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Construction and Building Materials 169 (2018) 403–413

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Construction and Building Materials


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

Effect of curing humidity on the fracture properties of concrete


Zhengxiang Mi, Yu Hu, Qingbin Li ⇑, Zaizhan An
State Key Laboratory of Hydroscience and Engineering, Tsinghua University, Beijing 100084, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 Fracture properties of concrete were


investigated under different
conditions.
 At early age, fracture parameters
remained almost constant during
drying.
 At later age, fracture parameters
decreased markedly with decreasing
curing humidity.
 Fracture mode changed from ductile
to brittle with reduction in curing
humidity.

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

Article history: This study investigates the influence of curing humidity on concrete fracture properties. Concrete fracture
Received 2 November 2017 energy, effective fracture toughness, and characteristic length were tested at five different ages using
Received in revised form 24 February 2018 wedge splitting specimens exposed to four different relative humidity values (30%, 50%, 70% and 98%).
Accepted 1 March 2018
Four environmental chambers capable of automatically controlling temperature and relative humidity
were constructed. A data averaging method for companion specimens was introduced. The test results
show that at the early age, fracture energy, effective fracture toughness, and characteristic length
Keywords:
remained almost constant during drying. As time elapsed, however, the influence of curing humidity
Fracture properties
Wedge splitting test
on the concrete fracture properties became increasingly pronounced; larger values of fracture energy,
Relative humidity effective fracture toughness, and characteristic length were measured by concrete specimens kept at high
Failure mode humidity. The concrete fracture mode also gradually changed from ductile to brittle with curing humidity
decreasing and hydration time elapsing.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction curing conditions owing to climatic variations. This results in the


formation of moisture gradients in concrete structures because of
Concrete is the most common structural material used in the water evaporation to the surroundings at lower relative humidity
modern times. It is often poured and operated in different environ- levels. The extent and severity of moisture gradients depend on
ments. Therefore, concrete structures face continuously changing many factors, such as ambient air relative humidity, temperature,
local rainfall, wind speed, and age at exposure. The properties of
⇑ Corresponding author. concrete are also impacted by curing conditions [1,2].
E-mail address: qingbinli@tsinghua.edu.cn (Q. Li).

https://doi.org/10.1016/j.conbuildmat.2018.03.025
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
404 Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413

Many studies investigated the effect of moisture gradient on the by the specimens cured at decreased relative humidity. With
behavior of concrete, and the results show that the reduced curing regard to the elastic modulus, Beaudoin et al. [17] observed that
humidity not only can negatively affect the hydration reaction and the static elastic modulus in compression decreases significantly
microstructural behavior of concrete, but can also seriously deteri- with reducing relative humidity, especially below 20% RH. Further-
orate its mechanical and fracture properties [3–5]. Powers first rec- more, they also reported that the elastic modulus shows a non-
ognized that cement hydration slows down at low internal relative linear response with respect to the relative humidity and that it
humidity and almost stops below approximately 80% RH [6]. In depends on the drying history. This is also confirmed by Alizadeh
other words, due to desaturation and the corresponding reduction et al. [18], who also reported that concrete would lose elastic mod-
of the internal relative humidity in the pores of a cementitious ulus if exposed to reduced humidity and hypothesized that such
material, cement hydration may nearly come to a halt and the reduction could be attributed to micro-cracking and other micro-
development of concrete properties may be hampered, even scale phenomena such as high porosity. Moreover, Yalcinkaya
though the system still includes considerable amount of water. and Yazici [19] studied the effect of relative humidity on the drying
This indicates that the development of various properties of con- strain and showed that the shrinkage of concrete, compared to that
crete structure depend on the available water, and if the structure at 100% RH, was increased by 33%, 46%, and 52% under 70% RH, 60%
is exposed to very low humidity, its surface hydration will cease RH, and 50% RH, respectively.
and strength and durability will decrease, which may cause surface However, very limited information is available on the fracture
cracking and may not afford the desired protection. This will grad- properties of concrete exposed to low humidity. Bazant et al.
ually hamper the hydration of the internal parts of concrete struc- [20] and Lau et al. [21] investigated the effect of moisture on the
tures, as the pore water is also lost through the drying surface. fracture properties of hardened concrete. They showed that both
Later, other researchers also observed a similar phenomenon. For the fracture energy and fracture toughness decrease with the
instance, Snyder and Bentz [7] found that the hydration of a increasing moisture, and they supposed that the degradation of
cement paste at 90% RH was lower than that under saturated con- fracture properties of concrete under moisture can be attributed
ditions. In particular, Jensen’s experimental results [8] revealed to internal pore water pressure, which would cause a very high dis-
that the hydration degree of C3S was about 67% after 365 days at joining pressure between the contacting cement pastes. In particu-
98% RH, but only about 4% when kept at 85% RH for 365 days. lar, data about the effect of curing humidity on the development of
The hydration degree was even smaller at a lower relative humid- concrete fracture parameters over time and long-term fracture
ity, and nearly no hydration took place below 43% RH. On the other properties have been barely reported to date.
hand, Flatt et al. [9] theoretically proved why C3S cease to hydrate Therefore, the objective of this study is to investigate how cur-
below 80% RH, and showed that this phenomenon is caused mainly ing humidity affects the development of fracture properties of con-
by the reduced water activity, which changes the solubility of C3S crete with age. Four different curing conditions were considered
so that it is in equilibrium with the pore fluid. Du et al. [10] simu- with a constant temperature of 20 °C under different relative
lated the reduction in the reaction rate caused by decreased humidity levels. The fracture parameters were measured after 3,
humidity, in which the hydration rate reduction factor indepen- 7, 14, 28, and 60 days.
dent of temperature and hydration degree was 1.0 at 100% RH
and it decreased to smaller values at lower humidity levels.
2. Experimental program
Regarding the influence of reduced relative humidity on con-
crete microstructure, Cong and Kirkpatrick [11] observed that the
2.1. Materials
polymerization of C-S-H does not change when the relative humid-
ity was varied from 9% to 100%; however, its local structure
The concrete mix proportions are listed in Table 1. The cement
becomes more disordered with decreasing relative humidity. Using
used was type I ordinary Portland cement with a density of 1450
nuclear magnetic resonance spectroscopy, Aparicio et al. [12]
kg/m3. The fine aggregate utilized was natural river sand with a
observed that the samples cured at 70% RH presented more tetra-
fineness modulus of 2.52, conforming to ASTM C33/C33M No.2.
hedral coordinated aluminum than those cured at 98% RH because
The crushed basalt passing the 20 mm sieve was applied as the
more aluminum was taken up by the C-S-H gel and the transforma-
coarse aggregate. Physical properties and gradations of the coarse
tion of AFt to AFm was promoted. Furthermore, the mean chemical
aggregate were examined using the test standards of ASTM C33/
reaction chain length of the C-S-H gel formed increased with
C33M No.67. The ratio of fine to total aggregate was 39% for all
decrease in curing humidity, and longer chains correspond to
concrete mixtures. The substitution rate of fly ash (ASTM Class A)
lower hydration degree. In addition, Sellevold and Bjøntegaard
was 25% for the total binder content, which was in order to reduce
[13] claimed that the thermal expansion coefficient of concrete
the heat of hydration for applications and save the cement. Potable
during maturation increase with decreasing humidity, where the
water was used for mixing concrete constituents and curing of the
reduction in humidity is owing to self-desiccation and/or drying
specimens. No further additive was employed. In order to achieve
of the environment.
better uniformity, the concrete was mixed for 6 min. In addition,
In general, the mechanical properties of concrete, both in term
an external vibrator was used for concrete compaction.
of strength and elastic modulus, decrease monotonically as a func-
tion of its curing humidity. Cebeci [14] showed that the compres-
sive strength of concrete reduced by 30% in 75% RH; and by 45% in 2.2. Specimen preparation and test set-up
33% RH as compared to the specimens cured in water. Saengsoy
et al. [15] found that the compressive strength of concrete cured Fracture tests were carried out on notched wedge splitting
in water and at 95% RH rapidly increased and became almost specimens. These specimens are characterized by a negligible
steady after 28 days. However, at 80% RH, the concrete strength influence of their self-weight on test results and by a considerably
develops slowly; especially at 60% RH, the strength hardly large fracture area to the specimen volume ratio, which is approx-
increased after 7 days, leading to a loss of approximately 41% in imately 4.6 times greater than that of a commonly used three-
the ultimate strength compared to those cured in water. It must point bending beam of equal volume [22]. However, compared to
be noted that Un and Baradan [16] concluded that the flexural a conventional wedge splitting test with one line support, two
strength is more sensitive to curing humidity than compressive hinge roller supports located at the center of the half section of
strength, and the smaller values of flexural strength are measured the specimens were utilized to improve their stability and to avoid
Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413 405

Table 1
Mixture proportions.

w/b Unit Weight (kg/m3)


Cement Fly ash Water Sand Gravel
/ / / 0–2.4 mm 2.4–5 mm 5–9.5 mm 9.5–16 mm 16–20 mm
0.4 351 117 187 701 11 316 612 155

unexpected failure of the specimens while preparing for the exper- inserting a steel plate inside the tensile face of a specimen with a
iment [23]. The principle of the test is schematically shown in constant thickness of 2 mm during concrete casting. The length
Fig. 1(a), where two steel loading devices with a roller bearing of the initial notch was 120 mm for each specimen, producing a
on each side were placed on the top of the specimen. A steel profile notch to height ratio of 0.4. The steel plates were carefully removed
with two identical wedges was fixed at the upper plate of the test- after approximately 4.5 h. A groove was made in the upper part of
ing machine. The wedges are pressed between the bearings, which the specimen to place two loading devices with a roller bearing and
leads to a horizontal splitting force. Neglecting the friction to attach the clip-gauge, where the size of the groove was big
between the wedge and the roller, the horizontal component act- enough to place loading devices and clip-gauge. Three identical
ing on the rollers can be evaluated using the following equation: specimens were prepared for each test age and relative humidity.
Although special care was taken while de-molding, moving, and
F
Fs ¼ ð1Þ placing the specimens, some specimens were still severely dam-
2 tan h aged in the notched section during handling. This is because the
where F is the applied vertical load; F s is the horizontal splitting notches are already present in low-strength concrete and also
force; h is wedge angle, which is equal to 15 in this test set up. because a splitting action may occur when the mold for the notch
The shape and dimensions of wedge splitting specimens is removed. For such damaged specimens, the reliable test results
employed in the experiments are shown in Fig. 1(b); the height may not be obtained; therefore, some spare specimens were also
of the specimens were larger than that used in the standard test prepared.
in order to obtain the fracture parameters independent of the size. All wedge splitting tests were carried out on an Instron testing
In particular, a single specimen height was adopted here because machine at five different ages (3, 7, 14, 28 and 60 days). The actual
the main purpose of our study is to investigate the influence of rel- experimental setup used is presented in Fig. 2. During the test, the
ative humidity on the fracture property of concrete rather than the primary deformation monitored was the crack mouth opening dis-
size effect. The concrete specimens were cast in steel molds, which placement (CMOD) which was measured with a clip-gauge having
were vibrated for at least 60 s in order to increase the density and an accuracy and capacity of ±0.0002 mm and 5 mm, respectively.
to eliminate air bubbles. The molds of the wedge splitting speci- The clip-gauge was mounted over the mouth of the initial notch.
mens were designed and manufactured as per the test require- All signals were continuously recorded by a commercial automatic
ments. Each mold was thoroughly cleaned, dried, and then date-acquisition system at rate of two readings per second. The
coated with a film of lubricating oil before any concrete was cast. loading actuator was controlled by the crack mouth opening dis-
The film of oil made it simpler to remove specimens from their placement with an initial rate of 0.04 mm/min. In the post-peak
molds once the curing process was complete. For all wedge range, the loading rate was gradually increased up to 0.08 mm/
splitting specimens, the initial notch (pre-crack) was created by min. This procedure was selected after several trials in order to

F 50mm

Wedge loading fixture


30mm

a0=120mm

300mm
tch
No

Roller bearing
Wedge
m
0m
12

300mm

(a) (b)
Fig. 1. Specimen for the wedge splitting test.
406 Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413

each relative humidity level during the period of curing. Since four
variations of relative humidity were used with five scheduled test-
ing ages and three companion specimens as a test group, the total
number of concrete wedge splitting specimens utilized in the
investigation was 60. Note that, in the following, ‘‘T” label repre-
sents the curing temperature, ‘‘RH” denotes the curing relative
humidity, and ‘‘A” indicates the age of curing unless otherwise sta-
ted. For instance, the specimen is labeled as T20RH98A3, whose
curing temperature, curing humidity and age are 20 °C, 98% RH
and 3 days, respectively.
After finishing, the concrete specimens were kept at ambient
conditions. The free surface of the molds was covered with an
impermeable plastic membrane to prevent desiccation in order
to reduce the influence of moisture gradients. When the concrete
specimens were allowed to set for 4.5 h, they become strong
enough to be removed from the steel plates and moved into their
corresponding curing humidity environment. For this, four equal
groups of concrete specimens together with their molds were
stored in four chambers with relative humidity levels that were
previously set to 30% RH, 50% RH, 70% RH and 98% RH and main-
tained there for 24 h. Subsequently, the specimens were removed
from the molds and shifted into the same chambers again and kept
Fig. 2. Actual wedge splitting specimen and test set-up.
as such until the time of testing. For the low-humidity specimens,
special care was taken while removing them from their molds
minimize the time needed to conduct experiment, as a result, the because of their slower hydration rate. This curing procedure
specimen completely failed in 30–40 min. Because of the use of a was adopted to ensure that all specimens had sufficient strength
very stiff computer-controlled servo-hydraulic closed-loop testing to avoid damaging while de-molding, moving and placing. Since
machine, the propagation of the main crack was well controlled, the setting time for the concrete was approximately 4.5 h, this pro-
and the complete load–CMOD curves were recorded using the cedure also guarantee that all specimens had the same properties
date-acquisition system. when the fracture parameters began to develop for a better com-
In addition to wedge splitting specimens, several companion parison. In other words, if the concrete specimens were exposed
cubes were also poured with the same batch of concrete to mea- to the corresponding relative humidity chambers immediately
sure the compressive strength and elastic modulus at 28 days for after mixing, they would achieve different degrees of hydration
each investigated humidity level. The dimension of each cube and microstructure before the fracture properties started to
was 100  100100 mm, which are in accordance with the Chi- develop, which would make the comparison more difficult [25].
nese standards DL/T 5150-2001 [24]. The mechanical properties Furthermore, the employed curing method also became more con-
were tested on an oil-pressure controlling testing machine, in sistent with practice, in which the effort is often made to maintain
which displacement control with a constant loading rate of 0.2 the curing condition for a certain period before exposure to the
mm/min of the jack displacement was adopted. The same speci- working condition. It must be emphasized here that the curing
mens were used to determine first the elastic modulus and then method of the cubes was the same as that of the wedge splitting
the compressive strength. After the elastic modulus was deter- specimens.
mined, the load was continuously exerted until the specimen After the desired curing period, the specimens were taken out
failed, thus obtaining the compressive strength of each specimen. from the chamber 3 h before the test and exposed to natural envi-
The compressive strength and elastic modulus were determined ronment until testing in order to ensure the relative humidity sta-
by averaging the test results of the four identical specimens, and bility during the experiment. At the ages of 3, 7, 14, 28, and 60
their values are presented in Table 2. days, the key fracture parameters of concrete were measured on
three companion specimens according to ASTM E 1820 [26]. The
averaged value of the three identical fracture specimens was used
2.3. Curing conditions to analyze the test data. For a given variable, however, if the devi-
ation between one replicate and the average of three companions
The curing temperature and relative humidity of the specimens was larger than approximately 10%, a spare specimen was tested
were automatically controlled by using four specialized chambers to increase the credibility of the test results.
capable of producing temperature between 0 °C and 80 °C and rel-
ative humidity between 30% RH and 98% RH. The maximum
humidity deviation and temperature deviation of the chamber 2.4. Data processing method for companion specimens
are ±2% RH and ±2 °C, respectively. Four different relative humidity
levels of 30%, 50%, 70% and 98% were used in this experiment to As mentioned above, three companion wedge splitting speci-
understand how curing humidity affects the concrete fracture mens were used for each test variable. However, because of the
properties with age. The temperature was controlled at 20 °C for diversity of individual specimens and the heterogeneity of con-

Table 2
Mechanical properties of concrete cured at different relative humidity.

Relative humidity 30% 50% 70% 98%


Compressive strength (MPa) 32.40 34.64 37.28 42.69
Elastic modulus (GPa) 24.77 26.72 29.01 34.36
Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413 407

crete, the experimental results in the same group might be differ- tion was not observable or not obvious before the load reached the
ent. Moreover, the averaged results are strongly dependent on the cracking limit of concrete. The initial slope of the ascending
method utilized to average the data. Therefore, in order to more branches increased with increasing age, because the strength and
accurately evaluate the fracture characteristics for each test, a data stiffness of concrete increases with age. Besides, the peak load also
process method was shown below. improved with time for all types of curing methods. For example,
For each wedge splitting specimen, approximately 3200 original in test specimens cured at 98% RH, the peak load increased from
data points were collected. At first, the points scattered far from 2.891 kN after 3-day curing to 5.014 kN after 60-day curing. This
the load-CMOD curve were filtered, and then one point was taken increase in the peak load also occured when the specimens were
about every 16 points in the load-CMOD curve in order to facilitate cured at low relative humidity, but the increased rate was smaller
the optimal fitting curve and make the curve more beautiful, where than that of the concrete cured at high humidity levels. Typically,
the number of data points could sufficiently represent the load- for the specimens cured at 30% RH, the peak load increased from
CMOD curve. Afterwards, in order to eliminate the influence of 2.714 kN after 3 days to 3.938 kN after 60 days.
fluctuation in the measurement, an average of three adjacent As the curing humidity was decreased, the peak load at each age
points (the given point and one point above and one below that reduced. Similarly, for a given curing humidity, the peak load gen-
point) was adopted. Subsequently, the filtered and averaged data erally increased significantly with the increasing age. For instance,
were imported into the mathematical software MATLAB and opti- at 60 days of curing age, the average peak load decreased from
mally fitted using rational function, with numerator and denomi- 5.014 kN at 98% RH to 4.373 kN at 70% RH, 4.092 kN at 50% RH,
nator degrees of 1 and 3, respectively. The correlation coefficients and finally to 3.938 kN at 30% RH with a final drop of 27.3%. Fur-
of regression curve R2 were more than 0.99 for all cases. The max- thermore, the curvature of the post-peak curve which reflected
imum load points of each specimen were obtained by averaging the property of the cracked specimen until breaking also depended
the peak points of the regression curve and measured curve whose on the curing humidity, and increased markedly with age. This was
fluctuation has been eliminated, which can further reduce the ran- related to the strengthening of the interfacial transition zone (ITZ),
domness and discreteness of the peak load. These average values where the stress concentration around the aggregate reduced and
correspond to the peak load (Fmax) and critical crack mouth open- new products in the ITZ pores showed increased crystallizations as
ing displacement (CMODc) of each specimen, respectively, and they the concrete became older. As a result, more aggregates were
are used to calculate the effective fracture toughness, as discussed pulled out from the matrix and the fracture path also transformed
later. gradually from around the aggregate to directly through the
When averaging the load-CMOD curve between the compan- aggregate.
ions, each data point in the load-CMOD curve should denote the
identical mechanical status. According to the equivalent elastic
3.2. Fracture energy
crack method, the fracture process zone is formed as the applied
load is increased, and the elastically equivalent crack extension
Fracture energy is defined as the energy required to create a
length reaches the maximum at the peak. After Fmax, the fracture
crack with unit surface area. For the wedge splitting specimen,
process zone begins to move forward along the crack path, keeping
fracture energy was calculated by the area under the measured
the maximum equivalent extension length [27]. Therefore, for each
load-CMOD curve divided by the ligament area, as shown in Eq.
specimen, 100 equally spaced CMOD values were evaluated from
(2). Since the complete failure of the wedge splitting test was
the zero point to CMODc and from the peak to the end point. It
approached asymptotically, the end point of the test was not easily
should be noted that the fracture test will never reach the loading
determined. Therefore, the test should be stopped at some point
level of zero since complete failure of specimen is approached
prior to the complete fractures, indicating that the measured work
asymptotically and the experiment is often stopped before total
of fracture does not represent the true fracture energy of the inves-
energy dissipation [28]. Thus, the end point of CMOD for each spec-
tigated concrete. For this, Elices et al. [29] suggested that true frac-
imen was taken such that the increment in the CMOD from the
ture energy should be estimated by using a far tail constant value.
peak to the end point was identical for each companion specimens
In this study, the tests were stopped when the descending region of
and the fracture energy was calculated at this point. The load val-
the load-CMOD curve showed a full tail, and the unmeasured part
ues corresponding to 200 equally spaced CMOD values were calcu-
of the tail part was inversely extended using the optimally fitted
lated by interpolating the processed test data set using MATLAB.
expression when the fracture energy was calculated. Moreover,
For each specimen, the 100th data point represents the same status
the self-weight of the specimen was neglected in the calculation
as that represented by the peak load status, and from 100th to
of fracture energy because it was compensated by two bottom sup-
200th all data points can be regarded as the same status because
ports, and the influence of the self-weight was insignificant for a
each point (or fracture process zone) is equally far from the peak.
not very large wedge splitting specimen.
Meanwhile, we can assume that the each equally spaced data point
in the ascending region also represents the same fracture status. W
Consequently, all of these equally spaced points denote the same GF ¼ ð2Þ
ðh  a0 ÞB
fracture status and the values of CMOD and the corresponding load
can be averaged. The averaged load-CMOD curves are discussed in where GF is fracture energy; W is the total work corresponding to
the following section. the area under the horizontal load-CMOD curve; h, a0 , and B are
the effective height, initial notch length, and thickness of the spec-
imen, respectively.
3. Results As mentioned above, for each series the mean curve was deter-
mined from the individual curves. The difference between the val-
3.1. Load-CMOD curves ues of GF determined from the mean curve and the average value of
GF measured from the individual test results should be lower than
Fig. 3 shows the typical load-CMOD curves of concrete exposed 1%. For each curing humidity, the average values of GF measured
to four different relative humidity levels at the five investigation from the load-CMOD curve are plotted in Fig. 4 as a function of
ages. These figures illustrate that the concrete was nearly in linear the age. Although each point in Fig. 4 represents the average of
elastic deformation at the early loading stages. Nonlinear deforma- three companion specimens tested, the error bars are not pre-
408 Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413

6 5
T20RH98A3 T20RH70A3
5 T20RH98A7 4 T20RH70A7
T20RH98A14 T20RH70A14

Load (kN)
Load (kN)
4
T20RH98A28 3 T20RH70A28

3 T20RH98A60 T20RH98A60
2
2

1
1

0 0
0 0.5 1 1.5 2 0 0.5 1 1.5 2
CMOD (mm) CMOD (mm)

5 5
T20RH50A3 T20RH30A3

4 T20RH50A7 4 T20RH30A7
T20RH50A14 T20RH30A14
Load (kN)

Load (kN)
3 T20RH50A28 3 T20RH30A28
T20RH50A60 T20RH30A60
2 2

1 1

0 0
0 0.5 1 1.5 2 0 0.5 1 1.5 2
CMOD (mm) CMOD (mm)

Fig. 3. Load-CMOD curves for wedge splitting specimens.

250 sufficient internal moisture. A similar phenomenon could be


observed for 30% RH, but GF tended to be a stable in a shorter time.
At a lower curing humidity, the shorter stable time can be attribu-
Fracture energy (N/m)

200
ted to the decrease in the internal humidity due to evaporation,
resulting in insufficient free water for the hydration reaction.
150 Fig. 4 also shows that at any age, a lower curing humidity always
led to a smaller value of GF , although the trend is similar. After 3
T20RH98
days of hydration, the GF of specimens kept in 30% RH was smaller
100
T20RH70 by 7.6%, 5.2% and 2.7% when compared to that of the concrete
T20RH50 cured at 98% RH, 70% RH and 50% RH, respectively. Furthermore,
50 the gap gradually increased as the concrete became older. Conse-
T20RH30
quently, at 60 days of curing age, the GF of specimens kept in
0 30% RH was 200.6 N/m, which was 17.4%, 12.3% and 7.1% smaller
0 10 20 30 40 50 60 than that of the concrete exposed to 98% RH, 70% RH and 50%
Age (day) RH, respectively. This indicates that the influence of curing humid-
ity on GF increased gradually with time, and the available free
Fig. 4. Variation of fracture energy with age for concrete cured at different relative
moisture became a critical factor for maintaining the later age
humidity.
hydration reaction.

sented for clarity. In any case, the deviation between one replicate 3.3. Effective fracture toughness
and the average of three companion was less than 10% with respect
to the average. For the nonstandard wedge splitting specimens, the following
As can be observed from Fig. 4, the fracture energy of concrete formula proposed by Xu et al. [30] can be used to calculate the
cured at low relative humidity was similar to that in standard cur- effective fracture toughness
ing condition. At the beginning, the value of GF tended to rapidly
increase in the first 7 days. On prolonging the curing ages, GF kept F smax 3:675½1  0:12ða  0:45Þ ac
K IC ¼ pffiffiffi  a¼ ð3Þ
increasing at a smaller rate, and eventually tended to reach a pla- B h ð1  aÞ3=2 h
teau value. Typically, for the 98% RH, GF was 150.4 N/m at 3 days,
181.3 N/m at 7 days, 199.8 N/m at 14 days, 220.1 N/m at 28 days, where K IC is the effective fracture toughness; F smax is the peak hor-
and 233.3 N/m at 60 days. The fracture energy continuously izontally load; ac is the critical effective crack length corresponding
increased with age and the slope was still relatively large, which to the peak load; B and h are the thickness and of effective height
means that a curing time of 60 days would not be enough to reach the specimen, respectively. Eq. (3) is valid within 1% accuracy for
a stable state for this humidity and the specimens sustained 0:2 6 a 6 0:8.
Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413 409

Once the initial crack propagation occurs under increased exter-

Effective fracture toughness (MPam1/2)


1.8
nal load, the nonlinear cohesive fracture process zone appears. In
this case, the practical physical crack is often simplified as an effec-
1.5
tive crack using the equivalent-elastic concept so that the linear
elastic fracture mechanics can be used to calculate K IC . In general,
1.2
the critical effective crack length can be evaluated in different
ways. For example, Karihaloo et al. [31] believed that ac can be
0.9
determined by measuring the peak load and the corresponding T20RH98
load point deflection. The two parameter fracture model proposed T20RH70
0.6
by Jenq and Shah [32] requires an unloading and reloading proce-
T20RH50
dure to estimate the value of critical effective crack length. Based
0.3 T20RH30
on the linear asymptotic superposition assumption, Xu et al. [30]
proposed another method to evaluate ac for nonstandard wedge
0
splitting specimen based on load-CMOD curves. This formula was
0 10 20 30 40 50 60
used in the present study and can be expressed as follows: Age (day)
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi!
13:18 Fig. 5. Variation of effective fracture toughness with age for concrete cured at
ac ¼ ðh þ h0 Þ 1   h0 ð4Þ different relative humidity.
9:16 þ CMODc  E  B=F smax

where E is the elastic modulus obtained from the initial compliance


hydration became low and was negligible below 30% relative
of load-CMOD curve; CMODc is crack opening displacement corre-
humidity [2]. Hence, the hydration reaction was expected to stop
sponding to F smax ; h0 is thickness of clip gauge holder; h and B are
earlier under low humidity condition, and the period that K IC
the effective height and thickness of the specimen respectively.
achieved the steady became slightly shorter with decreasing curing
The empirical expression is valid for0:3 6 a 6 0:7 within 2.9 per-
humidity. Typically, for 98% RH, K IC was 1.061 MPam0.5 at 3 days,
cent accuracy. Thus, the critical effective crack length of each spec-
1.232 MPam0.5 at 7 days, 1.361 MPam0.5 at 14 days, 1.455 MPam0.5
imen can be easily determined by substituting the measured E,
at 28 days, and 1.555 MPam0.5 at 60 days. The value of K IC at 60
CMODc and F smax into Eq. (4). The values of ac at different curing
days was 6.9% larger than that at 28 days. Furthermore, for 30%
humidity levels and ages are listed in Table 3. It is noted that ac
RH, K IC was 0.931 MPam0.5 at 3 days, 1.081 MPam0.5 at 7 days,
was dependent on the curing humidity and age, and its value varied
1.175 MPam0.5 at 14 days, 1.295 MPam0.5 at 28 days, and 1.357
between 165.2 mm and 179.6 mm. Further, ac decreased with rela-
MPam0.5 at 60 days. The value of K IC at 60 days was only 4.8% lar-
tive humidity decreasing and hydration time elapsing. This trend is
ger than that at 28 days. This also indicated that the internal
consistent with previous observations made by Kim [33].
humidity of the specimen did not fall to the critical value before
Fig. 5 illustrates the effective fracture toughness against age for
60 days but was sustained a condition that there was sufficient
different curing humidity, in which each point represents the aver-
internal moisture available for the hydration reaction. It can also
age values of K IC determined by the three replicate specimens. In
be observed from Fig. 5 that K IC of the concrete cured at low rela-
order to avoid presenting a messy plot, the error bars were omitted
tive humidity was smaller than that kept under standard curing
again. Compared with the fracture energy, a smaller scattering of
conditions at the same age; this was especially true at the later
data was observed in K IC , which may be explained by the difference
ages. For instance, at 7 days, for concrete cured at 30% RH, the
in the crack path. Owing to unstable propagation of the crack, its
value of K IC was reduced by about 13.9%, 11.1%, and 4.5% when
path became more arbitrary and redundant cracks also emerged,
compared to the corresponding value of the concrete kept in 98%
but the energy consumed by these random micro-cracks could be
RH, 70% RH and 50% RH, respectively. With the passage of the time,
not easily determined and were therefore neglected when calculat-
the difference in K IC slightly increased. Typically, after 14 days of
ing the fracture energy, resulting in a greater randomness of the
hydration, the K IC of concrete exposed to 30% RH was 1.175
fracture energy. However, K IC was determined before the forma-
MPam0.5, which was approximately 15.9%, 12.7%, and 4.7% smaller
tion of redundant and random micro-cracks.
than that of concrete kept in 98% RH, 70%RH and 50% RH, respec-
As shown in Fig. 5, K IC was a monotonically increasing function
tively. These results demonstrated that the curing humidity exert
of the age, irrespective of the curing humidity investigated, which
a growing effect on K IC with time. Also, we can again confidently
was similar to that noted in the development of GF with age. Dur-
conclude that the available free moisture was a key factor in deter-
ing the first 7 days, K IC increased rapidly with age because the
mining the hydration of concrete, especially at later ages.
cement hydration reaction was very rapidly in this stage. The
growth rate first became gradually larger, and then decreased after
reaching the maximum value, and the corresponding curves 3.4. Characteristic length
became steep. Afterwards, K IC slightly increased with age at a
slower rate and tended to be stable if the curing time was long Fracture energy or effective fracture toughness alone cannot be
enough. Once the internal relative humidity dropped below 80%, used to represent the brittleness of materials, which is commonly

Table 3
Critical effective crack length at different relative humidity levels and ages.

Age (days) Critical effective crack length ac (mm)


98% RH 70% RH 50% RH 30% RH
3 176.9 173.7 173.2 172.3
7 175.9 172.5 172.3 171.1
14 173.8 179.6 171.2 170.5
28 172.2 171.0 170.2 168.7
60 169.8 168.2 167.9 165.2
410 Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413

understood as the tendency of a material to fracture abruptly decreasing curing humidity. At 3 days, the Lch of concrete cured
before any significant irreversible deformation occurs. Therefore, at 98% RH was higher by 1.9%, 3.6%, and 5.7% relative to those
in order to describe the brittleness of concrete, Hillerborg et al. cured at 70%RH, 50% RH, and 30% RH, respectively. After 28 days
[34] introduced characteristic length (Lch ), defined as of hydration, the corresponding gap increased to 5.2% for 70% RH,
8.9% for 50% RH and 12.7% for 30% RH. However, at 60 days of
EGF the curing age, the Lch of the concrete cured at 98% RH was
Lch ¼ 2
ð5Þ
ft 363.8 mm, which was only larger by 3.8%, 5.9%, and 9.7% than that
of the concrete cured at 70%RH, 50% RH, and 30% RH, respectively.
where GF is the fracture energy; E is the elastic modulus; f t is the This indicates that the decreasing rate of the characteristic length
splitting tensile strength obtained using inverse analysis by match- due to the decreasing curing humidity increased with age until
ing the experimental specimen response data to the theoretical 28 days, and then decreased with age.
data. More specifically, the load-CMOD response was modeled
and fit over the experimental data source. A detailed derivation of
this method can be found in the literature [35]. If the elastic mod- 4. Discussion
ulus was not measured from the cubes, its value can also be calcu-
lated from the initial compliance of the load-CMOD curve for a As illustrated in Figs. 4–6, for different curing humidity,
wedge splitting specimen [32]. Kumar et al. [36] concluded that although the overall trend of the development of concrete fracture
almost the same value of can be obtained from the load-CMOD properties with age was similar, some deviations were observed.
curve and compressive cylinder test. Therefore, in this study, the Typically, at early stages, the cement hydration reaction was very
value of elastic modulus determined by the initial compliance rapid. Consequently, GF and K IC increased rapidly with age, regard-
was used to calculate the characteristic length. Because the charac- less of the curing humidity. The growth rate first became gradually
teristic length includes a combination of energy, stiffness, and increased, and then almost decreased after reaching the maximum
strength parameters, it is regarded as a synthetic brittleness value, and the corresponding curves became steep. However, the
parameter. period for this stage became slightly longer with the decreasing
According to the fictitious crack model [34], it is clear that Lch relative humidity. In the next stage, the hydration rate became
was proportional to the fracture process zone. The longer fracture smaller; therefore, GF and K IC slightly increased with age at a
process zone required higher energy, and this energy in micro- decreased rate. Normally, there should be a third stage, where GF
crack propagation was visible in the longer tail stress-strain curve. and K IC would gradually reached their respective ultimate values
Therefore, the smaller value of Lch corresponded with higher brit- with time. At high humidity, however, the third stage was not
tleness and lower strength against the cracking of concrete and observed or was not very obvious because the age of only up to
vice versa. 60 days was investigated in this study, which also implied that
Variation of Lch with age for concrete cured at different relative the internal humidity of the specimen did not reduce to the critical
humidity levels is depicted in Fig. 6. It is apparent that Lch was value. The increase in GF and K IC with age was attributed to the fact
strongly dependent on the age and curing humidity, and its value that ITZ between the aggregate and the paste, in which the greatest
varied between 513.1 mm and 328.5 mm. For the same curing con- number of micro-cracks formed, and it was the most sensitive zone
ditions, Lch decreased rapidly with the age until 28 days, and then within the concrete. Therefore, the cement paste became stronger
kept decreasing at a reduced rate. For instance, in the case of 98% because of the accumulation of new hydration products in ITZ
relative humidity, Lch continuously decreased from 513.1 mm at pores as the concrete became older. In fact, Elsharief et al. [37]
3 days to 494.3 mm at 7 days, 462.8 mm at 14 days, 409.4 mm at has demonstrated that the presence of a relatively large amount
28 days, and finally 363.8 mm at 60 days, with a significant loss of un-hydrated cement grains in the ITZ at early ages made the
of 149.2 mm or 29.1%. The decrease of Lch with age shows that con- ITZ porous. With time elapsing, the pores in the ITZ were filled
crete is more ductile at early ages. This is because, at early ages, a with hydration products, and the number and size of these pores
large amount of cement and water have not undergone the hydra- and that of cement paste reduced. The strength of the cement paste
tion reaction yet, and are gathered in the interfacial transition and ITZ also improved. Thus, the bridging effect and pulling of the
zone. As a result, the interfacial transition zone was porous and aggregate out of the matrix decreased, and the fracture path under
the cracking path became longer and more tortuous. Fig. 6 also load also transformed from bond zones or around aggregates to
shows that for the same age, Lch reduced dramatically owing to directly through the aggregates, as shown in Fig. 7. Furthermore,
the strength of the aggregate was much larger than that of the
cement paste and ITZ. Consequently, higher energy was required
550 T20RH98 to overcome the aggregates and the strengthened ITZ and cement
T20RH70 paste. Thus the larger values of GF and K IC were measured. With
Characteristic length (mm)

500 further strengthening of cement paste and ITZ, however, the frac-
T20RH50
ture mode did not change significantly, where only more aggre-
450 T20RH30 gates were pulled out from the matrix. Thus, the values of GF and
K IC kept increasing at a decreasing rate at later ages, and eventually
400 tended reach to a stable value.
More importantly, as mentioned above, the fracture properties
350 of the concrete were less dependent on the curing humidity during
early stages, where GF , K IC , and Lch for the concrete did not reduce
300 significantly as the relative humidity changed after 3 days of
hydration. However, at later ages, when part of the water was used
250 in the hydration reaction or was lost due to evaporation, the avail-
0 10 20 30 40 50 60
able water content became a critical factor for the continued
Age (day)
hydration. Starting at 7 days and continuing till 60 days, the values
Fig. 6. Variation of characteristic length with age for concrete cured at different of GF , K IC , and Lch became smaller with decreasing curing humidity,
relative humidity. in which GF , K IC , and Lch reduced approximately by 17.4%, 15.9%
Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413 411

(a) At 3 days of curing age (b) At 60 days of curing age

Fig. 7. Typical fracture surfaces of concrete at different ages.

and 14.6% respectively from 98% RH to 30% RH. Such trend agreed coefficient of the concrete increased with decreasing relative
with other limited number of independent investigation reported humidity [42], which further enlarged the mismatched deforma-
by other researchers in a somewhat different way. For instance, tion between the cement paste and aggregates and increased the
Hordijk et al. [38] observed that the concrete specimens became likelihood of micro-cracking. Consequently, the failure mode has
more brittle with lower humidity and the characteristic length also changed at low humidity levels owing to the weakening of
decreased with decreasing humidity. Bella et al. [39] reported that the bond zone and formation of micro-cracking, where the crack
after 7 days of hydration, the elastic modulus steadily decreased propagated around the aggregates and lesser aggregates were frac-
with relative humidity until 33% RH and then kept constant. Inves- tured, as shown in Fig. 8. As it was mentioned before, the strength
tigating three strength levels under humidity of 100% RH to 40% of the aggregate was much larger than that of the cement paste and
RH, Kwon et al. [40] demonstrated that the compressive strength ITZ, resulting in smaller values of GF , K IC and Lch at low humidity
for low, medium, and high strength levels decreased from 40.2 to levels. Further mechanism for the reduction in fracture parameters
25.2 MPa, 44.9 to 29.8 MPa, and 54.0 to 35.8 MPa respectively. was the reduced water activity [43]. Namely, in a concrete hydrat-
Patel et al. [2] found that curing humidity below 80% RH produced ing system, un-hydrated phases continuously dissolved and dif-
a coarsened pore structure with a large-diameter porosity three fused out into the pore solution forming new solid hydrated
times greater than that obtained with saturated curing, which phases. In the case of low humidity, however, the effective water
could adversely affect the fracture property and durability of was lower, and less water in the pores of material was available
in situ concrete. for dissolving un-hydrated phases and for reaction with the
The degradation of the concrete fracture properties at low cement. What’s worse, evaporation of water from an ionic solution
humidity raises a question: What phenomena occurred at the would be accompanied by the increase in the ionic concentrations,
microscopic level under these curing conditions? We believed that and if the saturation was reached, ionic precipitation would take
several different mechanisms were responsible for such reduction place, which further decreased the water activity and the amount
in fracture properties at low humidity. Firstly, this reduction was of the hydrating cement paste. It should be noted that higher con-
partly caused by the physical properties of the concrete. With centrations would probably give rise to higher reaction rates before
decreasing environmental humidity, the evaporation of the mois- a steady concentration levels were reached again, but in a smaller
ture inside the concrete accelerated, resulting in reduced water volume of water and with a lower reaction rate. Meanwhile, in the
available for the hydration reaction and a partial desaturation of case of insufficient water, the solubility of C3S would shift owing to
finer pores. As a result, hydration products could not continue in the negative capillary pressure in the pore liquid, which was a
the absence of water. Secondly, in the case of low humidity, the main factor in determining the equilibrium between C3S, C-S-H,
desiccation of concrete caused the shrinkage of the cement paste, and CH, and it can inhibit the hydration reaction of C3S [9]. Finally,
whereas the effect of this desiccation on the aggregates was less with decreasing curing humidity, the interlayer water reduced and
pronounced than on the cement paste [41]. The stress concentra- thus the basal-spacing of C-S-H decreased, yielding a more disor-
tions due to restraint deformation led to the formation of micro- dered local structures [11]. As a result, the concrete became a more
cracks in the ITZ, originally at larger aggregates even before load- porous structure, and the smallest values of GF and K IC were mea-
ing. Furthermore, at a given temperature, the thermal expansion sured for the concrete kept at 30% RH. In brief, all of these factors

(a) Cured at 30% RH (b) Cured at 98% RH

Fig. 8. Typical fracture surfaces of concrete specimens cured at different relative humidity.
412 Z. Mi et al. / Construction and Building Materials 169 (2018) 403–413

were related to phenomenon that fracture properties deteriorated From the perspective of engineering, the reduction of GF , K IC ,
with decreasing relative humidity. and Lch due to drying not only increased the likelihood of cracking,
A question related to our results is still unanswered: Why the but also exacerbated the durability of concrete structures. Thus,
fracture parameters did not change significantly with relative the influence of ambient humidity on the fracture parameters of
humidity at the early ages? According to the physical model pro- concrete should not be ignored while designing concrete structures
posed by Wittman [44], the capillary pressure inside the pores to avoid undesirable results. We believe that our work will provide
increased with decreasing moisture content, imposing a volumet- a better understanding of the fracture properties of concrete sub-
ric pressure that compressed the material and resulted in the jected to practical curing regimes and will also help designers in
strengthening of fracture properties. Moreover, this compaction checking the safety factor and the adequacy of the structure to
effect of increasing capillary forces was more pronounced at the safely withstand all applied loads.
early ages, when the solid skeleton of the hydration products
filled up the overall volume available less efficiently. Hence, the Acknowledgements
deterioration of the fracture properties owing to micro-cracking,
reduced water activity, and other such factors was partly com- This research work was supported by the National Natural Science
pensated by the compaction effect of capillary forces, eventually Foundation of China (51339003, 51579134), and the Research
resulting in quasi-constant GF , K IC , and Lch . With time, however, Fund of Tsinghua University (Grant No. 20161080079).
a more developed solid skeleton could better withstand the over-
all compaction. As a result, the compaction effect gradually weak-
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