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Original Article

Effect of early age loading on the subsequent


mechanical and permeability properties of concrete
and its mechanism analysis

Weipei Xue a,b,c,*, Hanwen Zhang a,b, Haopeng Li a,b, Wei Xu a,b
a
State Key Laboratory of Mining Response and Disaster Prevention and Control in Deep Coal Mines, Anhui
University of Science and Technology, Huainan 232001, China
b
School of Civil Engineering and Architecture, Anhui University of Science and Technology, Huainan 232001, China
c
Post-doctoral Research Station of Safety Science and Engineering, Anhui University of Science and Technology,
Huainan 232001, China

article info abstract

Article history: Modern construction methods often result in concrete structures bearing loads at an early
Received 26 April 2021 age, which is different from the stress condition under the standard curing in the labo-
Accepted 10 July 2021 ratory. This study experimentally examined effects of different ages and external loads on
Available online 16 July 2021 subsequent mechanical and permeability properties of concrete, and investigated the
mechanism of effect from the perspective of internal structure changes. The results show
Keywords: when the early age loading reaches 40% of the current concrete strength, the original in-
Early age loading ternal structure of specimens will be severely damaged, reflecting significant increase in
Concrete the proportion of mesopores and macropores and obvious connectivity cracks, thus
Mechanical property making the mechanical and permeability properties deteriorate, and the earlier the applied
Permeability property load, the greater of this deterioration. However, when loading at 10%, the original internal
Internal structure structure cannot be changed greatly due to the low load level, and some parts of the
original pores are even compacted rather than expanded which has little effect on sub-
sequent mechanical and permeability properties of concrete.
© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

research. Notably, such specimens are not subjected to any


1. Introduction form of external loading during the 28 days curing period
[5e8]. However, modern construction methods are committed
Concrete is widely used in construction projects, and its me- to shortening the construction period to the extent possible;
chanical property and permeability directly influence the as a result, construction organizations often apply significant
safety and long-term use of engineering structures [1e4]. Re- loading to concrete structures at an early age [9,10]. Chen et al.
searchers generally use concrete specimens that have been [11] carried out triaxial mechanical property tests on concrete
cured under standard conditions to carry out experimental

* Corresponding author.
E-mail address: xueweipei@aust.edu.cn (W. Xue).
https://doi.org/10.1016/j.jmrt.2021.07.051
2238-7854/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 4 : 1 2 0 8 e1 2 2 1 1209

after curing for 3, 7, 14, and 28 days to propose a mathematical influence of external load when studying the permeability of
model for the prediction of the triaxial mechanical behavior of concrete [23e25]. Yao et al. [26] investigated the mechanical
early age concrete. Schutter [12] conducted a series of studies property of shaft lining concrete under high pore water pres-
on the mechanical property, cracking behavior, and critical sure, and took samples from the failure section of the prism
chloride penetration depth of early age concrete that provided specimen to observe the development of microcracks in con-
a reference for the design of durable concrete structures. crete using a scanning electron microscope (SEM), and deter-
These studies focused on the mechanical property and mined the reasons for changes in the macroscopic properties
permeability of early age concrete, providing significant from a microscopic point of view. Although SEM can clearly
guidance. However, as mentioned above, during the con- observe the internal structure morphology of the sample, it
struction process, loads are often applied to early age concrete only analyzes the internal structure morphology of the local
structures. At an early age, the strength of the concrete is low observation area of the specimen. Kumar [27] used the mer-
and the development of the internal structure is not yet stable, cury intrusion method to observe the pore distribution of
thus even a small load may change the subsequent perfor- concrete; however, the high pressure applied during the test
mance of the concrete. The influence of early age loading on can easily destroy the original pore structure inside the
concrete performance in later periods must therefore be specimen and thus adversely affect the test results.
investigated. In this vein, Jiang et al. [13] applied 30% of the It is believed that the development of the internal structure
compressive strength of a lightweight aggregate concrete at has an important effect on the macroscopic properties of
ages of 1, 3, 7, and 14 days to study the influence of early age concrete [28,29]. Indeed, there are two important types of
compression on creep behavior. Ye et al. [14] loaded fly ash performance indices that describe concrete structures: me-
concrete at ages of 3, 5, and 7 days, observing that the chanical property and permeability. The former determines
resulting deformation increased with increasing loading age, the load bearing capacity of the concrete structure whereas
and that the compressive strength of 14 day aged concrete the latter affects their durability. Because early age construc-
decreased. Du et al. [15] studied the deformation of early tion loading is becoming increasingly common, and as a re-
concrete with time under progressive loading processes and view of relevant literature found that previous studies have
proposed a corresponding prediction model. Kim et al. [16] not investigated the influence of early age loading on the
proposed a creep development prediction model to explain subsequent mechanical property or permeability of concrete
the effect of time on the elastic modulus of concrete loaded at from the perspective of internal structure change [30e32], this
an early age. It can be seen that researchers have begun to pay study investigated the influence of the early age loading on the
attention to the influence of early age loading on the subse- subsequent mechanical property and permeability of con-
quent performance of concrete, mainly focusing on the crete. To do so, this study employed uniaxial compression
deformation. Besides, Zhuang et al. [17] studied the effect of tests to determine the mechanical property of early age loaded
early age loading on the axial compressive strength of con- concrete, and water permeability tests under variable
crete, only evaluated the strength of the specimens for each confining pressure to determine the permeability property of
loading age and magnitude, and did not investigate the cor- early age loaded concrete and nuclear magnetic resonance
responding change in the internal structure of the concrete. (NMR) technology to detect the distribution of microcracks
Indeed, the influence of early age loading on the subsequent and micropores within. Notably, NMR is a non-destructive
permeability of concrete has not been previously investigated testing method that can quickly establish the number of
[18e20]. pores and pore size distribution in a sample without
The load on a concrete structure in the service stage destroying the original pore structure. In addition, NMR fo-
constantly changes [21,22]. However, the change in the cuses on the analysis of the whole specimen, and the test area
permeability of concrete under loading and unloading re- covers a wide range of areas, which can be well complemen-
mains unknown, and urgently needs to be studied because it tary to SEM. In this study, NMR and SEM are combined to
can help to more accurately reflect the actual engineering analyze the internal structure of concrete under early age
situation. Unfortunately, scholars have not yet considered the loading, so as to obtain more comprehensive data and more

Fig. 1 e Concrete under loading and curing conditions at an early age (a) physical appearance and (b) schematic of loading
device.
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2.2. Specimen preparation


Table 1 e Concrete mix ratio.
Cement Fine aggregate Coarse aggregate Water The concrete used in this study contained P.O32.5 Portland
(kg/m3) (kg/m3) (kg/m3) (kg/m3)
cement with river sand (fineness modulus of 2.93) as the fine
380 662.11 1151.89 176 aggregate and limestone macadam (particle size range of
5e15 mm and crushing index of 8.7%) as the coarse aggregate.
The concrete mix proportions are shown in Table 1. Firstly,
convincing. The results of this research provide a reference for 150  150  150 mm cube specimens were cast for the
the design of concrete structures intended to bear construc- compressive strength tests at the different ages, shown in
tion loads at an early age. Table 2. Secondly, using the scheme described in Section 2.1,
the loads were applied to the cube specimens after 1 day, 3
days, and 7 days of curing until 14 days of curing had elapsed.
2. Materials and methods After 28 days of curing, cores were taken from the concrete
cube specimens using coring, cutting, and grinding machines
2.1. Early age loading application scheme in accordance with the GB/T50266-2013 standard [35] to
fabricate 50  100 mm standard cylinder specimens, and four
The early age concrete loading scheme applied in this cylinder specimens for each loading age and magnitude were
study was established using the stress monitoring results subjected to mechanical property tests of uniaxial compres-
of shaft lining concrete during underground engineering sion and water permeability tests under variable confining
construction [33,34]. The effects of loading at ages of 1 pressure to understand the influence of early age loading on
and 3 days with external loads of 10%, and 40% of the the mechanical and permeability properties of the concrete. It
corresponding compressive strength of the concrete at should be emphasized that when cutting, the uppermost and
those ages were accordingly evaluated. After 7 days of the lowermost ends of the specimens were first trimmed by
curing, the load levels of all specimens were adjusted to 20 mm to eliminate the inevitable variability of the pore
10%, and 40% of the compressive strength of the concrete structure in the vicinity of the concrete end faces. The internal
at that age. The load applied to the concrete specimens at pore structures of the concrete cylinder specimens were then
an early age must be constant over a long duration of observed though NMR tests. It should be noted that during
time. Although a servo pressure testing machine is able to normal use, a concrete structure is in a multiaxial stress state
apply a constant load, the test could be suspended due to [36]. Previous studies on the permeability of concrete have
a power outage during the experiment. Therefore, a set of ignored this by primarily applying impermeability tests or
early age loading devices was designed (as shown in chloride ion permeability tests without an external load
Fig. 1) to apply early age loading to the concrete speci- [37e39]. Therefore, this study investigated the permeability of
mens during the curing process. Once the concrete was concrete after early age loading under the action of external
loaded and cured to an age of 15 days, then the applied stress to obtain results that are relevant to the actual working
load was removed to allow the specimens to cure natu- conditions.
rally indoors to the age of 28 days. During this time, the
average temperature ranged from 19  C to 28  C, and the 2.3. Experiment procedure
relative air humidity was 85.1%.
Two steel plates with a yield stress of 235 MPa and di- A TAW-2000 electro-hydraulic servo pressure testing machine
mensions of 280 mm  280 mm  20 mm were used as the top was used to conduct the mechanical and water permeability
and bottom of the early age loading device. The four 22-mm tests. This machine has three independent control systems:
diameter threaded rods and eight nuts used to clamp the an axial pressure control system, a confining pressure control
plates together were made of grade 10.9 steel. A 100e500 N m system, and a pore water pressure control system. The testing
torque wrench was used to tighten the nuts to the torque machine uses an EDC full-digital servo controller from DOLI
required to achieve the desired load. As the early shrinkage of Elektronik GmbH (Germany) and a servo valve from MOOG Inc.
concrete leads to a reduction in the applied load, the torque of (USA). During experiments, data such as the axial stress,
each nut was checked every 36 h to ensure consistency with displacement, confining pressure, pore water pressure, and
the desired load. pore water flow can be recorded and displayed in real time by
As the sum of the vertical forces in the loading device is the TAW-2000. The mechanical properties (uniaxial
zero, the axial force in the threaded rod F ¼ P/4, where P is the compression) test used only the axial pressure control system,
total load applied to the concrete specimen. The required axial as shown in Fig. 2(a). In this test, the load was applied through
force in the threaded rods was thus converted into the deformation control at 0.05 mm/min, and the data describing
required torque using

Mt ¼ 0:2Fd (1)
Table 2 e Compressive strength of concrete of different
where Mt is the torque in N m, F is the axial force in the
ages.
threaded rod in N, and d is the rod diameter in mm.
Then, the relationship between P and Mt can be obtained as Time 1 day 3 days 7 days 28 days
curing curing curing curing
P ¼ 20 Mt =d (2) Compressive strength (MPa) 8.3 16.3 23.6 35.4
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Fig. 2 e Apparatus used for the (a) mechanical experiment (b) permeability experiment.

the resulting axial stress, axial strain, and circumferential 1  2n


strain were recorded automatically. The permeability test εve ¼ s1 (4)
E
required the simultaneous use of all three independent con-
where E is the modulus of elasticity, v is the Poisson's ratio,
trol systems. The pore water pressure was held constant at
and s1 is the axial stress.
1.3 MPa, and the applied confining pressure was increased in
Martin and Chandler [40] suggested that the total volu-
stages from 2.0 MPa, to 3.5 MPa, 5.0 MPa, and 6.5 MPa, then
metric strain of a specimen under uniaxial compression
decreased in the same stages back to 2.0 MPa. At each stage,
consists of its elastic volumetric strain and crack volumetric
the pore water flow was monitored until it was in a steady
strain. Therefore, the crack volumetric strain εvc was obtained
state of seepage. The system was then left for at least 1 h
by subtracting the elastic volumetric strain from the total
before the confining pressure was changed to the next stage,
volumetric strain as follows.
as shown in Fig. 2(b).
εvc ¼ εv  εve (5)

The crack closure stress (scc ), crack initiation stress (sci ),


3. Results and discussion
damage stress (scd ), and peak stress (sf ) are key stress
thresholds in the process of concrete deformation and failure,
The specimen nomenclature used to discuss the results was
an understanding of which is critical when analyzing the
defined to include both the specimen loading age as well as
macroscopic mechanical properties of concrete specimens
the loading level. The specimens loaded after 1 day of curing
and studying the evolution of microscopic cracks within. The
with 10% and 40% of the corresponding concrete compressive
crack closure stress (scc ) and crack initiation stress (sci ) were
strengths at that time are represented by C-1d-10 and C-1d-40,
determined from the horizontal segments in the crack volu-
respectively. Similarly, the specimens loaded after 3 days of
metric strain curve [41]. The reversal point in the total volu-
curing with 10% and 40% of the corresponding compressive
metric strain curve, i.e., the point at which the state of the
strength at that time are represented by C-3d-10 and C-3d-40,
specimen changed from compression to expansion, was used
respectively. Finally, C-N-0 represents a specimen with zero
to determine the damage stress (scd ).
load application at an early age, which was used as a reference
The critical stress thresholds of each group of specimens
for comparison.
were determined as shown in Fig. 3. According to these critical
stress thresholds, the rising uniaxial compression curve can
3.1. Effect of early age loading on mechanical properties
be divided into four phases. Phase I is the crack closure phase
of concrete
in which the initial cracks and pores in the concrete close due
to the applied compression. The behavior in this phase is
The mechanical properties of the specimens were used to
closely related to the initial micro crack density and geometric
determine the effects of early age loading on the performance
characteristics. In this phase, the axial stressestrain curve is
of the concrete. The strains and stresses in the concrete at
approximately concave with obvious nonlinear characteris-
various phases of loading were accordingly obtained from the
tics, the volume of the specimen is reduced, and the material
test results as follows.
is in a state of compression. This phenomenon is relatively
The volumetric strain εv was obtained by:
rare [42,43], which is shown in that stage I accounts for a large
εv ¼ εaxial þ 2εlateral (3) proportion of the whole deformation process. Phase II is the
elastic deformation phase, in which the crack volumetric
where εaxial is the axial strain and εlateral is the circumferential
strain remains unchanged, and no damage occurs inside the
strain.
specimen. The axial stress and axial strain exhibit a linear
The elastic volumetric strain εve under uniaxial compres-
relationship that can be used to determine the elastic
sion was calculated by
modulus and Poisson's ratio. Phase III is the stable crack
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Fig. 3 e Uniaxial compression stressestrain curve (a) C-1d-10 (b) C-1d-40 (c) C-3d-10 (d) C-3d-40 (e) C-N-0.

propagation phase, which begins at the crack initiation stress specimens subjected to early age loading clearly decreased
and characterizes the initiation of new microcracks in the significantly compared to the reference specimen. The ratio
specimen. In this phase, the total volumetric strain curve no (scd =sf ) also showed a downward trend, decreasing by 28e52%,
longer exhibits a linear change, showing instead a relatively indicating that early age loading had a significant impact on the
small and nonlinear increase. At this time, the specimen is damage stress. This impact is the result of the low strength of
still in compression, and only by increasing the load can early age concrete, which enables the load to affect the devel-
cracks continue to grow. The duration of this stage is greatly opment of the internal structure. The damage stress of the
affected by the early age loading, it is obvious that the curing specimen under uniaxial compression is therefore reached
process is not affected by the early age loading, and the
duration of this stage is the longest. Phase IV is the unstable
crack propagation phase, which begins at the crack damage Table 3 e Threshold stresses defining the phases of each
stress and indicates that new microcracks have begun to specimen group.
develop inside the specimen. As the load continues to in-
Specimen group C-N-0 C-1d-10 C-1d-40 C-3d-10 C-3d-40
crease, the volumetric strain curve turns downward, and the
scc (MPa) 6.61 4.01 4.58 6.79 6.04
specimen changes from being in compression to being in
sci (MPa) 11.88 16.31 12.06 12.50 11.80
tension. In this phase, the specimen reaches the peak stress scd (MPa) 32.14 19.72 15.08 15.31 15.99
and is destroyed [44,45]. sf (MPa) 34.49 34.01 22.62 34.39 24.85
The threshold points that define the phases in each spec- sci/sf 0.34 0.48 0.53 0.36 0.47
imen are shown in Table 3. The damage stress (scd ) of scd/sf 0.93 0.58 0.67 0.45 0.64
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Fig. 4 e Specimen crack patterns after failure.

earlier. The crack initiation stress (sci ) showed a slight increase, mainly the result of tensile failure, and the crack paths are
and the ratio (sci =sf ) increased by 6e56%. It can thus be roughly parallel to the loading direction. The macroscopic
concluded that the crack initiation stress of specimens under failure characteristics of these specimens are thus the result
uniaxial compression is delayed after early age loading, and of the joint action of the tensile failure surfaces and the shear
new cracks begin to occur only after the original cracks are slip surfaces. Besides, the earlier the age of load, the more
compacted and closed and the specimen passes through the cracks appear after the failure of the specimens and the macro
elastic phase. It can be seen in Fig. 3 that for specimens sub- cracks run through the middle of coarse aggregate. The dif-
jected to early age loading, the duration of Phase I is longer than ference is that under the load of 3 days age, the macro cracks
that for the reference specimen. During macroscopic failure, spread along the boundary of coarse aggregate.
the relative decreases in peak stress (sf ) observed for C-1d-10
and C-3d-10 were smaller than those observed for C-1d-40 and 3.2. Effect of early age loading on permeability of
C-3d-40. This indicates that an applied stress of 10% of the concrete
compressive strength of concrete at the time of loading had
little effect on the final strength development of the specimens According to Darcy's law, the water permeability of a con-
after 1 day and 3 days of curing because the stress level applied crete specimen under confining pressure can be calculated
at those times was insufficient to cause considerable change in using
specimen behavior. However, the internal structure of the
mQL
specimen loaded after 1 day was more unstable than that of the k¼ (6)
ADp
specimen loaded after 3 days [46]. The decrease in peak stress
caused by loading after 1 day of curing was thus slightly greater where k is the permeability in m2; m is the viscosity coefficient
than that caused by loading after 3 days of curing. The C-1d-40 of seepage water, that is 1.005  103 Pa at 20  C; A is the cross-
specimen was the most affected by early age loading, as its sectional area of the seepage water through the specimen in
peak strength was reduced by 34%, followed by the C-3d-40 m2; Dp is the osmotic pressure in Pa; Q is the flow rate in the
specimen, whose peak strength was reduced by 28%. It can
therefore be concluded that the earlier the loading age, the
more unstable the internal structure of concrete. If the load
applied to the concrete is sufficiently large relative to the curing
age, it will inevitably have an adverse effect on the develop-
ment of the internal structure, causing the peak stress to be
significantly reduced. According to the results of the uniaxial
compression tests conducted in this study, the early age load
applied to concrete should not exceed 40% of its strength at that
time, otherwise the subsequent safety of the concrete structure
will be seriously compromised.
The first row in Fig. 4 shows the fracture photographs of
each specimen type after loading, and the second row shows a
corresponding sketch of the fracture. Compared with the
specimen that was not subjected to early age loading, the
uniaxial compression failure of the concrete specimens
loaded at an early age exhibit obvious tensile failure surfaces Fig. 5 e Variation in initial permeability according to
and typical shear slip surfaces. The macroscopic cracks are specimen.
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Fig. 6 e Permeability variation curve under confining pressure for specimens (a) C-1d-10 (b) C-1d-40 (c) C-3d-10 (d) C-3d-40
(e) C-N-0.

water seepage specimen in m3/s; and L is the height of the shown in Fig. 6. In the loading stage, the permeability
specimen in m. decreased with increasing confining pressure. The decrease in
The permeability at the beginning of loading under a permeability was the greatest when the confining pressure
confining pressure of 2.0 MPa and pore water pressure of was increased from 2.0 MPa to 3.5 MPa, accounting for be-
1.3 MPa was defined as the initial permeability [47]. The initial tween 54.44% and 73.35% of the entire permeability decrease
permeability of each group of specimens is shown in Fig. 5, in over the duration of the test. It is believed that this was pri-
which it can be observed that the initial permeability of C-1d- marily caused by the initial crack and pore closure in the
40 was the highest, followed by C-3d-40. The initial perme- concrete, which considerably decreased the available seepage
ability of these two specimen groups was an order of magni- channels and thus the permeability. When confining pressure
tude greater than that of the other three groups. Thus, was first applied, cracks and pores were sensitive to increases
applying a load of 40% of the compressive strength of concrete in the confining pressure, which caused the cracks and pores
at an early age clearly results in a significant amount of initial to be compacted. As the confining pressure continued to in-
damage due to the corresponding change in the development crease, there were fewer cracks and pores that could be closed
of the internal structure of the concrete. The initial damage and compressed, resulting in a smaller reduction in perme-
reduces the number of pores and cracks in the internal ability. As the confining pressure was unloaded, the perme-
structure, which serve as the main channels for pore water ability gradually recovered, however, it did not reach the
seepage [48,49]. The earlier the age at which the load was initial permeability for each stage during confining pressure
applied, the greater the impact of this initial damage. The loading. This indicates that while the elastic deformation of
permeability of C-1d-10 was 6.64% less than that for C-N-0, but the specimen during the confining pressure unloading process
was 5.60% greater than that for C-3d-10. It is thought that can be recovered, the plastic deformation, which accounts for
under a small applied load, the initial cracks and pores in the a large proportion of the total deformation, is more difficult to
specimens were properly compacted, and new cracks and recover [50].
pores could not be generated, so the number of penetration In order to more intuitively describe the variation of the
channels was reduced and the permeability decreased. Criti- specimen permeability during the loading phase of the test
cally, the internal structure of concrete after 3 days of curing is under different confining pressures, the dimensionless
more stable than that after 1 day of curing, so the compaction permeability (DP) is used to reflect the influence of confining
effect is more significant and the permeability decrease is pressure sensitivity on permeability as follows.
more obvious in the latter case.
kil
The permeability curves of the five groups of specimens DP ¼ (7)
k0
evaluated under different confining pressures in this study are
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unloading, the attenuation dimensionless permeability


(ADP) is defined as:

kil  kiul
ADP ¼ (8)
kil
where kiul is the permeability of the ith stage under confining
pressure unloading, for which values of i ¼ 1, 2, and 3 corre-
spond to confining pressures of 2.0 MPa, 3.5 MPa, and 5.0 MPa,
respectively.
As can be observed in Fig. 8, the ADP tended to increase
during the gradual unloading of the confining pressure, cor-
responding to decreased permeability recovery performance
and indicating greater plastic deformation of the concrete
pore structure [51]. The analysis results thus demonstrate that
under low confining pressure, the pores and cracks in con-
crete were closed and strong plastic deformation occurred. As
Fig. 7 e DP curve of confining pressure loading section. a result, the ADP increased rapidly. Under high confining
pressure, the internal pores and cracks of the specimens were
all basically compacted, and the permeability reached a rela-
where k0 is the initial permeability and kil is the permeability tively low value; however, there remained some fine pores in
of the ith stage under confining pressure loading, for which the elastic deformation stage, so when the confining pressure
values of i ¼ 1, 2, 3, and 4 correspond to confining pressures of decreased, the permeability returned to its initial value, thus
2.0 MPa, 3.5 MPa, 5.0 MPa, and 6.0 MPa, respectively. decreasing the ADP. It can also be observed in Fig. 8 that the
As shown in Fig. 7, the DP curve shows a downward trend ADPs of the specimens subjected to an applied load of 40% of
with increasing confining pressure, which can be attributed to their compressive strength at either early age were signifi-
the unequal initial damage caused in concrete by the different cantly higher than those of the other three specimens, and
loading magnitudes and ages. The existence of pores and that the earlier the external load was applied, the greater the
cracks in this initial damage are compacted step-by-step with ADP. The results indicate that the internal pore structure of C-
increasing confining pressure. Clearly, the overall decrease in 1d-40 changed significantly, and that early age loading in-
DP was the largest for C-1d-40, as was the slope of each creases the quantity and size of pores and cracks in the con-
segment of the curve for this specimen. The results thus crete, even causing them to connect with each other, so that
indicate that the number of pores and cracks was the largest large plastic deformation of the pore structure occurs during
for this specimen, so the confining pressure had the greatest the later stages of applied confining pressure [52,53].
influence on the change in permeability. The results also show To compare the influence of different loading levels on the
that the initial damage caused by applying an external load of permeability of concrete loaded at different ages, the
40% of the strength at the time had the greatest influence after maximum permeability loss rate (MPLR) and permeability loss
1 day of curing. The overall decreases in DP for C-1d-10 and C- rate (PLR) are used to evaluate the reduction in permeability
3d-10 were lower than that for C-N-0, and when the confining and the degree of recovery, respectively. The reduction in
pressure was increased from 5.0 MPa to 6.5 MPa, the DP concrete permeability is higher for a specimen with a higher
changed very little for these specimens, indicating that the MPLR; the greater the PLR, the worse the recovery of concrete
number of pores and cracks that could be compressed inside
the specimen was extremely small. The initial damage caused
by an applied load of 10% of the strength at an early age was
observed to have less impact on the concrete DP than a 40%
applied load, and the later the age at which the external load
was applied, the smaller its adverse effect on DP. The change
in permeability according to applied confining pressure stage
can be divided according to DP: 2.0e5.0 MPa is the sensitive
area, in which the average DP was 61.43% and the attenuation
rate was the fastest; and 5.0e6.5 MPa is the insensitive area, in
which the average DP was 22.90% and the attenuation rate
was the slowest. This shows that the permeability of concrete
does not change uniformly with the increase in confining
pressure, and when the confining pressure is small, the
permeability decreases rapidly, then gradually slows, indi-
cating that the permeability of concrete is sensitive at the
initial stage and insensitive at the later stage to the increase in
confining pressure.
In order to more intuitively describe the permeability re-
covery under all levels of confining pressure during Fig. 8 e ADP curve of confining pressure unloading section.
1216 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 4 : 1 2 0 8 e1 2 2 1

permeability, and thus the greater the damage to the concrete


permeability.
The MPLR can be calculated by:

k0  kmin
MPLR ¼ (9)
k0
The PLR can be calculated by:

k0  kr
PLR ¼ (10)
k0
where kmin is the minimum permeability and kr is the
permeability under the minimum confining pressure during
unloading.
Table 4 shows that the MPLR and PLR of C-1d-40 were the
highest, followed by those of C-3d-40. It can be seen that
applying a 40% load at an early age had an adverse effect on
Fig. 9 e T2 spectrum distribution curve.
the development of the permeability of the specimens, and
the earlier the age of applied loading, the worse this effect. In
contrast, applying a 10% loading at an early age allowed the
specimens to be properly compacted, resulting in only a slight and that the signal amplitude reflects the number of pores
reduction in MPLR and PLR. [56,57].
The T2 spectrum distribution curve is shown in Fig. 9, in
which three obvious peaks can be observed, defined from
4. Mechanism of concrete macroscopic right to left as Peak 1, Peak 2, and Peak 3. The higher the
properties change under early age loading amplitude of the peak, the greater the number of pores in
the concrete specimen, and the longer the relaxation time
4.1. Pore structure characteristics of the peak, the larger the pore radius [57]. In Table 5, the
area under each peak of the T2 spectrum curves is reported
The macroscopic characteristics of the concrete mechanical to characterize the pore water content. When the age of the
property and permeability when subjected to the 10% and applied load was the same, the areas under Peak 1, Peak 2,
40% early age loading were found to be relatively similar in and Peak 3 increased with increasing load. The area under
Sections 3.1 and 3.2, as they are closely related to the effect Peak 3 with an applied load of 40% of the compressive
of loading on the internal structure of the specimens. strength exhibited the largest increase compared to C-N-0,
Therefore, once the cylindrical samples were prepared, the indicating that the applied load was sufficiently large to
MacroMR12 large-diameter NMR instrument was used to expand and connect the original small and medium pores
perform NMR tests to obtain the concrete pore distribution to form macropores. When load was applied at different
curve after the early age loading and to observe the changes curing ages, the primary macropores were more compacted
in the pore structure inside the specimen. Notably, NMR when subjected to a 10% load level: the area under Peak 3
technology has the advantages of not damaging the spec- decreased by 64.01% and 35.54% when loaded after 1 day
imen, allowing it to be reused (in this case, in the subse- and 3 days of curing, respectively, compared to C-N-0.
quent mechanical and permeability tests) [54]. The T2 When subjected to the 40% load level, a later loading age
spectrum data obtained by NMR reflects the distribution of corresponded to a decreased speed of macropore structure
the pore structure in the specimen, that is, the T2 value of development from 168.74% (1 day) to 130.62% (3 day),
pore water reflects the structure of the internal water indicating that the earlier the loading age, the more
environment [55,56]. The calculation principle used with obvious the effect of loading on the development of mac-
NMR is given by ropores. In summary, the T2 spectrum distribution curve
indicates that early age loading changes the original pore
1 S r
¼ rð Þ ¼ Fs (11) structure of concrete, and the earlier the age and higher the
T2 V R
load level, the greater the impact of loading on the pore
where R is the pore radius in um, r is the T2 surface relaxation structure.
strength in um/ms, S is pore surface area in cm2, V is pore As shown in Fig. 10, the pore size distribution curves of
volume in cm3, and Fs is the geometry factor. It can be the five specimen groups show three obvious peaks, again
observed in Eq. (11) that T2 is proportional to the pore radius, defined from left to right as Peak 1, Peak 2, and Peak 3,
corresponding to pore size ranges of 0.005e0.030 mm (small
pores), 0.3e2.4 mm (mesopores), and 5e350 mm (macro-
pores), respectively. It should be noted that the internal
Table 4 e MPLR and PLR for each specimen group.
pore structure of the specimens measured by NMR was
Specimen group C-N-0 C-1d-10 C-1d-40 C-3d-10 C-3d-40
mainly determined by the number of hydrogen ions in the
MPLR 76.26% 69.40% 93.33% 64.61% 81.91% water molecules in the specimens. Not only can the pores
PLR 63.78% 52.16% 86.61% 44.98% 78.70% in the concrete store water, but cracks can as well, so the
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 4 : 1 2 0 8 e1 2 2 1 1217

Table 5 e Area of each peak in T2 spectrum.


Specimen group C-N-0 C-1d-10 C-1d-40 C-3d-10 C-3d-40
Peak 1 area (a.u.) 68.35 74.46 97.60 72.77 85.54
Peak 2 area (a.u.) 236.79 267.07 339.97 262.29 308.03
Peak 3 area (a.u.) 12,671.33 4560.12 34,053.15 8161.56 29,222.22

pore distribution determined using the NMR results should 4.2. The observation of concrete microstructure by SEM
be generalized in a broad sense [58,59]. It can be seen from
Fig. 10 that C-1d-40 showed the highest distribution in Peak To further clarify the effect of early age loading on the internal
1, Peak 2, and Peak 3, indicating that there are many pores structure of concrete, a FlexSEM1000 with acceleration voltage
in this specimen. Wu [60] pointed out that the more pores of 0.3e20 kV and magnification of 55e300,000 was used to
there are in a specimen, the greater the impact of the initial observe the internal microstructure morphology of concrete
damage to the specimen on its permeability and mechani- affected by early age loading according to the standard of SEM
cal properties. Indeed, the initial permeability of C-1d-40 [63]. In order to ensure the realization of the research purpose
was the highest, and its mechanical properties decreased and the representativeness of the object, the sampling of the
the most. The proportion of small pores in Peak 1 of C-3d- object scanned by SEM is the section when the specimens are
40 was the smallest, but relatively increased in Peaks 2 and destroyed by uniaxial compression [26], and the sample size is
3; the proportion of macropores in Peak 3 was second only controlled at about 10 mm. The results of SEM show in Fig. 11,
to that of C-1d-40. This was much higher than that of the it can be clearly seen that when the load applied at the early
remaining three specimen groups. Thus, the mesopores age reaches 40% of the current concrete strength, the internal
and macropores were well developed, and the small pores microstructure has changed significantly, especially appeared
were compacted. Combined with the mechanical property the large width connectivity cracks, at the same time, the
and permeability measurement results, it is believed that compactness of the cementitious structure is obviously
an increase in the proportion of macropores in early age reduced, and there are some small cracks and holes on the
loaded concrete significantly reduces the macroscopic per- surface. The analysis suggests that this is due to the low
formance of the specimens. The proportions of mesopores strength and unstable internal structure of concrete at an
and macropores in C-1d-10 and C-3d-10 were close to or early age, which leads to the formation of cracks, resulting in
even less than those in the reference specimen, while the changes in the internal microstructure causing a reduction in
proportion of small pores was higher than that in the late macroscopic properties, which is consistent with the
reference specimen. This suggests that when a relatively substantial reduction in mechanical and permeability prop-
small load is applied at an early age, it is difficult to induce erties in this study. When loading at 10%, it can be found that
the original pore and crack expansion, and thus the influ- the arrangement between the particles of the specimens is
ence of the load is limited to the smallest pores. Mean- relatively uniform and neat, the cementitious structure is
while, it can be seen that the overall pore size distribution relatively tight, and there is almost no change compared with
of C-N-0 was very close to that of C-1d-10 and C-3d-10, the specimens of the benchmark group. In terms of macro-
which also showed similar mechanical property charac- scopic performance, the mechanical properties and perme-
teristics and permeability results in the macroscopic tests. ability of 10% early age loading are very close to those of the
The internal pore structure of a concrete specimen there- benchmark group.
fore has an important influence on its macroscopic per-
formance [61,62]. 4.3. Effect mechanism of early age loading on internal
crack development of concrete

The macroscopic properties of concrete are closely related to


the development of its internal cracks. In this study, the me-
chanical properties and permeability of concrete changed
which must be related to the variation in the path of internal
cracks development after being subjected to different levels of
early age loading. As shown in Fig. 12, there is a big difference
in the development of the internal crack structure between
the two when the external loads of 10% and 40% of the
compressive strength of concrete are applied respectively at
the age of 1 day. Since the 10% external load is too small to
cause a great change in the initial cracking; while the 40% load
is 4 times higher than that of the 10%, and the early age con-
crete strength is low, the internal structure development is
extremely unstable, which easily makes the initial stress point
position of crack development decrease or even below 40% of
Fig. 10 e Pore size distribution curve. the peak strength. Therefore, it can be seen that the external
1218 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 4 : 1 2 0 8 e1 2 2 1

Fig. 11 e Internal microstructure of concrete under early age loading (a) C-1d-10 (b) C-1d-40 (c) C-3d-10 (d) C-3d-40 (e) C-N-0.

load of 40% of the prevailing strength applied at 1 day can increased crack connectivity. When the early age load con-
cause significant changes in the internal crack structure, tinues to act for 14 days, the concrete continues to be cured
specifically in terms of more cracks, wider crack width, and without external load until 28 days. At this stage, the crack

Fig. 12 e Schematic diagram of effect of early age loading on crack development mode.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 4 : 1 2 0 8 e1 2 2 1 1219

structure development after 28 days is improved because of the number, width and connectivity of cracks, and an
the self-healing ability of the concrete compared with the increase in the number of macropores, a decrease in the
stage of early age loading [64]. However, due to the high degree compactness of cementitious structure, etc. These are
of variation in crack development caused by 40% of the early not conducive to the improvement of the macroscopic
age loading, the self-healing performance of concrete was still properties of concrete. Therefore, the structure should
limited at 28 days. The overall crack development of concrete be prevented from being subjected to a large construc-
subjected to early age loading at 3 days is basically the same as tion load prematurely in the construction process.
that at 1 day age, the difference is that the internal structure of
concrete at 3 days is more stable compared to 1 day, and the The results of this study are expected to serve as a refer-
impact on crack development is relatively small, since both ence for the improved design of concrete structures that will
the 1 day and 3 days are in the early age range, the difference be subjected to early age loading. Accurate design that con-
of the crack development between them is not particularly siders the effects of early age loading on the microscopic
large. characteristics and thus macroscopic behaviors of concrete
can ensure safe structures that perform as originally intended.

5. Conclusions
Declaration of Competing Interest
As it is becoming increasingly common for concrete structures
to bear loads at an early age during construction projects, the The authors declare that they have no known competing
changes in the mechanical property and permeability of con- financial interests or personal relationships that could have
crete under different loads at different curing ages were appeared to influence the work reported in this paper.
investigated in this study. A microscopic analysis of the inter-
nal pore structure changes was also conducted, and the rea-
sons for the observed variations in macroscopic performance
Acknowledgments
were thus determined. The following conclusions were ob-
tained from the results of this study.
This research was supported by the Anhui Provincial Natural
Science Foundation Youth Project (1908085QE185), Independent
(1) The magnitude of the load applied at an early age
Research Fund of The State Key Laboratory of Mining Response
should not exceed 40% of the compressive strength of
and Disaster Prevention and Control in Deep Coal Mines (Anhui
the concrete at that age, otherwise increasing numbers
University of Science and Technology) (SKLMRDPC20ZZ05),
of mesopores and macropores will develop in the con-
China Postdoctoral Science Foundation (2018M642502), National
crete, significantly deteriorating its mechanical prop-
Natural Science Foundation of China (51674006), National Col-
erty and permeability.
lege Students Innovation and Entrepreneurship Training Pro-
(2) Compared with the concrete that was not subjected to
gram (202010361023, S202110361046).
early age loading, it was found that once concrete was
subjected to early age loading, the crack stress point
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