1-s2.0-S0958946516301263-main
1-s2.0-S0958946516301263-main
1-s2.0-S0958946516301263-main
a r t i c l e i n f o a b s t r a c t
Article history: This paper presents an experimental study to characterize the mechanical behaviour, at the local scale, of
Received 10 September 2015 sound and degraded concrete after leaching. An experimental protocol was developed to study the ef-
Received in revised form fects of the calcium leaching mechanism at the interfacial transition zone (ITZ) on the mechanical
13 April 2016
properties of the cement-aggregate interface and bulk paste of model material. The process of lixiviation
Accepted 3 May 2016
Available online 10 May 2016
with deionised water occurs very slowly. The experimental study in the laboratory was accelerated by
replacing the water with an ammonium nitrate solution. To quantify the development and kinetics of
degradation at the cemented bond, the concrete leaching fronts were characterized at different levels of
Keywords:
Concrete
degradation using phenolphthalein and local mechanical tests (compression and tensile) and performed
Leaching on samples consisting of two aggregates bound by cement paste. Tests were performed on sound
Cement-aggregates scale samples at different hydration times and on chemically degraded samples. The results show the effect of
Interfacial transition zone (ITZ) leaching on the mechanical properties of the samples and making it possible to correlate the progress of
Mechanical tests leaching to the evolution of these locally considered properties. The experimental results show that there
is an ITZ effect on the alteration of the mechanical properties due to leaching.
© 2016 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.cemconcomp.2016.05.001
0958-9465/© 2016 Elsevier Ltd. All rights reserved.
242 M. Jebli et al. / Cement and Concrete Composites 73 (2016) 241e250
characterized by a higher porosity than the bulk paste and a high the same diameter (8.3 mm), and were bound by a cement paste
concentration of portlandite [4,11,16,31,40] which increases calcium (cement CEM II/B 32.5 N) with a ratio water/cement of 0.5 with a
leaching. The work of Zheng and al. [39] and Winslow and al. [37] circular cross section. Aitcin [2] found a reduction in the porosity
have also shown that ITZ provides a preferential path for the and thickness of the interfacial transition zone in the High-
transport of water and ions. In order to characterize the lixiviation Performance Concrete (HPC). Generally, the thickness of the ITZ
effect of the ITZ on mechanical properties, a series of experiments of the HPC is limited to 12 mm, whereas that of ordinary concretes is
was carried out by Carde and François [9] on a cement paste and about 50 mm. The distance between two aggregates was fixed at
mortar, with or without silica fume, demonstrating the effect of the 1.7 mm, this being the average distance between two large grains
ITZ on the mechanical properties of concrete. A recent experi- observed in a concrete [12]. According to the definition of De Lar-
mental study by Buzzi and al. [8] showed that a leached rock- rard [23], the distance between these two large adjacent aggregates
concrete interface at fixed leaching depth presents a radical separated by the cement paste is called the Maximum Paste
change of behaviour because of the local loss of mechanical Thickness (MPT). The MPT affects the compressive strength of
strength. concrete. When MPT decreases, the compressive strength in-
The process of lixiviation with deionised water occurs very creases. the interstitial space between aggregates mobilized by the
slowly [1]. It has been shown that for concrete with a water/cement ITZ also increase. Another explanation is crystal orientation of
ratio of 0.4, a degradation depth of 4 cm would necessitate a CeSeH, more the MPT is lower, more the hydrates are oriented,
leaching time about of 300 years and very few data are available in what improve resistance to compressive [23].
the literature about long term degradation of concrete by pure The geometric configuration of the sample is presented in Fig. 1
water [35]. In order to collect experimental data in a reasonable and the “material” data in Table 1. Simplified form of aggregates is
period of time, it is necessary to use an accelerated procedure. used. These were perfectly spherical and of the same size, as orig-
There are three methods to accelerate calcium leaching of cemen- inally proposed by Bisschop and Van Mier [5] to study the effect of
titious materials: application of an electric field [17,33], using aggregates on drying shrinkage in cement-based composites and
temperature [21] and using different chemical solutions to increase by Burlion and al. [7] to study microcracking in leached cementi-
concentration gradients between the interstitial solution and the tious materials. Demoulding was carried out after 24 h. The sample
aggressive environment [13,32]. Ammonium nitrate (NH4NO3) has obtained had a diameter of 8 mm and a height of about 18 mm: This
been chosen by several authors as a representative aggressive so- sample was regarded as representative. The samples were stored in
lution for these accelerated experiments [3,10,19,25,26,30,34]. The water saturated with lime at 21 C to reduce the leaching with
principle of accelerated degradation with ammonium nitrate is the water and the effects of drying shrinkage.
penetration of NH4þ and NO3 ions stemming from the dissolution The specific sample geometry selected allowed us to consider
of ammonium nitrate (Eq. (1)), in the interstitial solution by the concrete as a three-phase material: aggregates, cementitious
diffusion. The NH4þ ion reacts with the OH of the interstitial so- matrix and ITZ (Fig. 2). This allowed us to follow the direct effect of
lution (Eq. (2)) and the NO3 ion reacts with the calcium ions (Eq. leaching at the ITZ interface and also in the bulk paste. Two sets of
(3)). This consumption of Ca2þ ions disturbs the chemical balance of samples were examined: the first was kept in water saturated with
the calcium between the liquid and solid phases, causing the lime at 21 C (control series) and the second was immersed in the
dissolution of hydrates to free new calcium ions (Eq. (4)). aggressive ammonium nitrate solution (degraded series), after
Ca2þ þ 2NO
3 ⇔CaðNO3 Þ
2
(3)
equipped with a force sensor of 5000 ± 10 N for compression tests shown in Fig. 6 at different stages of hydration between 1 and 40
and 500 ± 1 N for tensile tests. The force applied to the sample and days.
the longitudinal displacements were measured in the axial direc- These figures show a significant increase in the force at rupture
tion during the test. and stiffness of the samples at the beginning of hydration, with
To perform mechanical tests, specific accessories were pro- almost constant values after more than three weeks of hydration.
duced, adapted to local testing. Fig. 4 shows the experimental de- The examined samples in the compression test show ductile
vice of the compression and tensile tests. Before each test, the behaviour at a very early age, which become increasingly brittle.
dimensions and weight of each sample were measured. For each The values of the force at rupture noted f ðjÞ (in Newton) and
duration of hydration and degradation, four samples are subjected stiffness kðjÞ, were estimated from the linear part of the slope of
to compression or tensile mechanical testing. force-displacement curve calculated as shown in Fig. 7, depending
on hydration time (in days); the compressiontest results are shown
2. Results in Figs. 8 and 9. There was an increase of the forces at rupture and
stiffness in compression during hydration with a drop in speed of
In this section, all the results obtained during mechanical testing evolution after 28 days.
are presented and discussed, for compression tests and tensile tests The evolution of the force was approximated by an exponential
for sound samples and chemically degraded samples by leaching. A function, based on the Eq. (6) presented in Eurocode 2 [14] to es-
preliminary study was carried out on sound samples to characterize timate the macroscopic resistance of concrete.
the behaviour of concrete during the hydration process at the local
scale in the cement-aggregate interface and the cement paste bond. fc ðjÞ ¼ bcc fc ð28Þ (6)
Interactions on this scale were analysed experimentally.
Where fc ð28Þ ¼ 1500 N is the force at rupture in compression of the
2.1. Sound samples
Fig. 4. Pictures of supports for (a) the compression test and (b) the tensile test.
Fig. 5. Pictures of the sample during compression test (23 days of hydration). Fig. 7. Method of measuring stiffness.
M. Jebli et al. / Cement and Concrete Composites 73 (2016) 241e250 245
Fig. 9. Evolution of stiffness as a function of hydration time during mechanical tests. Fig. 10. Pictures of the sample during tensile test (21 days of hydration).
246 M. Jebli et al. / Cement and Concrete Composites 73 (2016) 241e250
Using the p value, the other degradation time which be used for
qualitative estimates can be predicted, depending on the cement
type and characteristics of the acceleration method of degradation
used.
The evolution of the degradation kinetics has been shown
experimentally by other authors [20,24,29,34] using the same
method of accelerated degradation at the macroscopic scale. In our
case,
pffiffiffiffiffiffiffiffiat the local scale, the value of the slope p was equal to 2 mm by
day.
Chemical degradation of the concrete due to dissolution of the
hydrates caused a loss mass in the samples. Fig. 15 shows the loss of
mass in relation to the degraded rate d.
Fig. 18. Pictures of crack evolution of degraded sample during compression test after
72 h of degradation.
facies in the case of tensile tests show that cohesion loss occurs at
the cement paste-aggregate interface. Besides, the degradation of
the tensile strength properties occurs for relatively low degradation
rate. This suggests that the interface properties are more sensitive
Fig. 16. Mechanical behaviour of sound and partially degraded samples under
compression tests. to the degradation than those of the bulk paste. It is well known
that the porosity of the ITZ is always greater than the porosity in the
bulk paste. So, the chemical attack front, controlled by the diffusion
material, leading to the loss of cohesion between the bulk paste and of the ions, is naturally accelerated at the interface, more porous
aggregates as shown in Fig. 21. This results could not be observed and thus more permeable.
with phenolphthalein du to the weak thickness of ITZ. Fig. 22 illustrates this statement. It shows how the degradation
of the interface could be much faster than the degradation of the
3. Discussion bulk paste, and how it could be widely underestimated by the
overall degradation rate.
The chemical attack by leaching induces the total dissolution of The mechanical compression test showed the effect of leaching
the calcium hydroxide and progressive decalcification of CSH, in the cemented bond between the two aggregates. There was a
leading to an increase in porosity and a decrease of mechanical drop in force at rupture and there were changes in behaviour with
properties. Most experimental studies on the effect of the cemen- the increase of leaching, as is observed at macroscopic scale. This is
titious material leaching on mechanical properties are carried out explained by the increase in porosity due to dissolution of the hy-
on a macroscopic and mesoscopic scale. So it was of interest to drates. The chemical alteration of the interface did not affect the
perform experiments at the local scale to understand the degra- results of the compression test.
dation mechanism on this scale. As shown above, all the rupture The tensile test directly characterized the ITZ in our chosen
Fig. 17. Evolution of the force at rupture as a function of degraded rate during mechanical tests.
M. Jebli et al. / Cement and Concrete Composites 73 (2016) 241e250 249
Fig. 22. Diagram of the degradation evolution of the composite at the ITZ and the bulk
paste.
4. Conclusion
References
[13] A. Delagrave, Mechanisms of Chloride Ion Penetration of Normal and High 266e272.
Performance Cement Based Systems, Ph.D. thesis, Universite de Laval, Canada, [26] F. Lea, The action of ammonium salts on concrete, Mag. Concr. Res. 17 (1965)
1996. 115e116.
[14] B. EN, 1e1: 2004 Eurocode 2: Design of Concrete Structures, 1992. [27] J. Maso, La liaison entre les granulats et la p^ ate de ciment hydrate , in: 7e
me
, V. LHostis, H. Peycelon, M. Helie, A. Millard, P. Lachaize, Durabilite
[15] C. Galle du Congre s International de la chimie des ciments, Rapport principal, 1980.
beton des infrastructures et des colis pour le stockage graphite, 2004. Rapport [28] P. Mason, The effects of aggressive water on dam concrete, Constr. Build.
Technique RTDPC. Technical Report SCMME/04-672-A, CEA. Mater. 4 (1990) 115e118.
[16] E. Garboczi, L. Schwartz, D. Bentz, Modeling the influence of the interfacial [29] V. Nguyen, Couplage de gradation chimique-comportement en compression
zone on the dc electrical conductivity of mortar, Adv. Cem. Based Mater. 2 du be ton, Ecole des Ponts ParisTech, France, 2005. Ph.D. thesis.
(1995) 169e181. [30] V. Nguyen, B. Nedjar, J. Torrenti, Chemo-mechanical coupling behaviour of
[17] B. Gerard, O. Didry, J. Marchand, D. Breysse, H. Hornain, Modelling the Long- leached concrete: part ii: modelling, Nucl. Eng. Des. 237 (2007) 2090e2097.
term Durability of Concrete Barriers for Radioactive Waste Disposals, Tech- [31] J. Ollivier, J. Maso, B. Bourdette, Interfacial transition zone in concrete, Adv.
nical Report, Electricite de France (EDF), Direction des Etudes et Recherches, Cem. Based Mater. 2 (1995) 30e38.
Paris, France, 1996. [32] E. Revertegat, C. Richet, P. Gegout, Effect of ph on the durability of cement
[18] E. Guillon, F. Benboudjema, M. Moranville, Modelling the mechanical evolu- pastes, Cem. Concr. Res. 22 (1992) 259e272.
tion of a chemically degraded cement paste at the microstructure scale, in: [33] H. Saito, S. Nakane, S. Ikari, A. Fujiwara, Preliminary experimental study on the
FRAMCOS, vol. 5, 2004, pp. 12e16. deterioration of cementitious materials by an acceleration method, Nucl. Eng.
[19] F. Heukamp, Chemomechanics of Calcium Leaching of Cement-based Mate- Des. 138 (1992) 151e155.
rials at Different Scales: the Role of CH-dissolution and CSH Degradation on [34] C. Tognazzi, Influences couple es de la fissuration et de la de gradation sur
Strength and Durability Performance of Materials and Structures, Ph.D. thesis, transferts dans les betons, in: Congre s Universitaire de Ge nie Civil: Concours
Massachusetts Institute of Technology, 2003. Jeunes Chercheurs, 1998.
[20] F. Heukamp, F.-J. Ulm, J. Germaine, Mechanical properties of calcium-leached €gårdh, B. Lagerblad, Leaching of 90-year Old Concrete Mortar in Contact
[35] J. Tra
cement pastes: triaxial stress states and the influence of the pore pressures, with Stagnant Water, Technical Report, Swedish Nuclear Fuel and Waste
Cem. Concr. Res. 31 (2001) 767e774. Management Co., Stockholm (Sweden), 1998.
[21] S. Kamali, B. Gerard, M. Moranville, Modelling the leaching kinetics of cement- [36] F. Ulm, J. Torrenti, F. Adenot, Chemoporoplasticity of calcium leaching in
based materials influence of materials and environment, Cem. Concr. Compos. concrete, J. Eng. Mech. 125 (1999) 1200e1211.
25 (2003) 451e458. [37] D.N. Winslow, M.D. Cohen, D.P. Bentz, K.A. Snyder, E.J. Garboczi, Percolation
[22] S. Kamali-Bernard, D. Keinde, F. Bernard, Effect of aggregate type on the and pore structure in mortars and concrete, Cem. Concr. Res. 24 (1994)
concrete matrix/aggregates interface and its influence on the overall me- 25e37.
chanical behavior. A numerical study, in: Key Engineering Materials, vol. 617, [38] I. Yurtdas, S. Xie, J. Secq, N. Burlion, J. Shao, M. Sibai, P. Brossolet, B. Fraboulet,
2014, pp. 14e17. Trans Tech Publ. Couplage comportement me canique et perme abilite
: cas d’une p^ ate de ciment
[23] F. de Larrard, A. Belloc, The influence of aggregate on the compressive petrolier de grade
e chimiquement a 90 C, Rev. Eur. Ge nie Civ. 11 (2007)
strength of normal and high-strength concrete, ACI Mater. J. 94 (1997). 827e837.
go, Couplage chimie me
[24] C. Le Belle canique dans les structures en be ton arme [39] J. Zheng, C. Li, X. Zhou, Thickness of interfacial transition zone and cement
attaquees par l’eau-Etude expe rimentale et analyse nume rique, Ph.D. thesis, content profiles around aggregates, Mag. Concr. Res. 57 (2005) 397e406.
ENS de Cachan, France, 2001. [40] R. Zimbelmann, A contribution to the problem of cement-aggregate bond,
[25] C. Le Bellego, B. Ge rard, G. Pijaudier-Cabot, Chemo-mechanical effects in Cem. Concr. Res. 15 (1985) 801e808.
mortar beams subjected to water hydrolysis, J. Eng. Mech. 126 (2000)