH and 23°C from Day 1 onwards. Fig. 1. E€ect of type of curing on compressive strength, AASC, w=b ˆ 0:5. 348 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
  • 5. microcracking, show greater compressive strength than 100-mm diameter cylinders. 5. Pore size distribution It is well established that blended slag cement binders have a ®ner pore size distribution than OPC binders [9,22,27,20,26,28,35]. AAS is sensitive to the type of curing. When sub- jected to air curing, however, alkali activated slag binder has higher number of pores in the 100±10,000 nm range than OPC binder [1,10,12,13]. Hakkinen et al. [10] showed that as hydration proceeds, under drying con- ditions, activated slag binder has an increasing number of pores within the 1000±10000 nm range, whereas the number of pores for OPC binder remains constant. The cause of increasing porosity within the 1000±10000 nm range is microcrack development [12,13]. Fig. 4 shows the cumulative pore size distributions for bath cured AASP with w=b ˆ 0:5. At one day, the pore size distribution of AASP is coarse. From 1 to 3 days, there is a signi®cant shift towards a ®ner pore size distribution. The results show increasing pore re®ne- ment with increasing age. Fig. 5 shows the cumulative pore size distributions for sealed cured AASP with w=b 0.5. The pore size distributions are very similar to the bath cured results shown in Fig. 4. The bath and sealed paste samples that were under test were taken from the centre (interior) of the sample. However, microcracking was visible on the surface of the exposed AASP samples and therefore MIPS testing was also undertaken at the outside and midway between the centre and outside of the sample. Fig. 6 shows cu- mulative pore size distribution of exposed AASP at 3, 7, 28, and 56 days. Fig. 6 shows signi®cantly coarser pore size distribu- tion at the exterior and interior locations than bath and sealed cured specimens shown in Figs. 4 and 5, dem- onstrating the e€ects of lack of curing. The pore size distribution becomes coarser with distance towards the exterior of the sample, however the total porosity at 3, 7, and 28 days is very similar for all sample locations. At 56 days, the exterior pore size distribution is signi®cantly coarser and the total porosity higher than at the internal sample location and this is re¯ected by cessation of growth of compressive strength for concrete tested at the same age. Table 3 shows the proportion of pores within the mesopore, macropore, and voids/microcracks for AASP, based on the IUPAC [16]. There is a higher proportion of pores within the voids/microcracks pore size region up to 28 days. Many of the microcracks that were identi®ed and discussed above are too large to be measured by MIPS and hence are not shown in Table 3. Samples of 365 day AASC from standard cylinders that were subjected to bath, sealed, and exposed curing were tested by MIPS and the cumulative pore size dis- tribution for concrete subjected to each of the curing types is shown in Fig. 7. The pore size distributions of bath and sealed cured AASC are almost identical. This is despite the di€er- ences that were measured in compressive strength. Ex- posed AASC has considerably coarser pore size distribution than both bath and sealed cured AASC. For the exposed sample taken from the interior of the cylinder, the total porosity is almost the same as the bath and sealed cured samples. However, in the case of the exposed sample taken from the exterior, the total porosity is 3.67% greater than the sample taken from the interior of the exposed cylinder. Although there is likely to be errors introduced by aggregate contamination in the sample, the e€ect of microcracking on the pore size distribution is evident in the exposed samples. Fig. 4. Cumulative pore size distribution of bath cured AASP, w=b ˆ 0:5. Fig. 5. Cumulative pore size distribution of sealed cured AASP, w=b ˆ 0:5. F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352 349
  • 6. 6. Water sorptivity Fig. 8 shows that following exposed curing AASC has increasing water sorptivity at ages beyond 3 days, indi- cating the existence of a network of interconnected mi- crocracks within the sample that become progressively larger and continuous with increasing age. This indicates that the interconnected network of microcracks is a likely explanation for lower compressive strength of AASC following exposed curing. Fig. 8. E€ect of curing on water sorptivity. Fig. 6. Cumulative pore size distribution of exposed cured AASP, w=b ˆ 0:5. (a) 3 days, (b) 7 days, (c) 28 days, (d) 56 days. Fig. 7. Cumulative pore size distribution of bath, sealed, and exposed curing for 365 days. Table 3 Pore size proportions for AASP Age (days) % Mesopores (1.25±25 nm radius) % Macropores (25±5000 nm radius) % Voids/microcracks (5000±50,000 nm radius) 3 74.0 16.6 9.4 7 76.0 14.9 9.1 28 82.0 10.4 7.6 56 81.3 12.5 6.2 350 F. Collins, J.G. Sanjayan / Cement & Concrete Composites 23 (2001) 345±352
  • 7. 7. Conclusions The compressive strength is almost identical when comparing bath cured AASC cylinders with sealed cured cylinders for w=b ˆ 0:5. The laboratory exposed (23°C and 50% RH) cylinders have 41.4% and 53.5% lower compressive strength at 365 days than sealed and bath cured cylinders, respectively. Between 28 and 365 days the exposed cured cylinders show 17.2% strength loss. Exposed AASC showed visible surface microcracks. The majority of microcracks occur within the ®rst 3 days and are mostly of the size 0.01 mm. The frequency of the 0.01-mm crack size reaches a maximum at 7 days fol- lowed by crack width growth. The widths of micro- cracks are as high as 0.3 mm. The e€ect of microcracking on exposed AASC samples were evident by considerably higher total porosity and coarser pore size distribution that was measured by MIPS testing.The pore size distribution of exposed AASP is more porous than bath and sealed samples, with the po- rosity increasing with distance towards the exterior of the sample. Following exposed curing, AASC shows that visible microcracking on the surface and water sorptivity testing showed the samples to have high uptake of water compared with bath and sealed cured companion cylin- ders. The high uptake of water can be associated with a continuous microcracking and capillary network, which has lead to inferior compressive strength. This shows that should AASC be used for construction it is imperative that the concrete is well cured. Acknowledgements The ®nancial support for this project is jointly pro- vided by Independent Cement and Lime Pty Ltd., Blue Circle Southern Cement Ltd. and Australian Steel Mill Services. The authors thank the sponsors, especially Alan Dow, Tom Wauer, Katherine Turner, Wayne James, Paul Ratcli€, John Ashby, and Dr. Ihor Hinczak for the guidance and support. The enthusiastic participation of ®nal year student Dennis Kueh in this project is very much appreciated. The e€orts and assistance with the labora- tory work provided by Je€ Doddrell, Roger Doulis, and Peter Dunbar are also gratefully acknowledged. References [1] Anderson R, Gram H-E. Properties of alkali-activated slag. In: Anderson R, Gram H-E, Malolepszy J, Deja J, editors. Alkali- activated slag. Swedish Cement and Concrete Institute Report 1.88; 1988. p. 9±65. [2] Bamforth PB, Pocock DC, Robery PC. The sorptivity of concrete. In: Proceedings of the International Conference on Our World in Concrete and Structures, Singapore, 1985 August 27±28. p. 1±33. [3] Butler WB, Ashby JB. The in¯uence of curing environment upon the properties of concrete made using a variety of Portland cement supplements. 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