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Experimental observation of internal water curing of concrete

Article  in  Materials and Structures · March 2007


DOI: 10.1617/s11527-006-9132-x

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EXPERIMENTAL OBSERVATION OF INTERNAL WATER
CURING OF CONCRETE
Materials and structures 40(2) (2007) 211-220

Pietro Lura and Ole Mejlhede Jensen


Technical University of Denmark, Denmark
Shin-Ichi Igarashi
Kanazawa University, Japan

Abstract
Internal water curing has a significant effect on concrete. In addition to affecting hydration and
moisture distribution, it influences most concrete properties, such as strength, shrinkage,
cracking, and durability. The following paper is an overview of experimental methods to study
internal water curing of concrete and its consequences. The special techniques needed to study
internal water curing are dealt with along with the consequences of this process. Examples of
applications are given and new measuring techniques that may potentially be applied to this
field are addressed.

1 Introduction
Internal water curing affects many concrete properties, some of which can be used as
indicators of the characteristics of the internal water curing process and of its effectiveness. In
this paper, consequences of the internal water curing process are presented, ranging from the
most direct to the most remote. Where relevant, measuring techniques applied to study internal
water curing are described and the results briefly summarized; an extensive list of references is
given. Measuring techniques that may potentially address specific aspects of internal water
curing but have not been applied so far are also mentioned.

Internal water curing agents, e.g. lightweight aggregates, LWA, and super absorbent polymers,
SAP, may themselves have a significant influence on many concrete properties. If large
amounts of the internal water curing agent are incorporated in the mixture, such as in
lightweight aggregate concrete, LWAC, it may be complicated to separate the consequences of
internal water curing from the consequences of the inclusion of the internal water curing agent
in the concrete mixture. For example, internal water curing due to LWA reduces the
autogenous shrinkage, but incorporation of the LWA may reduce the modulus of elasticity of
the concrete, potentially increasing its shrinkage.

In this paper, the focus is on the applications where internal water curing is used purposefully
to avoid self-desiccation and its consequences. However, in the past decades, effects of
internal water curing have been observed mostly in LWAC, where internal water curing was
only a beneficial side effect of the use of LWA; therefore, observations and measurements on
LWAC will be mentioned when relevant.

2 Direct evidence of internal water curing

2.1 Internal relative humidity


Internal relative humidity (RH) is a measure of water activity (chemical potential) in the
cement paste. After separation of the effect of dissolved salts in the pore solution, the Kelvin
2

radius can be calculated from the internal RH [1]. Internally water cured pastes are ideally
hydrating in saturated conditions, with access to the separate water phase that is contained in
the water reservoir [2]. Consequently, they do not self-desiccate and their internal RH remains
close to 100% throughout hydration.

RH measurements with high-accuracy Rotronic stations (±1% RH) have been performed on
internally cured mixes with LWA and SAP [3, 4], showing in all cases higher internal RH
throughout hydration compared to mixes without internal water curing, see Figure 1.

Another technique for measuring internal RH in concrete is based on cast-in sensors. With RH
sensors becoming less expensive and smaller, it is possible to embed them in a concrete
structure [5] and monitor the internal RH on site with acceptable accuracy (±2% RH) for
months. However, temperature variations affect the measurements and should be taken into
account.

100
Relative humidity [%]

LWA20
95
SAP
LWA08

90

Reference

85
0 5 10 15 20
Time [days]
Figure 1. Measured internal relative humidity during sealed hydration at 30C of mortars with
and without internal water curing, modified from [3]. Water/cement ratio of the mortars is
0.35, with 8% by mass replacement of cement by silica fume. ‘Reference’ indicates the mortar
with no internal curing, ‘SAP’ the mortar with super absorbent polymers, ‘LWA08’ and
‘LWA20’ the mortars with 8% and 20% by mass replacement of sand by saturated lightweight
aggregates, respectively.

2.2 Degree of saturation


In a cement paste hydrating with free access to external water, the pore system remains
saturated throughout hydration. Therefore, the amount of water in the coarse capillaries of a
cement paste may indicate the effectiveness of internal water curing. Since water in the internal
curing agents exists as loosely held water in the LWA or in the SAP, special care should be
taken in the measurements to separate it from the capillary water phase in the cement paste.

For Portland cement systems, Powers’ model provides a way to calculate the water distribution
between the different phases [2]. The amount of the capillary water phase can be calculated by
measuring the evaporable and the non-evaporable water content during hydration by drying
3

followed by ignition, provided the water in the internal curing agent can be separated from the
pore fluid in the cement paste.
The amount of water and its distribution in different pore sizes can be measured by a number
of techniques, such as low temperature calorimetry [6], different types of neutron scattering
[7], or techniques based on nuclear magnetic resonance, such as relaxometry [8],
cryoporometry [8], magnetic resonance imaging, and diffusometry. Nuclear magnetic
resonance measurements are able to measure the amount of water in pores of different size,
which enables to distinguish between water in hydrating cement paste and water in the internal
curing agent. Preliminary experiments on the nuclear magnetic resonance characterization of
internal curing agents were conducted in [9]. With nuclear magnetic resonance, a single
sample can be followed during hydration, while other techniques are often destructive and
require multiple samples.

2.3 Sorption isotherm


Sorption isotherms of concrete with internal water curing may show differences from normal
concrete [10]. From sorption isotherms, information can be derived about the pore size
distribution, the distribution of pore fluid in the pores and the way water is held in the pores.

A possible source of error in the interpretation of the sorption isotherms is that water in the
internal curing agent might be confused with water in the pore system of the cement paste. In
particular, a great part of the moisture capacity at high RH might be due to the water
reservoirs.

Disadvantages of sorption isotherm measurements are that multiple samples are needed to
follow the concrete through hydration and that only measurements on old samples are
practical, since the measurements generally last for many months. Information on sorption
isotherms may be derived thermodynamically based on RH measurements as discussed in ref.
[11].

Sorption isotherms on old LWAC samples cured in sealed conditions [12] show higher
moisture content in concrete with pre-wetted LWA compared to dry LWA. Differences were
observed between concrete containing LWA with an open and coarse pore structure (LECA)
and concrete containing LWA with closed and fine pore structure (Stalite): whereas the initial
moisture content at saturation was very similar, the latter mixture showed higher moisture
content, between 97% and 55% RH, probably due to water entrapped in the LWA.

3 Primary consequences of internal water curing

3.1 Degree of hydration


Availability of extra water for hydration and high water activity lead to increased cement
hydration in internally water cured cement pastes with low water/cement ratio (w/c) [2].
According to Powers’ model [13], hydration of Portland cement in pastes with free access to
water stops when all the capillary pores are filled with hydration products or when all the
cement has reacted. Based on this concept, Figure 2 shows the ultimate degree of hydration of
pastes; at low w/c, differences are as high as 20%. The ultimate degree of hydration in
saturated conditions is the theoretical maximum achievable in the case of efficient internal
water curing of the concrete. By measuring degree of hydration of internally water cured
concrete and comparing it with the results of Powers’ model, or alternatively, with small
4

reference samples stored in water, an estimate of the efficiency of internal water curing can be
obtained.

In ref. [14], concrete mixtures with low w/c containing saturated LWA were crushed and
sieved to separate the cement paste, on which thermal gravimetric analysis showed an increase
of the degree of hydration from 0.67 to 0.82 from 180 to 360 days after casting. On the same
mixtures, X-ray diffraction showed more calcium silicate hydrate, calcium hydroxide and
ettringite at 360 days than at 180 days [14]. In ref. [15], higher non-evaporable water contents
were measured on LWA mortars compared to reference mortars without LWA. Other possible
techniques to estimate degree of hydration of internally water cured concrete include scanning
electron microscopy, solid-state nuclear magnetic resonance, heat of hydration, and chemical
shrinkage.

1
Ultimate degree of hydration [-]

0.9
Saturated
0.8

0.7

0.6
Sealed
0.5

0.4

0.3

0.2

0.1

0 0.35 0.42
0 0.1 0.2 0.3 0.4 0.5
w/c ratio [-]
Figure 2. Ultimate degree of hydration according to Powers’ model [2] of cement pastes cured
in saturated and in sealed conditions.

3.2 Internal water movement


When the cement paste self-desiccates due to hydration, a gradient in water activity is
generated within the concrete and water migrates from the water reservoirs into the cement
paste. Water movement within the concrete can be used as an indicator of the internal water
curing process and of its development in time.

In the simple experiment shown in Figure 3, LWA particles saturated with a weak ink solution
were cast in low w/c cement paste [16]. Samples were split open at regular intervals, showing a
coloured corona around the LWA particles that grew up to 1-mm thickness. However, this
experiment does not allow distinguishing ink movements due to water migration from
diffusion of ink particles in the pore fluid.

A significant reduction of the self-diffusion coefficient of water in cement pastes during


hydration was revealed by nuclear magnetic resonance diffusometry [17]. In the same study,
water migration from phenolphthalein-filled tablets was followed in a cement paste with w/c
0.25 by monitoring the colour change in the paste induced by the tracer. By combining the two
5

types of experiments, the authors in [17] concluded that phenolphthalein diffused for a
distance of 2 mm in the paste in the first day of hydration and very little afterwards.

Measurements of X- and -rays attenuation are established techniques to analyze moisture


profiles in concrete; however, these techniques reveal density differences and are not very
sensitive to water, which has a comparatively low density. Since the amount of curing water
moving from the water reservoirs to the cement paste is very small, these techniques are
generally associated with large scatter. 1D X-ray absorption was applied to study moisture
profiles in pastes with SAP [18] and with LWA [19]; in the latter study, a penetration distance
of the water from the LWA rim of at least 4 mm was measured. Three-dimensional x-ray
microtomography may provide an even more detailed view of water transport during internal
curing.

Magnetic resonance imaging was applied successfully to visualize water content of LWA [20]
and evolution in time of moisture profiles of LWA cast in cement paste [21]. With this
technique it is possible to obtain moisture profiles with sub-millimetre resolution [22].
Moisture profiles measured by proton-spin relaxation nuclear magnetic resonance possibly
offer the additional advantage of measuring both free and bound water at different locations.

An indirect measurement of penetration distance can be obtained by measuring autogenous


shrinkage reduction on mixtures with different spatial distributions of the internal curing agent
[23] (section 3.3). According to ref. [23], in the first days of hardening, internal curing water
penetrated from water-saturated LWA into the cement paste up to a depth of several mm,
which is consistent with measurements by other techniques. Moreover, in cement pastes with
low w/c or addition of silica fume, reduction of permeability of the cement matrix decreased
the penetration depth. However, if local expansion occurs in the internally-cured cement paste,
this would complicate the calculation of the penetration of the curing water from the reduction
in overall shrinkage of the concrete.

~1 mm

Figure 3. Coloured corona expanding around a LWA (Liapor) aggregate saturated with weak
ink solution and cast in white Portland cement paste of water/cement ratio 0.3 [16].

3.3 Autogenous deformation


Since emptying of the capillary pores in internally water cured cement paste is compensated by
the water reservoirs, lower tensile stresses develop in the capillary water and self-desiccation
6

shrinkage is consequently reduced [24]. Internally water cured concrete might even expand in
the first days after casting [4, 16]. Reduction of autogenous shrinkage is not only a proof of the
effectiveness of internal water curing, it is also its most beneficial practical consequence [25].
It results in lower self-induced stresses during restrained hardening and in reduced risk of
cracking of structures made with low w/c concrete (section 4.4).

However, the internal water curing agent itself may affect the deformability of the concrete
and thus influence the shrinkage in ways other than providing a water reservoir. For instance,
in LWAC, where large amounts of LWA are introduced in the concrete mixture, the elastic
modulus of the concrete is reduced. This may potentially increase the shrinkage of the
concrete, if some shrinkage of the cement paste is taking place despite the internal water
curing.

Reduction of autogenous shrinkage or occurrence of expansion in sealed specimens were


measured by several authors on mortars and concrete containing LWA [3, 16, 26-33] and on
cement pastes and mortars with SAP [3, 4]. All these measurements of autogenous
deformation were linear and started around setting or after 1 day, depending on the measuring
technique.

4 Secondary consequences of internal water curing

4.1 Mechanical properties


Increased degree of hydration in concrete with internal water curing is expected to improve its
mechanical properties, especially at later ages. An additional beneficial effect on mechanical
properties is obtained by avoiding internal microcracking (section 4.4), which may occur in
low water/binder concrete due to autogenous shrinkage.

Evaluation of the influence of internal water curing on mechanical properties is complicated by


the fact that the internal curing agent is introduced in the system and will influence its
performance. As a consequence, increasing the amount of the internal curing agent will reduce
the strength, counteracting the beneficial effects of the further hydration promoted by internal
water curing. Moreover, strength is also sensitive to the moisture state of the specimens, with
moist concrete showing lower strength than partly dry concrete. Also the pre-compression of
the aggregates, which might take place in high strength concrete due to autogenous shrinkage
[34], plays a role in the strength of the concrete.

In addition, in LWAC a strength ceiling exists that depends primarily on the strength of the
LWA and is independent of the matrix [35, 36]. On the other hand, stress homogeneity in
LWAC, due to similar elastic modulus of aggregates and cement paste [35], might reduce the
occurrence of internal microcracking compared to concrete with normal aggregates.

Increase of compressive strength or flexural strength in comparison with normal concrete,


especially at later age, was observed in concrete with LWA [14, 16, 37] and in mortar with
SAP or LWA [3]. In [14], addition of pre-wetted LWA to the mix produced concrete with
compressive strength continuously increasing up to 1 year and insensitive to curing conditions.
On the other hand, in one study, moist LWA lowered the compressive strength of LWAC
compared to dry LWA [26], probably because the w/c of the concrete was increased. In the
same study, elastic modulus of LWAC was not affected by water content of the LWA.
7

4.2 Porosity and pore size distribution


Increased degree of hydration in internally water cured concrete leads to a decrease of the
porosity. Theoretically, a low w/c cement paste with sufficient internal curing water may
hydrate until all capillary pores are filled with hydration products [13]. This will reduce the
total porosity of the cement paste and refine it: ideally, only gel pores will remain in the
cement paste.

Porosity and pore size distribution of internally cured concrete may be measured by a number
of techniques, for instance by water vapour sorption isotherms or image analysis based on
scanning electron microscopy. Measurements should preferably separate the porosity and pore
size distribution of the internal curing agent from those of the cement paste.

Porosity of the matrix in concrete containing LWA was measured by helium pycnometry after
crushing of the concrete and removal of LWA, showing a decrease between 180 and 360 days
[14]. On the same mixes, mercury intrusion porosimetry performed on pieces containing only
sand grains and cement paste showed refinement of the porosity in the same period.

Combined fluorescent microscopy, micro hardness measurements, and image analysis based
on backscattered-electron scanning microscopy [38, 39] showed lower porosity and greater
hardness of bulk cement paste in samples containing saturated-surface dry LWA compared to
paste with normal aggregates and plain cement paste.

4.3 Interfacial transition zone


Densification of the interfacial transition zone (ITZ) is supposed to occur when internal water
curing is performed with LWA. Water from the LWA will promote local hydration of the ITZ,
which will generally be denser compared to concrete with normal aggregates.

Scanning electron microscopy and energy-dispersive X-ray analysis have shown that cement
paste penetrates in the outer porous layer of the LWA particles, contributing to a paste-
aggregate bond stronger than with normal weight aggregates [40-42]. In particular, a dense and
homogeneous ITZ for LWA with a porous outer rim was observed, while for LWA with a
dense outer layer the ITZ was similar to the case of normal weight aggregates [43]. Internal
water curing ensures water saturation of the concrete and promotes the pozzolanic reaction at
the interface between LWA and paste, which may further contribute to strengthen the bond
[44, 45]. Kato et al. [38, 39] used fluorescent microscopy, microhardness measurements, and
scanning electron microscope image analysis to study internally cured samples with wet LWA
and samples with no internal water curing. Lower porosity and greater hardness were
measured in a 100 m-wide region around the saturated LWA (Figure 4). Indirect evidence of
the existence of good bond between LWA and cement paste is shown by the fact that cracks
generally propagate through aggregates instead of along their rim as would be the case with
normal aggregates. An example of this is shown in [46], where through-aggregate cracking
was observed by light microscopy on epoxy-impregnated samples subjected to severe drying.
Improvement of ITZ when using LWA is a highly debated subject, and there have been also
observation of poor ITZ attributed to air escape from dry LWA [47] or to insufficient water
content of the LWA [16].
8

Figure 4. Fluorescence microscope images of interfacial transition zone between cement paste
and normal weight aggregate (left) and saturated LWA (right) [39]. The darker interfacial
transition zone in the right picture indicates lower porosity and thus better bond.

4.4 Self-induced stress and cracking


If autogenous shrinkage of a cement paste is reduced, self-induced stresses produced by
restrained deformation will also decrease. Both the global stress acting on a concrete structure
and the local stress at the paste-aggregate interface will be affected. A direct consequence of
this is the reduced probability of macroscopic concrete cracking; moreover, the likelihood of
internal microcracking will also be reduced [46].

Additionally, in LWAC the elastic modulus of the concrete will generally be lower due to the
LWA and this will concur to reduce the global self-induced stresses. Moreover, the low
modulus of the LWA will also contribute to reduce the local stresses at the paste-aggregate
interface and the probability of internal cracking [35, 46]. Fluorescent microscopy and
microhardness measurements in the ITZ, already addressed in section 4.3, may also be used to
reveal reduction of interface microcracking in internally cured samples with LWA [39].

Many authors have measured self-induced stresses of concrete mixes containing LWA, mostly
using linear stress rigs [16, 28, 29, 31]. In all cases, the self-induced tensile stresses were lower
than in the reference concretes without internal water curing and the likelihood of early-age
cracking was reduced; in some cases, compressive stresses were measured at early age. Jensen
& Hansen [4] observed self-induced stress reduction in mortars with SAP by measuring
equivalent hydrostatic pressure in an annular shrinkage gauge (ring test). Mortars with SAP
did not crack while the reference mix did.

Direct measurements of the self-induced stress at the paste-aggregate interface can be


performed with a stress sensor [34], whose application to concrete with internal water curing is
straightforward.

According to [48], a higher internal relative humidity in concrete with internal water curing
would reduce the thermal expansion coefficient, thereby reducing stress development in
structures subjected to real, i.e. semiadiabatic, temperature regimes. However, evaluation of
9

this stress reduction is complicated by the superposition of autogenous and temperature-related


deformations, and can hardly be used as an indication of the effectiveness of internal curing.

4.5 Durability
A number of observations of the good durability of LWAC in extreme environmental
conditions may be attributed at least in part to the beneficial effect of internal water curing. On
the other hand, long-term observations of the durability of internally-cured high performance
concrete with either LWA or SAP are not available because of the novelty of the technique.
Many of the aspects discussed in the previous sections may potentially contribute to enhanced
durability of concrete with internal water curing: in particular high degree of hydration, low
porosity, reduced internal stresses, less cracking, and densification of the ITZ.

A reduction in permeability and diffusivity may be expected in internally water cured concrete,
especially at later age, due to depercolation of capillary pores in the cement paste (section 4.2).
However, an additional pore system is introduced into the concrete with the two available
techniques for internal water curing, SAP and LWA. Mathematically, it is possible to prove
that inclusion of a discontinuous phase has a minor influence on the diffusion properties of a
material [49]. As a general remark, permeability and diffusivity of LWAC appear to be
controlled more by the quality of the matrix than by the LWA [36], but the influence of
internal water curing on permeability and diffusivity is not fully clarified.

With regard to freeze-thaw durability, an advantage of concrete with fine LWA might be the
presence of a well-dispersed pore system, which may assist the air-entrainment pore system
[50]. In laboratory freeze-thaw testing programs, LWAC performed equal to or better than
normal weight concrete [50, 51]. For this particular purpose, SAP may be an even better
option: the pore system introduced with SAP for the scope of internal water curing can be
designed to work also as an air entrainment system when the pores have been emptied [4].

Cores taken from the U.S.S. Selma, a 70-year-old LWAC ship, and from the Chesapeake Bay
Bridge in Virginia [52] have demonstrated concretes with high integrity contact zone between
aggregates and matrix. Figure 5 shows a LWAC ship passing under a LWAC bridge during
World War II. These examples illustrate early applications of LWAC in extreme
environmental conditions that have demonstrated a surprisingly good performance over time.
10

Figure 5. Ship with hull made of lightweight concrete passing under lightweight concrete
bridge deck during World War II [52].

6 Final remarks

This paper provided an overview of evidences of internal water curing and experimental
methods to study them. In almost all cases, the experimental techniques reported or suggested
are well established in concrete material science and only minor adaptations or special care are
needed to extend their area of application to internal water cured concrete.

It is believed that a more quantitative foundation of the internal water curing concept should be
pursued through the application of scientifically-sound investigation techniques. This will
promote the acceptance and spread the use of internal water curing in concrete practice.

7 Acknowledgements

This paper was prepared for the RILEM Technical Committee TC 196-ICC, “Internal Curing
of Concrete”. The authors thank Prof. Konstantin Kovler (chair of TC 196-ICC), Mr. Dale
Bentz, and Prof. Erik Sellevold for their suggestions and insightful comments and Mr. Thomas
Holm for providing the picture shown in Figure 5.

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