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Unsaturated Capillary Flow within Alkali Activated

Slag Concrete
Frank Collins1 and Jay Sanjayan2

Abstract: Alkali activated slag concrete 共AASC兲, based on a binder that consists of 100% blast furnace slag that is activated by an
alternative alkali to conventional Portland cement, has considerable environmental benefits. Nevertheless, the durability of the exposed
surface zone of AASC needs consideration. The ingress of harmful agents is highly influenced by convection-induced effects; e.g.,
moisture gradients caused by exposure to rainfall or the wetting and drying effects in the splash zone of a marine environment that can
lead to high surface concentration of chloride. The convective effects also propagate steel reinforcement corrosion, once initiated, by
making available moisture and oxygen for the cathodic reaction at the steel reinforcement, as well as changing the conductivity of the
concrete surface zone. This paper reports the behavior of convection-induced uptake of water into AASC and ordinary Portland cement
concrete. The sensitivity to “exposed,” “sealed,” and “bath” curing and the resultant pore structure for concrete made with different
water/binder is contrasted.
DOI: 10.1061/共ASCE兲0899-1561共2008兲20:9共565兲
CE Database subject headings: Slag; Binders, materials; Unsaturated flow; Porous media; Concrete durability; Material tests.

Introduction with both bath and sealed cured AASC 共Fig. 1兲. Although past
investigations on AASC have assessed various types of durability
Ground granulated blast furnace slag 共GGBFS or “slag”兲 is often 共Bakharev et al. 2001; Malolepszy and Deja 1991; Byfors et al.
used in concrete as a supplementary cementitious material, 1989; Hakkinen et al. 1987兲, whether microcracking of AASC
whereby part of the ordinary Portland cement 共OPC兲 is replaced adversely affects durability of AASC, particularly unsaturated
by slag. The environmental benefits of using slag for concrete flow of capillary water, has not been previously assessed.
making are considerable: the construction industry not only The durability of the cover zone of concrete is often compro-
makes use of a by-product from steel making, but also reduces the mised by physical and chemical interaction with the external en-
CO2 emissions arising from the manufacture of cement 共Mehta vironment. Where the concrete is unsaturated and there is no
external water pressure acting on a concrete surface, the primary
1989兲. When used as partial replacement 共by mass兲 to OPC, slag
mechanisms of transport into concrete are convective-diffusion
blended cement shows sensitivity to a lack of water curing and
ingress 共e.g., the uptake of water due to capillary attraction兲. Cap-
has lower early-age strength compared to companion concretes
illary attraction of water contributes significantly to inflows by the
made with 100% OPC binders 共Hooton 2000; Swamy and
water phase as well as water-borne media 共for example, chlo-
Bouikni 1990; Wainwright 1986; Roy and Idorn 1982兲. To over-
rides兲. The convective transport mechanisms also contribute to
come the deficit in early age strength, slag can be activated by an
the propagation of corrosion, once initiated, by making available
alternative alkali to OPC; namely an alkali activated slag 共AAS兲.
moisture for the cathodic reduction of oxygen in the corrosion
In this paper, the activator studied consists of a sodium silicate
process as well as lowering the conductivity of the concrete. This
based alkali 共Collins and Sanjayan 2000b兲. AAS activated by so- investigation has sought to assess the effect of capillary suction
dium silicate is very sensitive to the curing environment 共Collins on the uptake of moisture within the cover zone of AASC.
and Sanjayan 2001; Collins 1999; Talling and Brandstetr 1989;
Anderson and Gram 1988; Malolepszy and Deja 1988; Kutti and
Malinowski 1982兲. The high sensitivity of AAS concrete 共AASC兲
Convective Transport in Unsaturated Conditions
to the type of curing has been shown to affect compressive
strength; Collins and Sanjayan 共2001兲 observed microcracking Concrete is a porous material and most field-exposed concrete is
and lower compressive strength on air-cured concrete compared partially saturated with water. Depending on the function and
characteristics of the concrete and the amount of external expo-
1
Senior Lecturer, Dept. of Civil Engineering, Monash Univ., Clayton, sure, a moisture/humidity gradient exists from the outer exposed
Victoria 3800, Australia. E-mail: frank.collins@eng.monash.edu.au skin of concrete to the inner core. In unsaturated conditions,
2
Associate Professor, Dept. of Civil Engineering, Monash Univ., where there is no applied external pressure head of water to an
Clayton, Victoria 3800, Australia. exposed concrete surface, but nevertheless a constant source of
Note. Associate Editor: Clarissa F. Ferraris. Discussion open until
water in contact, capillary suction is the convective transport
February 1, 2009. Separate discussions must be submitted for individual
papers. The manuscript for this paper was submitted for review and pos- mechanism that permits the ingress of water from the external
sible publication on November 20, 2007; approved on February 7, 2008. environment. Surface tension arises at the solid–liquid–gas inter-
This paper is part of the Journal of Materials in Civil Engineering, Vol. faces leading to spreading of water over the concrete surface and
20, No. 9, September 1, 2008. ©ASCE, ISSN 0899-1561/2008/9-565– inward within capillary pores. Water spreads along the capillary
570/$25.00. surfaces, forming a meniscus that is convex toward the wet side

JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / SEPTEMBER 2008 / 565


Table 1. IUPAC Pore Size Classification 共Adapted from McNaught and
Wilkinson 1997兲
Pore description Radius 共nm兲
Micropores ⬍1.25
Mesopores 1.25–25
Macropores 25–5,000
Entrained air voids, entrapped air voids, preexisting 5,000–50,000
microcracks

Fig. 1. Microcracks on AASC exposed to 50% RH and 23° C from


Pore Size and Capillary Attraction
Day 1 onwards
Pore sizes have been previously classified according to The Inter-
national Union of Pure and Applied Chemistry 共IUPAC兲 system
共Philip 1957; Richards 1931; Washburn 1921; Young 1805兲. 共McNaught and Wilkinson 1997兲, as summarized in Table 1. The
Modeling of capillary uptake of water in unsaturated concrete capillary pores that facilitate water movement by capillary tension
has been undertaken previously 共Tasdemir 2003; Razak et al. comprise both the mesopores and macropores, whereas the mi-
2004; Lampacher and Blight 1998; Hall 1977; Hall and Tse 1986; cropores are of radius too small to permit water movement unless
Winslow et al. 1994; Parrott 1992; Hanzic and Ilic 2003; Bam- water pressure is applied externally. Past investigations have
forth et al. 1985; Claisse et al. 1997; Volkwein 1993; Martys and shown the pore size distribution of slag–OPC blended cements
Ferraris 1997兲. The cumulative absorbed volume of water per unit becomes finer with increasing slag content 共Gjorv and Vennesland
area of the inflow surface 共m3 / m2兲, i, increases linearly with in- 1979; Shattaf et al. 2001兲. The use of slag as a cement replace-
crease of the square root of the elapsed time, t. The assessment ment material improved the characteristics of the pore structure
can be simplified by measurement of one-dimensional water up- when appropriate water curing was carried out. In the case of
take through initially dry concrete, assuming the pores are circu- AAS, the proportion of pores in the micropore size range tends to
lar, and deriving a sorptivity coefficient, S. The sorptivity be higher than OPC 共Collins 1999; Collins and Sanjayan 2000a兲.
coefficient, S, is commonly expressed as follows 共Hall and Tse
1986兲:
Experimental Program
S = i/tx 共1兲
Concrete Mixtures
where i⫽hydraulic diffusivity; Q / A 共Wt − Wd兲 / A; measured ex-
perimentally at designated test time intervals; Q⫽amount of The chemical composition and physical properties of the cemen-
water adsorbed 共mm3兲; A⫽cross section of specimen that was in titious binders used in this study are summarized in Table 2. The
contact with water 共mm2兲; t⫽time 共min兲; x = 0.5, generally for binders used are alkali activated ground granulated blast furnace
concrete, however in cases where either scaling or leaching oc- slag 共slag兲 and OPC conforming to the requirements of the Aus-
curs and the pore structure becomes modified, 0.25⬍ x ⬍ 0.5 can
occur 共Martys and Ferraris 1997兲; and S⫽sorptivity coefficient of
the specimen 共mm/ min0.5兲; the least squares fit of the 共i versus tx兲 Table 2. Properties of Cementitious Materials
line. Constituent/property Slag OPC
Water uptake is not completely due to capillary rise. Eq. 共1兲 is
SiO2 共%兲 35.04 19.9
based on moisture uptake within parallel tubes whereas capillaries
Al2O3 共%兲 13.91 4.62
within concrete are more random and have a complex pore sur-
face topology. External factors can be expected to influence the Fe2O3 共%兲 0.29 3.97
height of capillary rise, including, e.g., variable cross-section MgO 共%兲 6.13 1.73
shape, surface roughness, tortuosity of capillary pores, random CaO 共%兲 39.43 64.27
meeting, and divergence with adjacent pores. Specimen dimen- Na2O 共%兲 0.34 —
sions and maximum aggregate size of the concrete mix can cause TiO2 共%兲 0.42 —
scaling errors: arising from overinfluence of the coarse aggregate K2O 共%兲 0.39 0.57
共as a barrier兲 and the aggregate-paste transition zone 共as a more P2O5 共%兲 ⬍0.1 —
permeable path兲 on the measured water movement through the MnO 共%兲 0.43 —
test sample. Water entry is complicated by cracks and fractures in Total Sulfur as SO3 共%兲 2.43 2.56
the concrete; however Samaha and Hover 共1992兲 showed that, Sulfide Sulfur as S2− 0.44 —
although load-induced microcracks increased the overall porosity, Cl 共ppm兲 80 —
load levels up to 75% of ultimate compressive strength did not Fineness 共m2 / kg兲 460 342
affect the overall mass transport properties of concrete, whereas Loss on ignition 共%兲 1.45 2.9
oven-drying curing caused significantly higher water flow. Roels
Time to initial set 共h兲 N/A 2.0
et al. 共2003兲 considered the microcracks as part of the primary
Strength 共MPa兲 of 75⫻ 75⫻ 75 mm mortar 32.7
porosity, however the fractured cementitious matrix resulted in a cubes 共MPa兲
retardation rather than acceleration of the waterfront within the
3 days N/A 42.0
fracture itself. Despite the many influencing factors, the rate of
7 days 54.1
the uptake of water by capillary attraction provides a useful indi-
28 days
cation of the pore continuity of concrete.

566 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / SEPTEMBER 2008


Table 3. Summary of Concrete Mixture Proportions 共kg/ m3兲
Mixture designationa
AASC/ AASC/
Constituents OPCC AASC 0.45 0.33
OPC 360
Slag 360 400 500
Sodium silicate 66.9 74.4 92.9
Lime slurry 14.4 16 20
Free waterb 180 180 180 165
w/b 0.5 0.5 0.45 0.33
Fine aggregate 830 830 630 610
Coarse aggregate 共14 mm兲 1,130 1,130 1,310 1,260 Fig. 2. Compressive strength of bath, sealed and exposed cured
a
AASC⫽slag activated by powdered sodium silicate and lime slurry. The AASC, and reference OPCC; w / b = 0.5
lime slurry was composed of 1:3 共hydrated lime:water兲.
b
Adjustments made for water in aggregates 共to saturated surface dry con-
dition兲 and activator. Water Sorptivity Testing
Following curing for 1, 3, 7, 28, 56, 91 days, two cylinders were
tralian Standards AS 3582.2 and AS3972. The term water/binder tested for compressive strength and the remaining cylinders for
共w / b兲 ratio is used instead of the conventional water/cement ratio water sorptivity. Sorptivity tests were based on the procedure of
to include both the binders mentioned previously. The slag was Bamforth et al. 共1985兲. Scaling errors, as discussed in relation to
supplied with preblended gypsum 共2% SO3兲. The activators and Eq. 共1兲, were minimized by attention to sample dimensions and
adjuncts used in AASC were powdered sodium silicate and hy- environmental conditioning prior to and during testing. The ratio
drated lime. of sample diameter to maximum coarse aggregate size was 7.14.
The dry powdered sodium silicate activator was preblended Although the coarse aggregate and the aggregate-paste transition
with the slag in the dry form prior to use for concrete manufac- zone will influence the measured water uptake, it was considered
ture. Earlier mix trials with AASC 共Collins and Sanjayan 1999兲 the scaling errors would be acceptable provided that aggregate
verified the initial workability and strength was similar to OPC size/sample diameter was kept above 3.0. The test surface, where
concrete. The slag–activator reaction was not immediate and water–sample contact was made during testing, was fabricated as
AASC maintains better extended workability for 120 min, most smooth as possible 共particularly around the circumference兲 to
likely because the powdered sodium silicate has a slower release avoid undue water uptake. A key influencing factor on capillary
of alkali into the cement system 共as opposed to liquid sodium absorption is the moisture content of the concrete samples at the
silicates兲 that leads to a slower rate of initial reaction. The coarse time of testing. Following curing, the test samples were dried
aggregate consisted of 14 mm maximum size basalt with a spe- until constant weight was achieved at 23° C in a desiccator. The
cific gravity of 2.95 and 24 h water absorption of 1.2%. The fine dried weight, Wd, at 23° C was measured prior to testing. One test
aggregate consisted of river sand with a specific gravity of 2.65, face of each sample was placed on glass rods with the test face in
24 h water absorption of 0.5%, and a fineness modulus of 2.19. contact with 1 – 2 mm depth of water. The laboratory conditions
The concrete mixture proportions are summarized in Table 3. were kept at 25⫾ 2 ° C and 75⫾ 5% RH. The uptake of water,
Three different w / b ratios were made with AASC: 0.5, 0.45, and registered as vertical height rise and weight gain, was determined
0.33. A reference OPC concrete 共OPCC兲 mixture was made with over 4 h, with measurements undertaken at 5, 15, 30, 60, 120, and
w / b = 0.5. The materials used for concrete making, the method of 240 min from the time of commencement of the test. To deter-
preparing concrete mixtures in the laboratory, and the tests for mine the sorptivity coefficient of the samples under test, the hy-
fresh and mechanical concrete properties reported in this paper draulic diffusivity of water, 共Wt − Wd兲 / A, was plotted versus
were in accordance with the Australian Standard AS1012. time0.5 and the sorptivity was derived as the best-fit slope of the
linear relation.
Sample Manufacture and Curing
Samples were made for subsequent laboratory testing as follows: Results
Test cylinders made in accordance with Australian Standard
AS1012, Parts 8 and 9 共100 mm diameter and 200 mm height兲.
Compressive Strength
Following demolding, the cylinders were subjected to one of
three curing regimes: bath, exposed, or sealed. The definitions of The exposed samples showed visible surface microcracking that
the curing regimes are: may have contributed to significantly lower strength than the
1. Bath—immersed in saturated lime water at 23° C; sealed cured and bath cured samples 共Fig. 1兲. The majority of
2. Sealed—specimen is storage in two polythene bags and a microcracks occurred within the first 3 days and were mostly of
sealed container so that no moisture movement in or out of the size 0.01 mm. Collins and Sanjayan 共2001兲 reported strength
the specimen, the specimen temperature was maintained at retrogression of exposed cured AASC following 365 days expo-
23° C; and sure. Figs. 2–4 show strength development for different w / b fol-
3. Exposed—air exposed at 50% relative humidity 共RH兲 and lowing bath, sealed and exposed curing. AASC samples subjected
23° C. to exposed curing reached peak strength at approximately 56
Three samples from each curing exposure type were withdrawn days, whereas the OPCC reference mixture with w / b 0.5 共Fig. 2兲
for subsequent testing. had significantly higher strength development at later ages than

JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / SEPTEMBER 2008 / 567


Fig. 3. Compressive strength of bath, sealed and exposed cured Fig. 5. Water sorptivity versus age; bath curing
AASC; w / b = 0.45

more tortuous, and the resulting uptake of water by capillary at-


companion AASC 共22% higher strength at 56 days兲. In all cases traction becomes less. However, when comparing OPCC with
the strength of sealed cured cylinders is lower than bath cured, as AASC 共comparative data only for w / b of 0.5兲, the AASC/0.5 has
expected. Bath cured AASC shows almost identical strength to significantly higher sorptivity than OPCC/0.5, despite identical
OPCC at all ages. bath curing. This is in contrast with almost identical compressive
strength AASC and OPCC when cured under bath conditions. A
Hydraulic Diffusivity „i… versus Time0.5 likely explanation is that bath cured AASC is very sensitive to the
preconditioning immediately prior to the sorptivity test: oven stor-
The results showed a significant linear relationship for hydraulic age at 105° C until constant weight was achieved and then al-
diffusivity 共i兲 versus time0.5, even in the case of exposed AASC lowed to cool to 23° C in a desiccator. The preconditioning has
that had significant microcracking. The calculated R2 of the re- most likely had a damaging effect with respect to the generation
gression of all 82 samples 共6 data points per sample兲 was within of microcracks that have led to higher capillary uptake of water.
the range 0.91–0.98, indicating a strong linear relationship be- Following sealed curing 共Fig. 6兲, AASC shows higher water
tween i versus time.0.5 This follows earlier published results 共Hall sorptivity that companion bath cured samples and this reflects the
1977; Hall and Tse 1986兲. Past work by Martys and Ferraris slightly better pore refinement following bath curing. AASC with
共1997兲 and Lampacher and Blight 共1998兲 showed that i versus w / b 0.5 is significantly higher than comparable OPCC and has
time0.5 ceases to be linear at ages greater than 375 min 共or, time0.5 31% higher sorptivity at 56 days. When sealed cured OPCC/0.5
greater than 19.36 mm/ min0.5兲; in our investigation the test dura- retains very similar sorptivity to companion bath cured OPCC/
tion has been conducted well within the expected linear portion of 0.5. Similarly to the bath cured samples, AASC/0.33 and OPCC/
the i versus time0.5 relationship, however, the previous literature 0.5 had very similar water sorptivity at all ages, despite the
has not dealt with AAS binders. significant difference in w / b.
The most significant differences between AASC and OPCC
Water Sorptivity, Water/Binder Ratio, and occur between exposed samples, as shown in 共Fig. 7兲. All samples
Type of Curing show higher sorptivity than either sealed or bath cured samples
due to ongoing loss of concrete moisture leading to inferior hy-
The test results are summarized in Figs. 5–7. Following bath cur- dration of the cementitious components. AASC with w / b 0.5 has
ing, AASC, shows progressively lower sorptivity with increasing up to 81% higher sorptivity than companion OPCC samples that
age, as expected for well-cured concrete 共Fig. 5兲. As w / b of were bath cured. AASC with w / b 0.45 also shows high, but not as
AASC decreases, water sorptivity decreases, lower w / b and cur- significant difference, to AASC with w / b 0.5. The extensive mi-
ing within bath conditions provides ongoing hydration of the crocracking shown in Fig. 1 for AASC with w / b 0.5 and has
paste and a pore structure that becomes finer, less continuous and obviously been a major contributor to the higher water sorptivity.
At ages beyond three days, the increasingly higher water sorptiv-

Fig. 4. Compressive strength of bath, sealed and exposed cured


AASC; w / b = 0.33 Fig. 6. Water sorptivity versus age; scaled curing

568 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / SEPTEMBER 2008


due to a more continuous and open pore structure that is
assisted by microcracks. This situation is worse if exposed
curing is implemented instead of sealed or bath curing.
3. If AASC is to be used for construction purposes it is impera-
tive that good curing is undertaken.
4. AASC is vulnerable in service environments subject to high
ambient temperatures and drying conditions.

Acknowledgments

The financial support for this project is jointly provided by Inde-


pendent Cement and Lime Pty Ltd., Blue Circle Southern Cement
Fig. 7. Water sorptivity versus age; exposed curing Ltd., and Australian Steel Mill Services. The writers thank the
sponsors, especially Alan Dow, Tom Wauer, Katherine Turner,
Paul Ratcliff, John Ashby, and Dr. Ihor Hinczak for the guidance
ity indicates a more advanced network of interconnected micro- and support. The enthusiastic participation of final year students
cracks within the sample that have become progressively larger Soon Keat Lim and Eric Tan in this project is very much appre-
and more continuous with ongoing duration of exposed curing. ciated. The efforts and assistance with the laboratory work pro-
AASC with w / b 0.33 has similar sorptivity to OPCC with w / b vided by Jeff Doddrell, Roger Doulis, and Peter Dunbar are also
0.5. gratefully acknowledged.

Conclusions References

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