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Creep Behavior of Cement Paste, Mortar, and Concrete: The Role of

Relative Humidity and Interface Porosity

L. Sorelli1; J. Frech-Baronet2; and J.-P. Charron3

1
Civil Engineering, Université Laval, 1065 avenue de la Médicine, PLT2928-A. E-
mail: luca.sorelli@gci.ulaval.ca
2
Civil Engineering, Université Laval, 1065 avenue de la Médicine, PLT2928-A. E-
mail: jessy.frech-baronet.1@ulaval.ca
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3
Civil, Geological, and Mining Engineering, Polytechnique Montreal. E-mail:
jean-philippe.charron@polymtl.ca

Abstract

Delayed deformations in concrete under sustained loading may depend on complex

chemo-hydro-mechanical phenomena. Generally, the creep deformation of a cement
paste is distinguished in the short-term and long-term. Simply speaking, the former
can be associated to the diffusion of gel water in pores and cracks and it is mainly
volumetric (i.e., volumetric deformation), reversible, and bounded. The latter can be
associated to the sliding of the sheets of Calcium-Silicate-Hydrate (C-S-H), which is
mainly deviatoric (i.e., shape deformation), irreversible and with an unbounded
asymptotic deformation. From an experimental point of view, recent studies have
shown that microindentation is a powerful technique to quickly characterize basic
creep thanks to the reduced characteristic time of a sample size of few micrometers.
The objective of this project is twofold: (1) investigating the effect of relative
humidity on the creep behavior by microindentation; (2) characterize the viscous
behavior of the interface transition zones (ITZ) around a rigid inclusion. In particular,
the project investigated two different relative humidity, 33% and 85%, by considering
both creep and relaxation microindentation tests. The presented results show the
effect of the moisture content on the creep behavior of cement paste both at short and
long terms. In addition, the results showed that the ITZ zone around an aggregate
showed higher creep than the bulk cement paste. Those results provide new insights
to understand the role of water and interface porosity on the creep mechanisms of
concrete.

INTRODUCTION

Creep can have beneficial as well as negative effects on concrete structure.

For stress-to- strength ratio lower than 40%, compressive creep is considered linear
and it is usually additively split into the basic creep (i.e. no moisture transfer) and the
drying creep components. Creep in concrete is influenced by many factors, such as
the microstructure constituents, the porous network, the type of curing, the
temperature and relative humidity, and the loading time. Bernardi et al. employed a
triaxial load cell test to show that the short term creep is mostly volumetric, while the
long term creep is mostly deviatoric hinting on the coexistence of different
mechanisms (Bernard et al. 2003). The mechanisms which are mostly recognized for

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explaining concrete creep can be broadly classified as follows: (i) gel water diffusion
theory (Powers 1965); (ii) sliding of C-S-H sheets (Vandamme et al. 2009; Sanahuja
et al. 2010); (iii) gel compaction like a secondary consolidation process. More
recently, Sahidi et al. (Shahidi et al. 2014) have recently described the kinetics of the
creep by considering a viscous interface model which accounts for the lubricant role
of water. As for non linear creep is considered, Rossi et al. have lately proposed that
the interaction between the hygral gradients and the micro-cracks at the tip of
propagating cracks may play an important role in the creep deformation under
sustained loading (Rossi et al. 2012).
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The role of relative humidity on concrete creep is recognized to be of

paramount importance. However, the experimental results available in literature are
sometimes contradictory as the initial hygral conditions within the sample is often not
uniform since the hygral equilibrium within a sample of few centimeters can take
several months (Neville 1971). The compressive creep test of Troxell et al. over 30
years on concrete cylinders of 100 mm diameter and 150 mm height showed that,
after the hygral equilibrium has been reached at about 1 year, the rate of creep seems
quite independent of the relative humidity (Troxell et al. 1958). Contrarily, Bazant
proposed a parabolic relationship between the basic creep and the relative humidity
(Bazant et al. 1985) based on the experimental results of Wittman on millimeter size
samples (Wittmann 1968). Such apparent contradiction may be explained by the
difficulty, if not impossibility, of decoupling basic and drying creep within the
microstructure. The overall coupling was quantified by L’Hermite (L'Hermite 1959)
which assumed that the drying creep is covariant (i.e., multiplicative) with respect to
the shrinkage and the basic creep. Nowadays, microindentation technique have been
emerging for measuring the creep properties of cement-based materials as it allows
significant reduction of the time scale for observing creep phenomena (Nguyen et al.
2013; Pourbeik et al. 2013; Nguyen et al. 2014). Zhang et al. have proven that, for
several mix designs, the long term creep rate measured by microindentation and the
ones measured by compressive tests over 30 years are linearly correlated (Zhang et al.
2013). Furthermore, Zhang (Zhang 2014) recently showed that the relative humidity
can increases the long term creep rate by a factor of 5 when the relative humidity
level increases from 11% to 95%.
The scope of this work is to better understand the effect of humidity on the
short term and long term creep mechanisms. Does the relative humidity modify the
creep response of a cement paste? Does creep and relaxation behave as dual
mechanisms? Does the aggregate interface contribute to the overall creep?

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MATERIALS AND METHODS

Materials

This study employed a cement paste and a concrete made with ordinary
Portland (type I) with water-to-cement ratio (w/c) of 0.4. The concrete mix design
was adapted to have the same matrix characteristics of the cement paste. The samples
were cast in cylinder molds of 100 mm and 150 mm diameters. They were then cured
at 100% R.H for 28 days and then stored at 50% RH for 2 months. The samples were
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tested 90 days after casting to reduce the effect of aging. Before testing, a cubic
sample of 30 mm side was cut out from the center of cement paste and concrete
cylinders. Secondly, a coarse grinding was performed with the used of abrasive paper
and water in order to smooth the edge of the samples. Thirdly, the surfaces were
polished by 1 μm fineness diamond suspension oil-based solution. Finally, a 0.250
μm fineness diamond paste serve to finalize the polishing. Special attention was paid
to keep the samples leveled since the angle of indentation could influence the results
of measurement. After polishing, the samples were put in an ultrasonic bath to
remove any trace of diamond particles left on the surface. The sample were cured for
2 weeks at the testing relative humidity before microindentation testing which is
enough to guarantee the hygral equilibrium of the micrometer zone under testing.

Humidity Chamber

In order to control the relative humidity (RH) and CO2 concentration, an

hermetic enclosure was built specifically for this research project. The system
consists of a closed circuit where the hermetic enclosure is connected in series to an
Erlenmeyer flask containing a saturated salts solution and a pump. The use of
saturated solution of salt is required to reach specific humidity equilibrium (Table 3.
for details). The system being a hermetic closes loop allows the air to pass multiple
times through the saturated salts solution. The relative humidity and CO2
concentration are continuously monitored by two sensors within the chamber. In this
work different relative humidity, such as 33% and 85% were considered.

Table 1. Salts used to control the relative humidity

Solubility in water
Salts RH at 20°C
(g/100mL)
Lithium Chloride (LiCl) 11.3 ± 0.3 84.25
Magnesium Chloride ( MgCl2 ) 33.1 ± 0.1 54.3
Magnesium Nitrate ( Mg ( NO3 )2 ) 54.4 ± 0.2
125.0
Potassium Chloride (KCl) 85.9 ± 0.3 34.4
Lithium Chloride (LiCl) 11.3 ± 0.3 84.25

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Surface roughness

The sample surface were carefully prepared for cement paste and concrete specimens
according to a well established protocol (Miller et al. 2008). The Roughness Mean
n n
Square (RMS), which is a statistical parameter defined as follows Rq 2 = 1 n 2  zij2
j =1 i =1

where i and j are the position of each pixel in a plane, was checked by Atomistic
Force Microscope (AFM). Topographic images were carried out on three different
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zones: the inclusion (granulates/sands) zone, the ITZ and the paste zone. A Gaussian
filter was applied to filter out the wave larger than 8.0 μ m (Miller, Bobko et al.
2008). The Rq value was obtained by averaging three selected topographic area of 50
μm by 50 μm per zone of interest. The Rq for the cement paste was about 65 ±36 nm,
while the Rq for the ITZ was about 56 nm±31 nm (Figure 1).

(a) (b)
Figure 1. AFM imag: (a) cement paste wit average Rq=65 nm; (b) ITZ with
average Rq=56 nm.

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Basics of microindentation

Microindentation has become a powerful technique to quantitatively measure

the elasticity and hardness of cement paste and other hydrates products (Nguyen,
Alizadeh et al. 2013; Pourbeik, Alizadeh et al. 2013; Nguyen, Alizadeh et al. 2014).
During an indentation test, the force (P) and the penetration depth (h) are measured
simultaneously, while the indenter tip penetrates into the film (Figure 2a). A typical
P-h curve (Figure 2b) is constituted by a loading curve up to the maximum load Pmax,
followed by an unloading curve. Note that the loading curve profile parabolic in the
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ideal case of conical indenters with no friction on the tip-material interface. For this
study we employed a Berkovich-type indenter which is three-sided pyramid with an
equivalent cone semi-angle θ of 70.3º as shown in Figure 2a. The analysis of the P-h
curve consists in extracting the indentation properties, such as: the indentation
( )
Modulus M = S π ( 2β AC ) and the indentation Hardness H = Pmax /AC. The
coefficient β accounts for the non symmetrical shape of the indenter. The projected
area AC of the indenter-sample contact depends on the contact depth hc (Figure 2.a).
The contact stiffness S=dP/dh is the slope measured during the initial stages of the
unloading curve (Figure 2.b). The Young modulus E of an isotropic material is
estimated from the indentation modulus M as follows :
M = (1 − υ ) E + (1 − υ ) Ei , where Ei and νi are the elastic modulus and the
−1 2 2

Poisson’s ratio of the diamond tip, which are equal to 1141 GPa and 0.07,
respectively; while E and ν are the Young modulus and the Poisson’s ratio of the
material, respectively. Furthermore, to account for the tip imperfection, the contact
area function, AC = π 2 a , is calibrated according to a standard procedure on a
reference fused silica sample. It is usually estimated by the Oliver and Pharr method
with the next equation AC = 3 3hC2 tan 2 θ , where hc = hm − ε Pmax S . The geometry
correction factor β and the intercept factor ε are 1.034 and 0.75, respectively, for
Berkovich-type indenter (Fischer-Cripps 2011).
Figure 2c shows an experiment where the load is linearly applied over a time
τL, then held constant over a time τH, and finally reduced to zero over a time τU.
While plastic deformation often occurs during loading, it is generally assumed that
the unloading curve is elastic. Different coefficients have been defined to describe the
creep mechanism from an indentation tests. As for a creep microindentation test, the
asymptotic creep behavior ( t → ∞ ) can be characterized by the Long Term (LT)
contact creep modulus C LT proposed by (Vandamme and Ulm 2009), which
essentially describes the logarithmic asymptote of the creep rate, as follows
def
1 Pm P
CLT = lim t →∞  = lim t →∞ 
= m [GPa] (1)
t L(t) t 2a h 2 au x1
U

where the indentation compliance L(t) = M(t)−1 , x1 is the term of the logarithmic
penetration depth function. h ( t ) = x1log ( t τ ch + 1) which is employed to fit the creep
curve. We remind that aU is the radius of the contact area at unloading, which is

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supposed to be rather constant during the holding time. Vallée et al. (Vallée 2013)
proposed to normalize CLT by the initial indentation modulus as follows
def
C P
cLT = LT = β m [ −] (2)
M0 S x1
Notably, cLT is independent of the elastic stiffness of the material and the radius of
the contact area.
P hmax
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(a) P (b) (c)

Pmax h
P
Pmax  dP 
S =  Pmax
 dh  hmax
1
hmax
h h
c θ Ac

h f hf hmax t
τL τH τU
(a) (b) (c)
Figure 2. Indentation test (a); Curve P-h (b); Curves P-t and h-t for a creep
microindentation test.

Herein, we define a contact Short Term (ST) creep modulus which describes the very
short term creep as the asymptotic behavior right after the load is applied ( t → 0+ ) as
follows
 
def
M (t) P(t) P τ
cST = limt →0 = limt →0 = β m ch = τ ch cLT [−] (3)
M0 Pm S x1
As for the relaxation indentation test, Vallée et al. (Vallée 2013) defined a
dimensionless Long Term (LT) contact relaxation modulus r∞ for describing the
logarithmic asymptote as follows
def
M P P
rLT = limt →∞ −  0 = limt →∞ −  m = m [−] (4)
t M (t) t P(t) x '1

where x1 is the term of the logarithmic penetration depth function,

ΔP ( t ) = − x '1 log ( t τ 'ch + 1) which is employed to fit the creep curve. As for the short
term relaxation behavior, we define here a contact Short Term (ST) relaxation
modulus as follows:
def
M P P τ'
rST = lim t → 0 −  0 = lim t →∞ −  m = m ch = τ ch' rLT [ −] (5)
M (t) P (t) x '1

The experimental tests are carried out as following. First a 5 x 5 grid of micro-
indentation tests was performed on the cement paste for each relative humidity for
both test condition, i.e., creep and relaxation. To check the repeatability the creep test
series were repeated. Then, the ITZ zone was characterize by creep microindentation

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tests over a grid of 5 lines of 20 indentation points in the proximity of the

inclusion/cement paste interface at a relative humidity of 35%. The distance of each
point from the interface was calculated by digital microscope. The results were
averaged for indentations separated in groups according to the distance from the
interface, such as: <20 μm, 20-40 μm, 40-60 μm, 60-80 μm and >80 μm.

RESULTS
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The average results for the test series of creep and relaxation for different relative
humidity are summarized in Table 2 in terms of indentation modulus M and hardness
H. Figure 3 shows an example of indentation grid for the cement paste tested at 35%
with the mapping of the indentation Modulus M and Hardness. As average, at lower
humidity the material is slightly stiffer (+10%) and harder (+25%). Notably, those
results confirm the previously one obtained by Zhang (Zhang 2014). Table 3. shows
the results of the creep and relaxation tests on the cement paste at different relative
humidity. Figure 4a shows the average creep curve penetration depth vs. time (h-t) for
the different relative humidity. Figure 4b shows the average relaxation curve load vs.
time (P-t) for the different relative humidity. A variation of humidty from 35% to
85% causes a reduction of the creep modulus CLT of a factor between 2 and 3 (i.e.,
the creep increase). This result is again coherent with the results of Zhang (Zhang
2014). The effect of varying the humidity from 35% to 85% strongly increases the
short term creep modulus cST , which means the short term creep reduces when the
humidity is higher. Notably, those observations are confirmed by the relaxation tests
for which the contact relaxation modulus ( rLT ) reduces of about 100% when the
humidity is increased from 35% to 85%, i.e., creep doubles. Analogously to the creep
tests, the short term contact relaxation modulus ( rCT ) increases when relative
humidity increases, i.e., the short term creep reduces. Table 3 shows the depth rates
calculated over a period of 3 seconds.
Table 2. Mean results of microindentation for all the test series.
Indentation Indentation
Modulus [GPa] Hardness [MPa]
Creep test at 35% r.h. 14.3 214.6
Creep test at 35% r.h. 12.0 191.0
Creep test at 85% r.h. 13.3 187.6
Creep test at 85% r.h. 11.5 153.0
Relaxation test at 35% r.h. 15.5 202.6
Relaxation test at 35% r.h. 13.3 212.8
Relaxation test at 85% r.h. 13.1 135.8
Relaxation test at 85% r.h. 11.6 115.8

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(a) (b) (c)

Figure 3. Example of indentation grid on the cement paste for r.h.=33% (a);
mappingof the M-modulus (b); mappring of the Hardness (c).

Table 3. Mean results of creep and relaxation test on cement paste for different test series.
Creep tests at Pm=8N Relaxation test at hm=40 μm
CLT τ ch cLT cST dh rLT τ 'ch rST dh
R.H. -3
¶ [GPa] [sec] [-] [-]10 dt [-] [sec] [-] dt
-3 -3 -3
10 [μm/sec] 10 10 [μm/sec]
t=0 t=300 t=0 t=300
35% 141 5.2 10 52 385 0.6 41 0.02 1 -710 -0.58
35% 98 13.5 8 110 434 1.0 35 0.20 7 -645 -0.66
85% 57 114.9 4 495 488 1.8 18 0.71 13 -832 -0.73
85% 45 84.7 4 334 560 1.8 19 0.45 9 -694 -0.64

(a) (b)
Figure 4. Effect of the relative humidity on the mean response of a cement paste
by microindentation: creep response (a); relaxation response (b)

The characterization of the ITZ in concrete samples is summarized Table 4. Figure 5

shows the indention grid on the interface aggregate-cement paste as well as the
average creep curves for points within different distance ranges. It is evident that
there exists a weakened zone of about 60 μm with reduced M and H likely, which is
likely due to a greater porosity. As for creep, the ITZ zone showed a reduced CLT with

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respect to the point far away (>80 μm) which means that the creep rate of the ITZ
zone can be up to twice that of the bulk cement paste.

Table 4. Average microindentation properties of the ITZ zone for creep tests at Pm=50 mN.
Distance τ ch dh
hm M H CLT cLT cST
from [sec] dt
[μm] [GPa] [MPa] [GPa] [-] [-]103
inclusion 10-3 [μm/sec]
t=0 t=300
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<20 μm 2.4 16.2 250 157 16.2 10 34 290 32

20-40 μm 2.4 19.8 409 242 19.8 12 22 558 26
40-60 μm 2.1 26.3 556 259 26.3 10 53 188 24
60-80 μm 2.3 24.1 425 266 24.1 11 6 1928 26
>80 μm 2.2 24.9 476 333 24.9 13 31 434 21

(a) (b)
Figure 5. Grid microindentation on ITZ of an aggregate (a) Average creep
curves at different distance zone from the interface (b).

CONCLUDING REMARKS

This works present an original characterization of the creep of cement paste

and ITZ of concrete by microindentation at various relative humidity (35% and 85%).
The preliminary conclusions are drawn:
(1) The indentation modulus of cement paste is slightly greater for low
humidity. The hardness is significantly greater for low humidity;
(2) The cement paste shows greater creep rate at higher humidity 85% as
confirmed by both creep and relaxation results;
(3) The ITZ of 60-80 μm around an aggregate presents a lower stiffness and
hardness and is more viscous that the bulk matrix.
The research is being extended to other relative humidity levels to statically confirm
the present results.

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REFERENCES

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L'Hermite, R. (1959). What do we know about the plastic deformation and creep of
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