Construction and Building Materials: I. Yurtdas, D. Chen, D.W. Hu, J.F. Shao

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Construction and Building Materials 47 (2013) 165–174

Contents lists available at SciVerse ScienceDirect

Construction and Building Materials


journal homepage: www.elsevier.com/locate/conbuildmat

Influence of alkali silica reaction (ASR) on mechanical properties


of mortar
I. Yurtdas a,⇑, D. Chen b, D.W. Hu c, J.F. Shao b,c
a
LGC, GRESPI, EA4694, University of Reims, Reims, France
b
University of Hohai, Nanjing, China
c
LML, UMR8107 CNRS, University of Lille I, Villeneuve d’Ascq, France

h i g h l i g h t s

 Mechanical and hydraulic properties of ASR affected mortar are studied. ASR process at 60 °C and 95% RH lasts 100 days.
 After ASR, the increase in compressive strength of reactive mortar is more significant than that of non-reactive one.
 The densification of ITZ could mostly explain the higher increase of reactive mortar strength.
 Bending strength and elastic properties are more affected by ASR induced microcracking.
 Permeability and porosity measurements can provide useful data for the evaluation of ASR induced microcracking.

a r t i c l e i n f o a b s t r a c t

Article history: This experimental investigation deals with effects of ASR on the mechanical properties of cement-based
Received 29 June 2012 materials. Two selected mortars, only differentiated by the chemical nature of the aggregates used (reac-
Received in revised form 19 April 2013 tive and non-reactive) are investigated. After a maturation period of 28 days, triaxial compression tests
Accepted 28 April 2013
with different confining pressures (0, 5, 15 MPa), bending tests, porosity and permeability measurements
Available online 3 June 2013
are carried out on a part of the samples in order to obtain a reference state as the sound material while
the other part is stored in a controlled environment with temperature of 60 °C and relative humidity of
Keywords:
95% for ASR development. During this period of storage, the axial expansion of samples for the two mor-
Alkali silica reaction
Mortar
tars studied is monitored. After 100 days of storage in the controlled environment, the above cited tests
Microcracking and measurements are performed again in order to evaluate the effects of ASR. In addition, microstruc-
Triaxial compression tural analyses are also carried out in order to better understand various phenomena which occur in mor-
Mechanical properties tars before and after storage of samples in controlled environment. It is found that the increase of
Transport properties mechanical strength under compression is more significant in the reactive mortar than in the non-reac-
Microstructure tive one. This can be attributed mainly to its more compact microstructure in the ITZ, shown by the
microstructural analyses, compared with the non-reactive mortar. However, the ASR process induces a
decrease of bending strength, which is directly related to tensile strength, in reactive mortar. Moreover,
the elastic modulus and Poisson’s ratio of the reactive mortar decrease due to the ASR process. These
results indicate that the tensile strength and elastic properties are more significantly affected by the
ASR expansion related microcracking than the compressive strength. The microcracking due to the ASR
is also detected through the permeability and porosity measurements.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction microcracks. The gels fill the microcracks in the aggregates and
paste as well as the voids. The extent of the ASR induced
Alkali silica reaction (ASR) is one of the degradation process and deterioration is influenced in particular by the reactivity (moder-
refers to chemical reaction between the reactive silica phases in ately or highly) [1–3,5,8,9], quantity, size and particle size distribu-
the aggregates and the alkali hydroxides in the pore solution of tion of the reactive aggregates [1–3,6,8,10–14], the amount of
cement-based materials [1–8]. The reaction results in the forma- available moisture [1–4,13,15,16], amount of available alkalis
tion of alkali-silica gels and/or alkali–calcium–silica gels. These [1–3,8,10,12,15], porosity of material and pre-existence of micro-
gels which absorb water and swell can lead to the formation of cracks [1–4,15].
Many studies have been carried out in order to evaluate the
⇑ Corresponding author. Tel.: +33 326918052. mechanical performances of ASR affected concrete. For this
E-mail address: ismail.yurtdas@univ-reims.fr (I. Yurtdas). purpose, uniaxial compression and tension tests are generally

0950-0618/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2013.04.046
166 I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174

performed. Some authors reported a decrease in the uniaxial Table 1


compressive strength of concrete [17–21] whereas others did not (a) Mortar composition, and (b) aggregate size grading of sands.

observe such a diminution due to the ASR related expansion Components Quantity [kg/m3]
[16,22–24] over the period of experimental study. The uniaxial (a)
compressive strength of concrete decreases in particular when Sand (inert or reactive) 1613
the aggregates are highly reactive [5,9,25]. Further, the cores taken Cement CEM I 52.5 R 538
from ASR affected structures can have high residual uniaxial com- De-ionised water 269
Total alkali in mortar 15
pressive strength [20,21], especially at early age of ASR develop-
ment [20]. It seems that the uniaxial compressive strength of Aggregate diameter [mm] Aggregate fraction [%]
(b)
ASR affected concretes continues to increase or does not vary com- 0.08–0.16 25
pared with 28 day compressive strength in particular when the 0.63–1.25 50
aggregates are slowly or moderately reactive [5,9,25]. However, 2.5–4 25
whether the uniaxial compressive strength increases or not during
the development of the alkali silica reaction, a clear degradation of
elastic modulus is observed [2,3,5,9,16,17,22,23,25] and the mate- mortar) was fabricated with an inert crushed limestone sand while the reactive
rial becomes more deformable [9,17,22,24]. The elastic modulus is mortar (designated as R mortar) was fabricated with a reactive crushed siliceous
thus very sensitive to the ASR induced damage, and decreases even limestone sand [6,13]. The mortars were fabricated with specific sand grains com-
posed of only three different grain-size fractions: fine aggregates with an equivalent
if the aggregates are slowly or moderately reactive. This sensitivity
diameter between 0.08 and 0.16 mm; medium aggregates with an equivalent diam-
is also reported for the direct tensile strength, which decreases eter between 0.63 and 1.25 mm and coarse aggregates with an equivalent diameter
drastically with the ASR expansion [5,18,19]. The evolution of the between 2.5 and 4 mm. For each mortar, the sand grains were composed of 25% of
concrete flexural strength also seems to be affected by the ASR fine aggregates, 50% of medium aggregates and 25% of coarse aggregates (Table 1b).
[5,9,19,22,25]. It is also observed that a high strength concrete These fractions were obtained by sieving; the sands were then washed to be dis-
posed of very fine particles and dried before use. CEM I 52.5 R with a high alkali con-
has a better resistance than an ordinary strength concrete against
tent of 1.11% Na2Oeq and demineralised water were used to cast the mortars. The
the harmful effect of the ASR damage [5]. Therefore, these results alkali content was increased to 15 kg/m3 by adding NaOH to the mixed water.
show that the ASR does not influence in the same way all of the Prismatic (40  40  160 mm3) and cylindrical (£ 36  100 mm3) samples
mechanical properties. It is found that the good indicators of the were prepared for this study. The prismatic samples were used for the monitoring
of length variation in order to determine the expansion of material. The bending
quality of the ASR damaged concrete are the elastic modulus and
tests were also performed on prismatic samples. The cylindrical samples were used
the tensile strength (in particular direct tensile strength). Note that in uniaxial and triaxial compression tests, and in permeability and porosity
the simple increase in the alkali content alone leads to a drop of the measurements.
mechanical properties of concrete without reactive aggregates Three days after the casting, the samples are de-moulded and kept in sealed
[26]. This phenomenon should also be taken into account in the bags for 28 days at ambient temperature. During this period of conservation, the
cylindrical samples were sliced to obtain smaller samples for various tests. This
evaluation of the mechanical degradation by ASR.
operation was done under dry conditions in order to avoid any leaching of alkalis
Most concrete structures can also be subjected to multi-axial [13]. After 28 days of maturation, a part of the samples were stored in a tempera-
mechanical loading during their service life. The effect of applied ture and humidity controlled chamber with temperature of 60 °C and relative
stresses on ASR development should be underlined [16,24,27]. humidity (RH) of 95% for ASR development. According to some previous investiga-
For instance, it is reported that the volumetric expansion of con- tions [2,4,8,13,16], this intermediately high temperature can facilitate the begin-
ning and increase the initial kinetics of the ASR process.
crete generated by ASR is constant whatever the stress state along
the three directions (axial creep stress and passive restraint),
which means the occurrence of expansion transfer in the less com- 2.2. Testing program and experimental device
pressed direction [24,27]. It is also necessary to understand the
The following tests and measurements are carried out during experimental inves-
influences of ASR on the mechanical properties of materials under
tigation: three point bending tests on prismatic samples (40  40  160 mm3),
such complex loading conditions. It is also useful to characterize uniaxial (Pc = 0 MPa) and triaxial compressive tests (Pc = 5 and 15 MPa) on cylindrical
the evolution of hydraulic properties induced by ASR. The results samples (£ 36  72 mm3), permeability measurement on cylindrical samples (£
obtained will contribute to the improvement of constitutive 36  27 mm3) and porosity measurements on cylindrical samples (£
models for ASR affected materials as well as design tools for the 36  16 mm3). The three point bending tests are performed in order to evaluate ten-
sile strength of material. In the present work, we also propose to investigate the ASR
ASR affected structures. Such results will be also helpful for the effect on compressive mechanical strength. As the compressive strength of cement-
efficiency of the maintenance procedures and repair works. The based material depends on hydrostatic stress, multi-axial compressive tests are
present work is devoted to the experimental study of the evolu- needed. In practice, triaxial compressive tests on cylindrical samples are commonly
tions of mechanical and hydraulic properties of ASR affected mor- carried out to determine failure surface of geomaterials. Such tests are performed
in the present work with two different confining pressures. These tests and measure-
tar. For this purpose, two groups of mortar samples are fabricated
ments were performed respectively after a period of 28 day maturation and after
respectively with reactive and non-reactive aggregates. Triaxial 100 days of conditioning of samples at 60 °C and 95% RH. The results obtained after
compressive tests with different confining pressures (0, 5 and 28 day maturation were taken as the reference values. The change in length of sam-
15 MPa) and bending tests are performed. The expansion, porosity ples was measured during the conditioning of samples. All tests and measurements
and permeability evolution are determined. Moreover, a micro- were performed after a cooling period of samples for at least 6 h at ambient temper-
ature. The length change of the prismatic samples (equipped with stainless steel
structural analysis is also carried out by using scanning electron studs at both end) during time are measured on three samples for each mortar with
microscopy (SEM) together with Energy Dispersive X-ray Spec- a mechanical retractometer.
trometry (EDS). In the following, the experimental program is first Uniaxial and triaxial compression tests were carried out using a hydraulic press
described and then the results obtained are presented and dis- under displacement controlled condition. The axial displacement rate used is 2 lm/
s. The tests were performed with loading-unloading cycles in order to evaluate the
cussed by comparing the behaviours of the two groups of mortar.
variation of elastic properties during mechanical loading. A triaxial cell was used in
order to apply confining pressures by injection of oil into the cell. The axial strain
2. Experimental investigation was measured by LVDT while the radial strain was obtained with the help of a spe-
cial strain ring [28]. However, the radial strains could not be measured in the case of
2.1. Material composition, sample preparation and conditioning uniaxial test because of brittle failure of the samples which seriously destroy the
strain ring. The triaxial compression tests are classically conducted with two load-
The study was undertaken on two groups of mortar whose composition was in- ing phases: increase of hydrostatic pressure until the desired value (5 or 15 MPa)
spired by Poyet et al. [6,13]. The mortar samples had a water to cement ratio of 0.5 and application of the deviatoric stress by keeping the radial stress constant. The
and sand to cement ratio of 3 (Table 1a). The non-reactive mortar (designated as NR deviatoric strength is identified as the maximum (peak) deviatoric stress reached
I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174 167

0.45 Note that each mechanical, porosity and permeability test was re-
0.40 peated at least two times in the same conditions in order to be rep-
resentative. However, only the averaged data will be presented
0.35
here for the reason of clarity.
Expansion [%]

0.30 mean value of NR samples


mean value of R samples
0.25 3.1. Linear expansion of mortar
0.20
Fig. 1 shows the evolution of the average expansion of NR
0.15
mortar and R mortar. Recall that the expansion of the mortars is
0.10 monitored during the conditioning period of samples in the con-
0.05 trolled environment with 60 °C and 95% RH after 28 day matura-
0.00 tion. All measurements are performed at ambient temperature.
0 10 20 30 40 50 60 70 80 90 100 110 As expected, the expansion of the NR mortar is very weak, approx-
Time [day] imately 0.02%. In opposite, the expansion of the R mortar is signif-
icant, about 0.40% after 52 days. This means that the ASR induced
Fig. 1. Linear expansion of the NR mortar and R mortar.
expansion is about 0.38%. The expansion of NR mortar is an intrin-
sic expansion mainly due to water absorption, and reaches a max-
during the test. Three-point bending tests were carried out on prismatic samples
imum value after about 6 days. The kinetics of the expansion of the
with a loading rate of 0.1 lm/s using a specific bending system mounted on the
hydraulic press. R mortar is very high up to approximately 25 days and the expan-
Porosity and permeability, which are considered as key parameters for the sion is stabilized after 50–60 days. The higher the level of aggre-
durability analysis of concrete structures, were also studied. The mortar permeabil- gates reactivity is the higher will be the weight gain [25]. Notice
ity was measured by injection of de-aromatized oil into mortar samples. The use of that this expansion is mainly due to the presence of the medium
such fluid, which does not react with cement, is recommended to determine the
intrinsic permeability [29,30] of mortar. Samples are dried up to a constant weight
and coarse size aggregates. The presence of reactive fine aggregates
at 60 °C before testing. The permeability is determined with the steady flow regime. leads to a reduction in expansion [6,10–13]. In addition, the expan-
After the application of a confining pressure of 4.5 MPa, the oil is injected from the sion obtained by the mixture of the three fractions remains lower
bottom surface of sample under a constant pressure of 0.5 MPa. The outlet pressure than the sum of the expansions obtained for each fraction of aggre-
on the upper surface is equal to the atmospheric pressure. Assuming that the fluid
gates [6,13] (the expansion for a given reactive fraction is obtained
flow is in one dimensional condition, the axial permeability is easily calculated by
measuring the flow rate at the outlet face of the sample. The porosity of mortar is by replacing the two other fractions by non-reactive ones).
determined by simply comparing the sample mass in dried condition (at 60 °C) and
that in saturated condition under vacuum. A satisfactory drying of porous network 3.2. Microstructural characterization
is obtained with this moderate temperature but it is possible that some small pores
that can be created by ASR are not detected by this porosity measurement. It is also
possible that the ASR leads to the creation of an occluded porosity, which cannot be
The analysis of microstructure of mortar was performed using
detected by the measurement of porosity. Note that some microcracks can be in- SEM coupled with EDS. Figs. 2 and 3 show respectively the general
duced by the drying process and then affect the permeability [31] and porosity of appearance of the two materials on polished section and the details
mortar. However, in case of permeability, a part of the induced microcracks should of their matrices on fresh fracture after the maturation period. The
be closed by the application of confining pressure up to 4.5 MPa.
two mortars present a rather similar microstructure. However, the
Furthermore, microstructural characterization was also carried out on the two
groups of mortar by SEM together with the elementary microanalysis by EDS in or- sample of R mortar appears slightly more micro-porous than the
der to better understand various physical phenomena that occur in materials before sample of NR mortar. In addition, the rate of hydration is also
and after the ASR process. Polished sections and fresh fracture surfaces were ana- rather close for the two materials. Their matrices are mainly con-
lysed after the end of the experimental campaign (approximately 11 months after stituted of calcium-silicate hydrates (C-S-H) which are very often
the casting). This investigation was very useful to understand the evolution of the
mechanical behaviour induced by the ASR.
in granular form, accompanied by portlandite (Ca(OH)2), and by
some crystals of acicular ettringite often in the occluded air voids.
After the conditioning period of the samples at 60 °C and 95%
3. Experimental results and analysis RH, clear differences are observed on these two groups of samples.
It is observed that the R mortar contains gels due to ASR (Fig. 4).
This section presents the main results obtained from the exper- The elementary micro-analysis shows that the majority of these
imental investigation. The emphasis is put on the effects of ASR gels are alkali–calcium–silica gels. Fig. 4b illustrates the occurrence
process on the mechanical and hydraulic properties of mortar. of different generations of gels in an occluded air void. First, the gel

Fig. 2. General appearance (polished section, retro-diffused electrons) of NR (a) and R mortars (b) after maturation period: 1 – anhydrous clinker, 2 – aggregate, 3 – matrix in
relatively compact zone, 4 – matrix in relatively micro-porous zone.
168 I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174

Fig. 3. Detail of matrices (fresh fracture, secondary electrons) of NR (a) and R (b) mortars after maturation period: 1 – occluded air void, 2 – C-S-Hs, 3 – portlandite, 4 –
ettringite.

Fig. 4. (a) Appearance of the gel in an occluded air void in a R sample after conditioning at 60 °C and 95% RH (fresh fracture, secondary electrons): 1 – gel, 2 – cementitious
matrix, (b) detail of (a): 1 – C-S-Hs more or less impregnated by the gel, 2 – smooth gel, 3 – smooth gel, 4 – re-crystallisation of the gel.

impregnates more or less the C-S-Hs in the vicinity of the occluded to form C-S-Hs. The occurrence of this reaction and the impregna-
air wall, which leads to a decrease of the micro-porosity (1). Then tion of C-S-Hs by gels would lead to the compact facies of C-S-Hs.
the gel forms a deposit in the occluded air void where it has Overall Figs. 4–7 seem to indicate that there is a densification of
smooth facies (2). Afterwards, a last generation of gel forms a the microstructure, particularly a densification of the ITZ [32] by
deposit on the previous one (3). There is a crystallisation on the the presence of ASR gels (filling of the ITZ porosity, some impreg-
surface (4) that remains free. nation of C-S-Hs and possible reaction of the silica of gels with
Fig. 5 shows the general appearance of two materials on pol- portlandite to form the new C-S-Hs), in the R mortar.
ished section (retro-diffused electrons). The R sample presents a
relatively more compact microstructure than the NR sample. The
interfacial transition zone (ITZ) of many aggregates of NR sample 3.3. Effect of ASR on mechanical behaviour
presents a micro-porous structure (dark zones around aggregates)
whereas that of R sample is very often compact. Moreover, micro- 3.3.1. Multi-axial compression
cracks also appear in the R sample due to ASR expansion (a part of An example of the results obtained is presented in Fig. 8. This
these microcracks could be linked to the sample preparation figure shows the evolution of the axial and radial strains versus
process). However, the occurrence and the intensity of these deviatoric stress during triaxial compression tests with a confining
microcracks are not always the same for each tested sample (not pressure of 15 MPa. It can be seen that after the maturation period,
shown here). the mechanical behaviour of the NR mortar and R mortar are very
On the other hand, Fig. 6 indicates that the NR sample has a rel- close with a slightly higher deviatoric strength for the later one.
atively micro-porous matrix near an air void (fresh fracture, sec- However, important differences appear after the conditioning of
ondary electrons) while the R sample has a relatively compact samples at 60 °C and 95% RH. For the NR mortar, the deviatoric
matrix. The details of these matrices near an aggregate are shown strength increases slightly due to cement hydration and the mate-
in Fig. 7. It can be seen from Figs. 6 and 7 that the C-S-Hs appear rial behaviour becomes more brittle compared with the behaviour
often in granular and fibrous form in the NR sample and in a rather after maturation period. For the R mortar, the increase in deviatoric
compact form in the R sample. Notice that the portlandite content strength is much more important, which indicates a much more in-
in the R sample seems lower than that in the NR sample. This could tense chemical activity. Its behaviour becomes also more brittle
be due to the fact that the silica of gels reacts with the portlandite compared with the behaviour after maturation period.
I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174 169

Fig. 5. General appearance (polished section, retro-diffused electrons) of two mortars after conditioning at 60 °C and 95% RH: (a) NR sample: 1 – anhydrous clinker, 2 –
aggregate, 3 – matrix in relatively compact zone, 4 – micro-porous transition zone, (b) R sample: 1 – anhydrous clinker, 2 – aggregate, 3 – matrix in relatively compact zone, 4
– compact transition zone, 5 – microcrack.

Fig. 6. Appearance (fresh fracture, secondary electrons) of matrices of two mortars after conditioning at 60 °C and 95% RH: (a) NR sample with relatively micro porous matrix:
1 – granular C-S-Hs, 2 – portlandite, 3 – occluded air void, (b) R sample with relatively compact matrix: 1 – dense C-S-Hs, 2 – ettringite in an air void.

Fig. 7. Detail of matrices of two mortars near an aggregate after conditioning at 60 °C and 95% RH: (a) NR sample: 1 – granular and fibrous C-S-Hs, 2 – aggregate, (b) R sample:
1 – compact C-S-Hs, 2 – aggregate.

3.3.1.1. Multi-axial compressive strength. Fig. 9 presents the evolu- uniaxial compression, triaxial compression with 5 MPa confining
tion of deviatoric strength versus confining pressure for the two pressure and triaxial compression with 15 MPa confining pressure
sets of mortar after maturation period and after conditioning per- for the NR mortar. For the R mortar, the strength increases by
iod at 60 °C and 95% RH for the development of the ASR expansion. about 42%, 38% and 26% respectively in uniaxial compression, tri-
Depending on confining pressure, the mechanical strength in- axial compression with 5 MPa confining pressure and triaxial com-
creases during the conditioning period of samples. For instance, pression with 15 MPa confining pressure. On the other hand, the
the strength increases by about 14%, 12% and 6% respectively in results issued from the tests after the maturation period show that
170 I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174

120 As indicated earlier, the mechanical behaviour of cement-based


Deviatoric stress [MPa]
materials affected by ASR is often studied under uniaxial compres-
100 4 sion. Results of some authors [5,9,16,17,19,22,24,25] are recapped
in Table 2 where the reference state for the evaluation of the var-
2
80 3 iation of mechanical properties with ASR is that corresponding to
1 maturation period. In this table, NR concrete, R concrete and HR
60 concrete correspond respectively to concrete made with non-reac-
Pc=15MPa tive (NR), moderately or slowly reactive (R) and highly reactive
40 (HR) aggregates. In addition, R or HR concrete does not necessarily
mean that all the aggregates are reactive but only a part of the
20 aggregates can be reactive. The results obtained from this study
Radial strain Axial strain on the evolution of uniaxial compressive strength with ASR process
0
are different from those reported by Ahmed et al. [25] and Giaccio
-0.02 -0.01 0 0.01 0.02 0.03 0.04 et al. [9] who observed a decrease in the uniaxial strength of R con-
crete compared with that of NR concrete. Their results indicate that
Fig. 8. Triaxial compression tests with confining pressure of 15 MPa: (1) and (2) for the ASR does not necessarily prevent the increase in mechanical
NR and R samples respectively after 28 day maturation, and (3) and (4) for NR and R
samples respectively after conditioning at 60 °C and 95% RH.
strength (this is sometimes also true for HR concrete, see the re-
sults of Monette et al. [22] in Table 2), at least during the period
of experimental campaign, but this increase can be weak compared
110 with the concrete without reactive aggregates. On the other hand,
Deviatoric strength [MPa]
Larive [16], who studied the mechanical behaviour of two con-
100 cretes fabricated with the aggregates (sand and gravel) of the same
90 origin than those used in the present study, observed that the uni-
axial compressive strength of the R concrete and NR concrete in-
80 creases approximately by 71% and 69% respectively compared
70
with their reference strength at 15 days. These results seem to
show that the uniaxial compressive strength of a cement-based
60 material with reactive aggregates can be as high as that of a mate-
NR samples after maturation period rial without reactive aggregates. However, Multon [24] observed
50 R samples after maturation period
NR samples after conditioning at 60°C and 95% RH
that the uniaxial compressive strength of R concrete is significantly
40 R samples after conditioning at 60°C and 95% RH lower than that of NR concrete when the samples are stored in
Confining pressure [MPa] water at 38 °C (see Table 2). Indeed, the author reported that after
30
0 5 10 15 20 2 years of conditioning of samples in water at 38 °C, the uniaxial
compressive strength of NR concrete increased by 77% (from 35
Fig. 9. Failure stresses versus confining pressure for NR and R mortars after 28 day to 62 MPa) while this increase was only about 22% (from 38.6 to
maturation and after conditioning at 60 °C and 95% RH. 47 MPa) for R concrete. That could come from a more significant
development of swelling in water leading to induced microcrack-
ing. For our study, we could also have obtained a decrease in uni-
the multi-axial compressive strength of the R mortar is slightly axial strength of R mortar compared with NR mortar if our samples
higher than that of the NR mortar (3–9%). After the conditioning had been kept in water. Moreover, it is difficult to imagine exactly
of samples at 60 °C and 95% RH, the deviatoric strength of the R the evolution in time of the compressive strength of our R mortar
mortar becomes significantly higher than that of the NR mortar stored in controlled environment with 60 °C and 95% RH but it is
(23–34%). Thus, the relatively small difference of multi-axial quite possible that the ASR induces, at very long term, an impor-
strength between the two materials at the reference state becomes tant micro-cracking. That could also lead to a strength reduction
significant after the conditioning period for ASR process. after the first phase where the strength increases. Note however
After the maturation period, the very slightly higher mechanical generally a decrease in mechanical strength can be clearly ob-
strength of the R mortar with respect to the NR mortar seem to be served in a relatively short period of time for concrete with highly
well correlated with the microscopic analysis indicating that the reactive aggregates [5,9,17,25] even if only a part of aggregate is
microstructure of the two mortars is overall rather similar and that reactive [9,17,25]. It is worth to mention that the geometry of sam-
their rate of hydration is close each other. The fact that the rela- ples to be tested (for instance, cubic or tall prismatic samples) also
tively micro-porous zones are more frequently observed in the R has importance on the obtained strength results [19].
mortar does not seem to have any measurable effect on multi-axial In order to study the evolution of failure parameters due to ASR
strength. On the other hand, the important increase of the multi- process, the classical Drucker–Prager criterion is used here and ex-
axial strength of the R mortar after the conditioning period comes pressed in the following form:
from its more compact microstructure compared with that of the pffiffiffiffi
NR mortar as illustrated by the SEM images. The relative compact- f ¼ J 2  arm  k ¼ 0 ð1Þ
ness of the R mortar is mainly related to the improvement of ITZ
properties (Figs. 5 and 7). Indeed, it is well known that the ITZ con- J2 is the equivalent stress (second invariant of deviatoric stress ten-
stitutes the weakest link in ordinary strength cement-based mate- sor), rm is the mean stress; a and k are two failure parameters
rials because of its higher porosity compared with that of bulk respectively related to the friction coefficient and cohesion of mate-
paste. Therefore, the densification of ITZ by the presence of gels rial. These twopparameters
ffiffiffiffi are determined by drawing the failure
would increase the strength greatly. Thus, it can be said that over surface in the J2  rm plane as shown in Fig. 10. The values ob-
the period of this experimental investigation the compactness of tained are presented in Table 3. One can see that the conditioning
the material plays a dominant role with respect to the induced of the samples at 60 °C and 95% RH mainly leads to an increase in
microcracking, which leads to the increase of the deviatoric cohesion of materials, respectively by 16% for NR mortar and 37%
strength of R mortar. for R mortar. The friction coefficient remains nearly unchanged
I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174 171

Table 2
Effect of ASR on the evolution of uniaxial compressive strength (fc) and Young’s modulus (E).

Reference Material Maturation period Conditioning period for ASR Variation of


development mechanical
properties at the end
of conditioning
period [%]: decrease
(-), increase (+)
fc E
Ahmed et al. [25] NR concrete 28 days in water at 20 °C 12 months in water at 38 °C 40 16
R concrete 13 67
HR concrete 35 92
Clayton [19] R concrete 28 days in water at 20 °C 4 months in water at 38 °C 11 (cubes) –
30 (tall –
prisms)
Giaccio et al [9] NR concrete 28 days, samples covered with Identical to the maturation 66a 6
R(1) cotton sheet then placed in plastic bags mode, uniaxial test when axial 40b 18
concrete (including 5 ml of water) which are stored at 38 °C expansion
R(2) between 0.11 and 0.18% 5a 59
concrete
c
HR concrete 9 10
Marzouk and Langdon R concrete 28 days in de-ionised water at ambient temperature 3 months in de-ionised water at 80 °C 21 61
[5] 3 months in NaOH solution at 80 °C 2 31
HR concrete 3 months in de-ionised water at 80 °C 13 26
3 months in NaOH solution at 80 °C 26 –
Monette et al. [22] HR concrete 28 days at 20 °C and 100% RH 147 days in 1 N NaOH solution at 38 °C 54 68
Pleau et al. [17] NR concrete 7 days in moist curing at 23 °C About 2 years at 38 °C and 100% RH 12d 11
HR concrete 33d 64
Larive [16] NR concrete 15 days at 23 °C, samples covered with plastic and aluminium About 22–23 months at 38 °C and 69 8
R concrete sheets RH > 95% 71 22
Multon [24] NR concrete 28 days at 20 °C, samples covered with aluminium sheets 2 years at 38 °C and 30% RH, samples 23 2
covered with aluminium sheets
R concrete 11 6
2 years, samples placed in water at 38 °C 77e 9
22f 24
a,b,c
Obtained at 250 days, 485 days and 120 days respectively.
d
Obtained with regard to 28 day compressive strength.
e,f
Obtained on NR concrete and R concrete respectively.

for the first and slightly increases, by 5%, for the second one. Conse- mortar becomes much lower than those of the NR mortar by
quently, it can be said that the ASR influences mainly the cohesion 8–17% and 37–39% respectively. Thus, the difference between the
of reactive material, at least in case of the present study. Moreover, elastic coefficients of the two materials is increased after the con-
the friction coefficient of the R mortar is equal to that of the NR ditioning of samples.
mortar while its cohesion is higher (by 8%) after the maturation per- Thus, in spite of an important increase in multi-axial compres-
iod. The conditioning of the samples at 60 °C and 95% RH leads to an sive strength, the Young’s modulus of the R mortar decreases
improvement of friction coefficient (6%) and cohesion (26%) of R slightly after ASR process. As underlined already by several
mortar with respect to NR mortar. authors, this shows a more important sensitivity of the Young’s
modulus to the development of ASR which leads to induced
3.3.1.2. Elastic properties. The evolutions of elastic properties were microcracking. This is the reason that a reduction in the Young
also investigated during multi-axial compression tests and com- modulus of reactive concrete is obtained whereas its compressive
pared between R and NR mortars. The initial values of elastic coef- strength continues to increase. Moreover, it seems that there is no
ficients are determined on the third cycle of loading-unloading of significant influence of the confining pressure up to 15 MPa on
each test. Moreover, as indicated earlier, the Poisson’s ratio could the decrease in Young modulus. A higher confining pressure
not be determined in the case of uniaxial compressive test (see would be necessary to observe a possible closure of the ASR in-
Section 2.2). The evolution of the initial Young’s modulus and Pois- duced microcracks. The reduction in the Young’s modulus of reac-
son’s ratio versus confining pressure are presented on Figs. 11 and tive concrete reported by Giaccio et al. [9], Larive [16], Multon
12 respectively. As for the deviatoric strength, the elastic coeffi- [24], Marzouk and Langdon [5] and Ahmed et al. [25] were 18%,
cients also depend on confining pressure. Both the elastic modulus 22%, 24%, 31% and 67% respectively (see also Table 2). Ahmed
and Poisson’s ratio increase with confining pressure. Regarding the et al. [25] even obtained a drop up to 92% for their highly reactive
conditioning effects, the initial Young’s modulus of NR mortar concrete (see also Table 2). On the other hand, even if the results
nearly does not change while its Poisson’s ratio increases by 12– of the present study indicate a sensitivity of Poisson’s ratio to the
13% after the conditioning of the samples at 60 °C and 95% RH. ASR induced damage, such a sensitivity is not observed by Larive
For the R mortar, the initial Young’s modulus decreases by 5–8% [16] and Multon [24]. However, a clear decrease of Poisson’s ratio
and the Poisson’s ratio by 20% after the conditioning of the samples is also reported by Giaccio et al. [9] on their highly reactive
at 60 °C and 95% RH. On the other hand, the tests after the matura- concrete.
tion period show that the Young’s modulus and Poisson’s ratio of
the R mortar are lower than that of the NR mortar by 0–11% and 3.3.2. Bending strength
12–13% respectively. After the conditioning of samples at 60 °C Table 4 gives the values of average bending strength of two
and 95% RH, the Young’s modulus and Poisson’s ratio of the R mortars after the maturation period at ambient temperature and
172 I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174

70 the conditioning period at 60 °C and 95% RH. The bending strength


(J2)0.5 [MPa]
increases by 44% for the NR mortar and by 5% for the R mortar.
60 Unlike the multi-axial compressive strength, the increase in the
bending strength of R mortar is marginal compared with that of NR
50
mortar. This shows again a higher sensitivity of the flexural
40
strength to the ASR induced microcracking compared with the
compressive strength [2–5,9,18,19,22,25]. This could be explained
30 by the closing of the ASR induced microcracks under compressive
stress whereas the tensile stress in flexion tests quickly leads to
NR mortar after maturation period
20 R mortar after maturation period the propagation of the microcracks [2,18]. Note that Ahmed et al.
NR mortar after conditioning at 60°C and 95% RH [25] obtained on their concrete with low reactive aggregates a
10 R mortar after conditioning at 60°C and 95% RH reduction by 49% of the bending strength compared with the
σm [MPa] 28 day bending strength whereas, as indicated above, the compres-
0
0 10 20 30 40 50 60 sive strength increased. Marzouk and Langdon [5] also reported a
reduction by 24% for their moderately reactive concrete with re-
Fig. 10. Representation of failure surfaces according to D–P criterion for NR and R
spect to the 28 day bending strength, while the compressive
mortars after 28 day maturation and after conditioning at 60 °C and 95% RH.
strength of the concrete almost did not vary. For a concrete fabri-
cated with highly reactive aggregates, the drop of bending strength
Table 3 due to the ASR can reach up to 84% [25].
Friction coefficient and cohesion of mortars after 28 day maturation and after
conditioning at 60 °C and 95% RH for ASR development.
3.4. Variation of porosity and permeability due to ASR
Material Friction coefficient (a) Cohesion (k) (MPa)
NR mortar After maturation 0.81 11.48 Table 5 shows the average values of water porosity after the
after 0.80 13.36
conditioning
28 day maturation period and after the conditioning of samples
R mortar After maturation 0.81 12.35 at 60 °C and 95% RH. After the maturation period, the porosity of
after 0.85 16.86 the two mortars is nearly identical. However, after the condition-
conditioning ing period of samples, the porosity of the NR mortar does not
change whereas that of the R mortar varies from 15.9 to 17.2% cor-
responding to an increase of about 8%. This increase is mainly due
to the ASR induced micro-cracking: the gels formed by the ASR ab-
35000 sorb water and expand leading to the formation of microcracks.
Young's modulus [MPa]
Table 6 gives the evolution of the permeability to de-aroma-
30000 tized oil after the maturation and conditioning of samples respec-
tively. After the maturation period, the permeability of two
mortars is very close each other, as was the case for porosity. It
25000
is observed that the permeability decreases after the conditioning
of the samples at 60 °C and 95% RH for the two mortars, due to the
20000 hydration process and improvement of ITZ. However, the reduction
NR samples after maturation period
R samples after maturation period
in the permeability is less important for the R mortar than for the
NR samples after conditioning at 60°C and 95% RH NR mortar, respectively by 76% against 84%. Furthermore, after the
15000
R samples after conditioning at 60°C and 95% RH period of maturation, the permeability of the R mortar is only 5%
Confining pressure [MPa] higher than that of the NR mortar. After the conditioning of the
10000 samples, the permeability of the R mortar becomes 56% higher
0 5 10 15 20 than that of the NR mortar.
Fig. 11. Evolution of initial Young’s modulus versus confining pressure for NR and R
Thus, the porosity of the two materials before and after condi-
mortars after 28 day maturation and after conditioning at 60 °C and 95% RH. tioning of the samples at 60 °C and 95% RH has different evolution
than that suggested by the mechanical test results. Neither the in-
crease in the multi-axial strength of the NR mortar nor that of R
mortar after conditioning of samples can be detected by the mea-
0.3 surement of porosity. Instead of a decrease, an increase of porosity
Poisson's ratio
is observed for the R mortar. Thus, a priori, the determination of
0.25 porosity does not contribute to really understand what occurs on
the mechanical feature. However, the porosity increase of the R
0.2 mortar could be seen as a sign of ASR induced microcracking.
The porosity measurement can be useful in this sense. But, as the
0.15 compactness of the material dominates on the increase in porosity,
NR samples after maturation period
the multi-axial strength of R mortar increases rather than
0.1 R samples after maturation period
NR samples after conditioning at 60°C and 95% RH Table 4
R samples after conditioning at 60°C and 95% RH Average bending strength of mortars after 28 day maturation and after conditioning
0.05
at 60 °C and 95% RH for ASR development.
Confining pressure [MPa]
0 Material Bending strength Bending strength
5 10 15 20 after maturation (MPa) after conditioning (MPa)
NR mortar 5.2 ± 0.1 7.5 ± 0.6
Fig. 12. Evolution of initial Poisson’s ratio versus confining pressure for NR and R
R mortar 7.6 ± 0.4 8.0 ± 0.1
mortars after 28 day maturation and after conditioning at 60 °C and 95% RH.
I. Yurtdas et al. / Construction and Building Materials 47 (2013) 165–174 173

Table 5 in the present work have clearly shown that the tensile strength
Average porosity of mortars after 28 day maturation and after conditioning at 60 °C and elastic modulus (and also Poisson’s ratio) were more signifi-
and 95% RH for ASR development.
cantly affected by the ASR induced microcracking than the com-
Material Porosity after maturation (%) Porosity after conditioning (%) pressive strength. Our results confirmed those reported in some
NR mortar 15.6 ± 0.5 15.5 ± 0.8 previous works. However, in the present study, we have further
R mortar 15.9 ± 0.8 17.2 ± 0.7 studied the evolution of microcracks induced by ASR process by
the permeability and porosity measurements. In particular, the
measurement of permeability provides a good way to evaluate
the ASR induced microcracking. Finally, microstructural analyses
have been well correlated with mechanical tests, permeability
Table 6
Average permeability of mortars after 28 day maturation and after conditioning at and porosity measurements. Note that it will be very useful to
60 °C and 95% RH for ASR development. investigate the effects of ASR at very long term. This investigation
will enable the influence of an additional ASR induced damage on
Material Permeability after Permeability after
maturation (10–16 m2) conditioning (10-16 m2) the evolution of mechanical properties, in particular compressive
strength, and hydraulic properties of R mortar to be evaluated.
NR mortar 5.6 ± 0.1 0.9 ± 0.1
R mortar 5.9 ± 0.1 1.4 ± 0.1
Acknowledgements

The present work is supported by the Chinese Ministry of Water


decreasing. To some extent, the permeability measurement seems
Resources’ special Funds for Scientific Research on Public Causes
to better correspond to what is observed on the mechanical level.
(Grant No. 200801057) and the National Natural Science Founda-
Indeed, one can note a decrease in the permeability of two materi-
tion of China (Grant No. 51009061). The microstructural analysis
als which corresponds to a reduction in available flow paths to
was conducted by LERM. The authors are very grateful to Dr. N.
fluid. However, like porosity, the permeability of the R mortar is
Rafaï for his valuable comments and discussions.
also higher than that of the NR mortar (by 56%). This suggests
the occurrence of microcracking after the conditioning of samples.
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