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Construction and Building Materials xxx (xxxx) xxx

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Construction and Building Materials


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

Basic creep and fracture response of fine recycled aggregate concrete


Ange-Therese Akono a,b,⇑, Jiaxin Chen a, Mimi Zhan a, Surendra P Shah a
a
Department of Civil and Environmental Engineering, Northwestern University, United States
b
Department of Mechanical Engineering, Northwestern University, United States

h i g h l i g h t s

 FRCA mortar exhibits a high volume fraction of low-density C-S-H.


 The nanoporosity of the C-S-H is higher in FRCA than in NS mortar.
 The fracture toughness of FRCA mortar is 8% lower than that of NS mortar.
 The elastic modulus of FRCA mortar is less than half that of NS mortar.
 The logarithmic creep modulus is much lower for FRCA than for NS mortar.

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

Article history: We investigate the basic creep and fracture response of fine recycled aggregate concrete using nanoscale
Received 19 February 2020 mechanical characterization modules integrated with nonlinear micromechanical modeling and machine
Received in revised form 13 September learning methods. Fine recycled concrete aggregate mortar exhibits a larger volume fraction of microp-
2020
ores and low-density calcium silicate hydrates compared to natural sand mortar. In return, natural sand
Accepted 24 September 2020
Available online xxxx
mortar exhibits a larger volume fraction of hard aggregates. The macroscopic logarithmic creep modulus
for fine recycled concrete aggregate mortar is five times lower than that of natural sand mortar. Finally,
the fracture toughness of fine recycled aggregate concrete is 8% lower than that of plain concrete.
Keywords:
Recycled aggregate concrete
Ó 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
Creep indentation (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Fracture toughness
Scratch test

1. Introduction tools are needed to understand the creep behavior of recycled


aggregate concrete.
Recycling concrete aggregates represents a sustainable Although prior investigations have reported an increase in
approach for concrete production. The viability of the reuse of creep behavior for fine recycled aggregate mortars, the underlying
demolition concrete waste and natural disaster concrete debris mechanisms are not fully understood. Domingo-Cabo et al. [5]
as a source of sand for new concrete synthesis was supported by showed that fully replacing coarse aggregates with recycled coarse
pilot projects at the structural scale [1,2]. Yet, a major hurdle aggregates in concrete cylinders leads to an increase of 51% in
towards the insertion of recycled concrete aggregates in industry creep deformation. Silva and coworkers [6] formulated theoretical
is the lack of durability data regarding recycled aggregate concrete. models for the prediction of the creep behavior of concrete struc-
In particular, creep is an important measure of durability and a tures made with coarse recycled concrete aggregates. Seara-Paz
major concern for concrete structures. For instance, severe deflec- et al. [7] studied the long-term deformation for cylindrical concrete
tions in long-span prestress concrete bridges have been linked specimens for up to 1000 days and reported higher creep deforma-
with concrete creep [3]. Concrete creep is a complex phenomenon tions for coarse recycled concrete aggregate mortar. After review-
that depends on multiple factors, one of them being the type of ing a significant amount of published data from 100 publications,
aggregates [4]. Thus, new investigations and advanced predictive Lye et al. [8] concluded that the creep strain increases as the
replacement fraction of coarse recycled aggregate increases and
they proposed an empirical formula to predict the creep of recycled
⇑ Corresponding author at: Department of Civil and Environmental Engineering, aggregate concrete. Cartuxo et al. [9] reported a logarithmic creep
Northwestern University, 2145 Sheridan Road Rm A132, 60208 Evanston IL, United evolution for fine recycled concrete aggregate mortar. In addition,
States.
they showed that the presence of superplasticizer significantly
E-mail address: ange-therese.akono@northwestern.edu (A.-T. Akono).

https://doi.org/10.1016/j.conbuildmat.2020.121107
0950-0618/Ó 2020 The Authors. Published by Elsevier Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article as: Ange-Therese Akono, J. Chen, M. Zhan et al., Basic creep and fracture response of fine recycled aggregate concrete, Construction
and Building Materials, https://doi.org/10.1016/j.conbuildmat.2020.121107
Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

improves the creep response of fine recycled concrete aggregate


mortar. The higher creep response of recycled aggregate concrete Specimen water absorption capacity (%) Specific gravity (g/cc)
has been attributed to the presence of residual mortar in recycled
NS 0.76 2.62
aggregates [10,11], and the higher porosity of recycled agrgegate FRCA 14.71 2.05
[12]. Yet, a fundamental understanding of creep mechanisms in
fine recycled concrete aggregate mortar is lacking.
Furthermore, the fracture response of fine recycled concrete tive is to understand the influence of the composition and
aggregate mortar is not fully understood. Bordelon et al. [13] con-
microstructure of fine recycled concrete aggregate on the fracture
ducted flexural tests on single-edge notched specimens for plain and creep properties of the resulting mortar.
concrete and recycled coarse aggregate concrete. They observed a
Both natural sand (NS) and fine recycled concrete aggregates
43% decrease in fracture energy due to the addition of coarse recy- (FRCA) were further characterized using water absorption tests
cled concrete aggregates. Guo et al. [14] reported a 20% reduction
and specific density tests, as shown in Table 1. The water absorp-
in fracture energy following three-point bending tests on notched tion capacity of fine recycled concrete aggregate, 14.71 %, is an
coarse recycled aggregate concrete. Their results resonate with the
order of magnitude greater than that of natural sand, 0.76%. Our
findings of Ghorbel & Wadeh [15]. Kazemian et al. [16] reported a tests agree with prior findings of a higher water absorption for fine
significant improvement in the fracture response of recycled recycled concrete aggregate[17]. Similarly, the specific density of
coarse aggregate concrete following pretreatment of the recycled
fine recycled concrete aggregate, 2.05 g/cc, is much smaller than
coarse aggregates in an acidic environment. However, despite that of natural sand, 2.62 g/cc.
numerous studies on recycled coarse aggregate concrete, few stud-
Table 1 displays the mix design of both natural sand mortar and
ies have examined the fracture behavior of fine recycled aggregate recycled concrete aggregate mortars. We followed standard ASTM
concrete.
C 305 for the casting procedure. After casting, the specimens were
We seek to investigate the durability of recycled aggregate con- poured into prismatic molds, covered with plastic film, and left to
crete with a focus on basic creep and fracture response. In partic-
cure for 24 h under vibration. Afterwards, the specimens were
ular, our aim is to predict the macroscopic basic creep and demolded and stored in a moist curing chamber at 20 ± 1 C for
connect the macroscale response to microstructural and chemical
24 h. The cured prismatic specimens were then stored in ethanol
features. To this end, we employ advanced nanoscale mechanical overnight to stop the hydration and stored under vacuum until fur-
testing such as scratch-based fracture testing and
ther processing.
nanoindentation-based creep testing integrated with machine
learning methods. First, we present our materials and experimen-
tal procedures, then, we describe the underlying theoretical frame- 2.2. Methods
work, and finally present and discuss our results.
2.2.1. Scanning electron microscopy analyses
We conducted environmental scanning electron microscopy
2. Materials and methods
(ESEM) observations on uncoated specimens using an environmen-
tal scanning electron microscope, FEI Quanta 650, in the Electron
2.1. Materials
Probe Instrumentation Center at the Northwestern University
Atomic and Nanoscale Characterization Experimental Center. ESEM
Both local sand and recycled concrete aggregate were provided
analysis was conducted under low vacuum with an accelerating
by Ozinga Concrete (Chicago, IL). We used only fine recycled con-
voltage of 15–25 kV, a walking distance of 11 mm, and a magnifi-
crete aggregates, with a diameter less than 4.75 mm. A brass sieve
cation level in the range  52–274.
was utilized to separate fine recycled concrete aggregates from
Prior to ESEM analysis, the specimens were prepared through a
coarse aggregates. Fig. 1 displays environmental scanning electron
rigorous grinding and polishing procedure in two steps. First, the
microscopy images of both natural sand and fine recycled concrete
natural sand and fine recycled concrete aggregate mortars speci-
aggregate. Natural sand is round and smooth, whereas fine recy-
mens were embedded in a low viscosity epoxy resin and cut in
cled concrete aggregate lays in a diffuse zone that is the interfacial
4-mm thin slices using a low-speed diamond saw. Second, the
transition zone. The thickness of the interfacial transition zone is
specimens were ground in stages using a semi-automated grinder
variable, reaching a maximum thickness of 100 lm. In addition,
polisher mounted with silicon carbide grinding pads with a fine-
the interfacial zone is composed of hardened cement paste, small
ness ranging from 50 lm down to 0.25 lm. In between each size
hard aggregate particles, microcracks, and micropores. Our objec-
of abrasive, the specimens were cleaned with N-decane using an
ultrasonic bath, and dried using compressed air.

2.2.2. Indentation testing


Creep indentation tests were conducted using an Anton Paar
nanohardness tester equipped with a Berkovich diamond indenter.
Prior to testing, the contact area function of the indenter was cal-
ibrated using a reference material. For both natural sand mortar
and fine recycled concrete aggregate mortar, a 20  20 indentation
grid was conducted with an inter-indent spacing of 20 lm, result-
ing in 400 indentations tests performed per material. Each inden-
tation test was characterized by a loading/unloading phase of
30 s, a holding phase of 180 s, and a maximum vertical load of 2
mN. The vertical force and penetration depth were measured using
Fig. 1. Environmental scanning electron microscopy images of a) natural sand, b)
transducers with an acquisition rate of 45 kHz and a resolution of
fine recycled concrete aggregate. (1)= hard aggregate. (2) = interfacial transition respectively 20 nN and 0.01 nm. All testing took place in an envi-
zone. (3) = epoxy resin. ronmental chamber to reduce the effect of drying creep.
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Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

Table 1 level and understand the influence of composition and microstruc-


Mix design for both natural sand (NS) mortar and fine recycled concrete aggregate ture on the long term behavior at the macroscopic scale. To this
(FRCA) mortar. SP = superplasticizer. NS = Natural sand. FRCA = Fine recycled
concrete aggregates. DI water = Deionized water. For both mix designs, the w/c ratio
end, we formulate a multi-scale conceptual model for mortar, that
is 0.44, the sand-to-cement ratio is 2 and the superplasticizer to cement ratio is 0.5%. is shown in Fig. 2. At the binder level, the micro-structure is porous
and heterogeneous and composed of calcium hydroxide, capillary
NS mortar (kg/m3) FRCA mortar (kg/m3)
pores, clinker, and small aggregates. These micro-constituents are
Cement 638.90 587.27 embedded in the calcium-silicate-hydrates (C-S-H) matrix. In turn,
DI water 281.10 258.38
SP 3.30 3.03
the C-S-H matrix is nanoporous and composed of low-density cal-
NS 1277.80 N. A. cium silicate hydrates and high-density calcium silicate hydrates.
FRCA N. A. 1174.55 An important question is to predict the long term mechanical
response at the macroscopic scale given the creep behavior of indi-
vidual microconstituents. Assuming a logarithmic dependence for
2.2.3. Scratch Testing the creep behavior of individual constituents and assuming a sta-
Microscopic scratch tests were conducted using an Anton Paar tistically disordered microstructure, nonlinear micromechanics
scratch tester with a Rockwell C scratch probe. The scratch probe solutions predict an effective creep response that obeys a logarith-
consists of a cone of half-apex angle 60 ended with a sphere of mic creep law [19]. In that case, the homogenized contact creep
tip radius R ¼ 200 lm. During each scratch test, the vertical force modulus C hom depends on the individual contact creep measure-
was linearly increased up to a maximum value of 5.5 N over a ment C i;16i6441 according to the following implicit equation [19]:
scratch length of 9 mm at a scratch speed of 18 mm/min. The ver-
tical and horizontal forces and the penetration depth were mea- X
441
1 X
441
C =C hom
 ¼  i  ð4Þ
sured using synchronized force sensors with a resolution of 0.1 i¼1
hom
1 þ 12 ðC i =C Þ  1 i¼1 1 þ 2 ðC i =C
1 hom
Þ1
mN and a displacement sensor with a resolution of 0.3 nm. For
both natural sand mortar and fine recycled concrete aggregate Similarly, the macroscopic plane strain modulus M hom can be
mortar, a set of 13 tests were conducted per material. obtained by application of a micromechanics consistent scheme
according to:
3. Theory
X
441
1 X
441
M =Mhom
 ¼  i  ð5Þ
3.1. Creep characterization via indentation testing hom
1 þ ðM i =M Þ  1 hom
i¼1 1 þ 2 ðM i =M Þ1
1 1
i¼1 2

In order to extract the viscoelastic parameters from indentation We solved the two implicit equations Eqs (4) and (5) using a
tests, we rely on analytical solutions developed by Vandamme and recursive algorithm implemented in the computer programming
Ulm [18] for indentation tests in viscous solids. The key idea is to language Python.
estimate the creep compliance LðtÞ from the increment in penetra-
tion depth during an indentation with a constant vertical load P. By
3.3. Fracture characterization via scratch testing
application of Hertzian contact solutions and of the viscoelastic
correspondence principle, the first time derivative of the creep
We applied nonlinear fracture mechanics to compute the frac-
compliance depends on the change in depth hðtÞ _ during the hold- ture parameters from the horizontal force F T and penetration
ing period according to [19,20]: depth d measurements during scratch testing. In particular, we uti-
_
2aU hðtÞ
lized the size effect law model for scratch testing that we previ-
_
LðtÞ ¼ ð1Þ ously developed in [25–28]. Consider a scratch test with an
Pmax
axisymmetric probe as depicted in Fig. 3. A is the horizontally
where P max ¼ 2 mN is the maximum load, and aU is the contact projected-load bearing contact area whereas p is the perimeter.
radius at maximum load. Moreover, we adopt a logarithmic model Both A and p are functions of the scratch probe geometry and of
[21] for the contact creep compliance because the creep behavior of
concrete structures, such as prestressed concrete bridges [3] and
cylindrical and prismatic concrete specimens [22], has been shown
to obey a logarithmic law within the 3–10 year span. Our logarith-
mic model reads as follows:
 
1 1 t
LðtÞ ¼ þ ln 1 þ ð2Þ
M 0 4C s
where M0 is the initial plane strain indentation modulus, C is the
contact creep modulus, and s is the logarithmic creep characteristic
time. Although we have chosen to use a logarithmic creep law to
interpret the microindentation creep tests, an alternative is to use
a power-law function [23]. Finally, the initial plane strain modulus
M0 and the indentation hardness H are computed according to [24]:
1 S Pmax
M¼ ; H¼ ð3Þ
2 aU pa2U

3.2. Homogenization of basic creep characteristics


Fig. 2. Multiscale conceptual model of natural sand mortar and fine recycled
We seek to probe the creep response of both natural sand and concrete aggregate mortar. C-S-H = calcium silicate hydrates. CH = calcium
fine recycled concrete aggregate mortar at the micro-constituent hydroxide.

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Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

4. Results

4.1. Microstructural characteristics

We employed environmental scanning electron microscopy to


explore the microstructure of both natural sand mortar and fine
recycled concrete aggregate mortar as shown in Fig. 4. Moreover,
we conducted a statistical deconvolution of the gray level his-
togram so as to identify chemical phases based on their gray levels.
Figs. 4 a) -b) display the raw ESEM images. For natural sand mortar,
we observe angular hard grains, 200–700 lm in size, laying in a
porous matrix composed of calcium silicate hydrate phases, micro-
pores, and calcium hydroxide (in light grey). For fine recycled con-
crete aggregate mortar, we observe a single micropore of diameter
120 lm. In addition, we observe hard grains, 100–300 lm in size,
laying in the porous matrix made of calcium silicate hydrate
phases and calcium hydroxide.
We conducted a cluster analysis to identify chemical phases
Fig. 3. Schematic representation of a scratch test in a heterogeneous material. a) based on the grey levels. Figs. 4 c) -d) display the phases identified.
Side view. b) front view. F T is the horizontal force, d is the penetration depth, p is For natural sand mortar, hard grains or hard aggregates account for
the perimeter, and A is the horizontally-projected load-bearing contact area.
more than 45% of the microstructure. In contrast, for fine recycled
concrete aggregate mortar, hard grains account only for 26% of the
the penetration depth d. Based on experimental observations microstructure. However, our phase analysis based on grey level
[29,30], we assume the presence of a semi-horizontal crack ema- faces some limitation as there are similarities between the gray
nating from the tip of the probe. For a fracture-dominated process level signature of aggregates and C-S-H phases. Thus, additional
in a brittle materials, the linear elastic fracture mechanics (LEFM) spatially-resolved nanoscale mechanical probing is required. Nev-
solution was formulated to evaluate the energy release rate. To this ertheless, environmental scanning electron microscopy observa-
end, the J-integral was utilized in which the change in elastic strain tions predict a higher volume fraction of C-S-H and a lower
energy is evaluated from the perspective of an observer tied to the volume fraction of hard aggregates for fine recycled concrete
tip of the moving crack. The equation that connects the horizontal aggregate mortar compared to natural sand mortar.
force F T to the fracture toughness K c and the penetration depth d
reads [31–33]:
4.2. Creep compliance curves

pffiffiffiffiffiffiffiffiffi Fig. 5 a) displays the indentation response of select microcon-


FT ¼ Kc 2pA ð6Þ
stituents: micropores, low-density calcium silicate hydrate, high-
density calcium silicate hydrate, calcium silicate hydrate mixed
where 2pA is the scratch probe shape function, which is calibrated with calcium hydroxide (C-S-H + CH), and hard aggregate. Signifi-
using a reference material. However, cement-based composites are cant differences in both the indentation response and the creep
quasi-brittle materials, meaning that their behavior is intermediate response are observed. The indentation curve on hard aggregate
between brittle and ductile. Moreover, quasi-brittle materials such yields the lowest maximum penetration depth, 172 nm. Mean-
as cementitious materials are characterized by a large nonlinear while, the maximum penetration depth is 285 nm, 427 nm, and
softening zone or fracture process zone, which is the siege of non- 608 nm for respectively calcium silicate hydrates mixed with cal-
linear behavior such as distributed microcracking or void coales- cium hydroxide, high-density calcium silicate hydrate, and low-
cence. Upon microcracking a stress redistribution occurs leading density calcium silicate hydrate. The indentation curve on the
to a structural size effect. In the case of scratch testing, the energetic micropore yields the highest maximum penetration depth,
size effect law reads [25–28]: 873 nm. Given that the plane strain elastic modulus and the inden-
tation hardness are calculated from respectively the slope at
unloading and the maximum penetration depth according to Eq.
0
Bf (3), the indentation curves indicate that the microconstituents
rN ¼ qffiffiffiffiffiffiffiffiffiffiffiffi
t
ffi ð7Þ
can be ranked according to their strength and elastic properties.
1 þ DD0
The creep response for the binder micro-constituents is shown
in Fig. 5 b). The hard aggregate hardly creeps as the penetration
depth remains almost constant during the holding phase. For the
where rN ¼ FAT is the nominal strength, D ¼ A=ð2pÞ is the nominal remaining constituents, we observe a monotonic increase in the
0
size and Bf t and D0 are the size effect law parameters. The fracture penetration depth as the vertical force is held constant and equal
toughness is then correlated to the size effect law parameters via: to 5 mN. The C-S-H + CH phase registers a 6% increase in penetra-
tion depth whereas the high density C-S-H and the low-density C-
0
pffiffiffiffiffiffi S-H phases register respectively a 9% and 11% increase in penetra-
K c ¼ Bf t D0 ð8Þ tion depth. The increase in penetration depth is related to the mag-
nitude of the logarithmic creep modulus according to Eqs. 1,2.
We employed a nonlinear constrained optimization scheme to
0 Thus, a higher creep deformation is observed for low-density C-
compute the size effect law parameters, Bf t and D0 . Defining
S-H than for high-density C-S-H.
x ¼ lnðDÞ and y ¼ lnðrN Þ, the model function is y ¼ ln pffiffiffiffiffiffiffiffiffiffiffiffiffiffi
M
.
NþexpðxÞ The differences in creep response between low-density C-S-H
The size effect law parameters are then computed form the con- and high-density C-S-H is due to the local structural arrangement.
stants M and N as: K c ¼ M; D0 ¼ N. We used Jenning’s C-S-H colloidal model [34] for C-S-H consisting
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Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

Fig. 4. Environmental scanning electron microscopy images of mortars. a) and c) Natural sand mortar; b) and d) Fine recycled concrete aggregate mortar.

of 4-nm globules that are packed in clusters. Each saturated glob- signatures—values of M and H— that have been reported in the sci-
ule consists of layered C-S-H and the chemical formula for globule entific literature [20,19]. The indentation modulus of low-density
is 1.7 CaOSiO21.4 H2O [35]. The globules are spheroidal in shape C-S-H is MðLD C  S  HÞ ¼ 17:11 GPa, whereas for high-density
[36–39]. As a result of the granular structure, the creep mecha- C-S-H, and for C-SH + C–H, the indentation modulus is respectively
nisms in calcium silicate hydrates involve the motion of interlayer MðHD C  S  HÞ ¼ 26:03  29:05 GPa and MðC  S  H þ CHÞ ¼
water, the motion of C-S-H globules, friction between C-S-H nano- 54:40  60:33 GPa. Similarly, the logarithmic creep modulus for
grains, and the rearrangement of nanopores and nanoscale parti- low-density C-S-H is CðLD C  S  HÞ ¼ 29:26 GPa, and for high-
cles. For instance, Alizadeh et al. [40] showed that the density C-S-H and for calcium hydroxide mixed with C-S-H, we
viscoelastic response of C-S-H is due to the motion of the interlayer have respectively CðHD C  S  HÞ ¼ 53:93  59:67 GPa and
water along with bonds breakage and new bonds formation during CðCH þ C  S  HÞ ¼ 216:52  312:86 GPa. In particular, the loga-
the motion of C-S-H globules. Vandamme and Ulm showed that the rithmic creep modulus of C-S-H mixed with C–H is almost five
long term logarithmic creep of concrete is due to the rearrange- times higher than that of low-density C-S-H. As for hard aggre-
ment of nanoscale particles [41,42]. Low-density C-S-H corre- gates, their indentation modulus and logarithmic creep modulus
sponds to a disordered packing of C-S-H globules whereas are almost an order of magnitude higher than that of low-density
high-density C-S-H corresponds to an optimal packing order of C-S-H. Thus, the large differences in mechanical response between
C-S-H globules. As a result of packing order differences, disordered micro-constituents will influence the overall mechanical response.
vs. optimal, there is a wider range of degrees of freedom enabling We observe stark microstructural and compositional differ-
motion and resulting in a larger creep deformation of low-density ences between natural sand and fine recycled concrete aggregate
C-S-H compared to high-density C-S-H. mortar. Natural sand mortar has a higher volume fraction of hard
aggregates, 43%, compared to fine recycled concrete aggregate
4.3. Chemo-mechanical phase distribution mortar, 16%. In contrast, fine recycled concrete aggregate mortar
has a significant fraction of micropores, 15%, and a higher fraction
In order to assess the distribution of chemo-mechanical phases, of low-density C-S-H, 33%, compared to natural sand mortar. In
we performed a statistical deconvolution analysis. The principle of turn, natural sand mortar exhibits a higher fraction of high-
statistical deconvolution is, for each material, to represent the dis- density C-S-H, 45%, and of C-S-H mixed with CH, 12%, compared
tribution of the indentation moduli, indentation hardness values, to fine recycled concrete aggregate mortar, respectively 35% and
and logarithmic creep values ðMi ; Hi ; C i Þ16i6400 as a mixture of indi- 9%. Thus the presence of fine recycled concrete aggregate has an
vidual phases, each phase being characterized by a Gaussian distri- impact on the proportion of hydration products, the pore structure,
bution [43]. We utilized an Expectation Maximization algorithm and the gel porosity of the resulting mortar.
along with a Bayesian information criterion [44] to identify the We quantified the total porosity in both natural sand mortar
optimum number of phases. and fine recycled concrete aggregate mortar. The micro-porosity
Table 2 displays the characteristics of the microconstituents is given from the phase distribution after the statistical deconvolu-
identified and Figs. 6,7 display the phase distribution using cluster tion analysis, whereas the nano-porosity is computed from the
analysis graphs. The calcium hydrated phases, low-density C-S-H volume fraction of low-density calcium silicate hydrates and
and high-density C-S-H, were identified based on their mechanical high-density calcium-silicate-hydrates according to:

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Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

the larger fraction of low-density C-S-H. The total porosity of fine


recycled concrete aggregate mortar is significantly higher than that
of natural sand mortar. This result agrees with prior studies that
reported a more porous microstructure for fine recycled concrete
aggregate mortar. For instance, Gomez-Soberon et al. using Nitro-
gen gas adsorption tests [45] and mercury intrusion porosimetry
tests [46] reported an increase in porosity values for mortar with
various levels of replacement of coarse aggregates with coarse
recycled concrete aggregates. Similarly, Kou et al. [47] reported
higher levels of porosity for concrete cylinders cast using recycled
concrete aggregates even 5 years after curing, although in their
study they used coarse recycled aggregates. These studies resonate
with Chakradhara et al.’s investigation [48] that found a higher
pore ratio for concrete specimens with recycled coarse aggregate.
However, the underlying reasons for the higher porosity of recy-
cled aggregate mortar were not explained. In turn, our study
uncovers the determinants of porosity in fine recycled concrete
aggregate mortar, namely the higher levels of microporosity and
the larger volume fraction of low-density C-S-H.
An important consequence for the higher porosity of fine recy-
cled concrete aggregate mortar is a higher permeability, thereby
facilitating water and chloride ion transport. Prior studies have
related the porosity to environmental attack such as chloride ions
and carbonation. For instance, the diffusivity of chloride ions and
the permeability of water for mortar was shown to be strongly cor-
related to the hydration degree, the water-to-cement ratio, and to
the pore structure [49]. For instance, for concrete with w/c = 0.4
and at a 75% hydration degree, the critical pore radius was found
to be equal to 17 nm. Thus, the larger nanoporosity of fine reycled
concrete aggregate mortar poses real issues for durability. Our
findings agree with studies by Levy and Helene [50] who reported
a higher water absorption for concrete cast using both coarse and
fine recycled concrete aggregates.

4.4. Fracture response

Fig. 5. Indentation curves (a) and creep behavior (b) of chemomechanical micro- Figs. 8 a) and b) display representative residual panoramas after
constituents of natural sand mortar and fine recycled concrete aggregate mortar.
scratch tests respectively on natural sand mortar and on fine recy-
1 = micropores. 2 = low-density C-S-H. 3 = high density C-S-H. 4 = Calcium
Hydroxide mixed with C-S-H. 5 = Hard aggregate. cled concrete aggregate mortar. The residual panorama on natural
sand mortar displays several grains and few pores. In contrast, the
grains are sparser and there are more microvoids on the residual
u ¼ /LDCSH ð1  gLDCSH Þ þ /HDCSH ð1  gHDCSH Þ ð9Þ panorama of the fine recycled concrete aggregate mortar, pointing
to stark microstructural differences. Figs. 8)) c)- d) display the
where gLDCSH ¼ 0:65 is the packing density of low-density C-S-H and energetic size effect law in dimensionless form applied to both nat-
gHDCSH ¼ 0:74 is the packing density of high-density C-S-H [19]. ural sand mortar and fine recycled concrete aggregate mortar.
Table 3 lists the values of the nanoporosity and of the total porosity Overall, the experimental data points are distributed along the
for both natural sand mortar and fine recycled concrete aggregate ductile-to-brittle transition curve with a convergence toward the
mortar. linear elastic fracture mechanics curve for large D=D0 values. The
The nanoporosity of fine recycled concrete aggregate mortar, brittleness index D=D0 ranges from 0.01 to 100 for both natural
21%, is twice higher than that of natural sand mortar, 12%, due to sand mortar fine recycled concrete aggregate mortar. The presence

Table 2
Chemo-mechanical phase distribution for natural sand mortar and fine recycled concrete aggregate mortar. M is the plane strain modulus, H is the indentation hardness, C is the
logarithmic creep modulus, and s is the logarithmic creep characteristic time. HD C-S-H = high density C-S-H. CH = calcium hydroxide.

Phase Vol (%) M, GPa H, GPa C, GPa


Natural Sand Mortar
HD C-S-H 45 29.05 0.82 53.93
C-S-H + CH 12 60.33 2.07 216.52
Hard aggregates 18 110.60 5.77 897.13
Hard aggregates 25 116.29 12.19 4150.77
Fine Recycled Concrete Aggregate Mortar
Micropores 15 10.04 0.28 14.31
LD C-S-H 33 17.11 0.53 29.26
HD C-S-H 35 26.03 0.88 59.67
CH + C-S-H 9 54.40 2.35 312.86
Hard aggregates 7 104.86 8.54 2057.68

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Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

Fig. 6. Chemo-mechanical phase distribution in a) natural sand mortar and b) fine recycled concrete aggregate mortar. For each material, N ¼ 400 nanoindentation tests were
conducted. M is the plane strain modulus and C is the logarithmic creep modulus.

Fig. 7. Chemo-mechanical phase distribution in a) natural sand mortar and b) fine recycled concrete aggregate mortar. For each material, N ¼ 400 nanoindentation tests were
conducted. M is the plane strain modulus and H is the indentation hardness.

5. Discussion
Table 3
Pore structure of natural sand (NS) and fine recycled concrete aggregate (RCA) 5.1. Macroscopic basic creep properties
mortars.

NS mortar RCA mortar Table 5 lists the homogenized values of the creep modulus C hom
microporosity (%) 0 15 and of the plane strain modulus M hom for both natural sand and fine
nanoporosity (%) 12 21
recycled aggregate mortar. We predict a 50% decrease in the elastic
Total porosity (%) 12 37
modulus by replacing 100% of natural sand with fine recycled
aggregate concrete. Similarly, Evangelista and Brito [53] reported
of low values of the brittleness index, in the [0.1,10] range, points an 18% decrease in elastic modulus for concrete cubes with fine
toward the predominance of nonlinear fracture behavior. Thus, we recycled concrete aggregates; however, their concrete cubes con-
observe a nonlinear fracture behavior with a convergence toward tained natural coarse aggregates, which explained the lower value
brittle fracture for large penetration depths. of the decrease in elastic modulus. In turn, our findings are consis-
Table 4 lists the values of the size effect law characteristic tent with the study of Xiao et al. [54]. They conducted uniaxial
length D0 and of the fracture toughness. For natural sand mortar, compression tests on 100  100  100 mm concrete cubes cast
pffiffiffi
the fracture toughness is K c = 0.86 ± 0.15 MPa m. This value is in with coarse recycled concrete aggregate. A 45% reduction in elastic
agreement with tabulated values of the fracture toughness for modulus was observed for a 100% coarse aggregate replacement
plain concrete [51,52]. A high variability (17%) of the fracture ratio. In our study, we trace back the lower elastic modulus of fine
toughness is observed for natural sand concrete, and this variabil- recycled concrete aggregate concrete to the pore structure and the
ity is much higher (19%) for fine recycled concrete aggregate mor- packing density of C-S-H phases.
tar. An 8% decrease in fracture toughness is observed for fine The macroscopic logarithmic creep modulus for fine recycled
recycled concrete aggregate mortar compared to natural sand mor- concrete aggregate is found to be five times greater than that of
tar. Our findings agree with macroscopic fracture tests conducted natural sand mortar. Our results are in sharp contrast with Silva
on recycled coarse aggregate concrete in the scientific literature et al.’s results [6] that found that the creep coefficient for concrete
[13,14,16,15]. Thus, replacing natural sand by fine recycled con- made with 100% recycled concrete aggregate will not exceed 1.8
crete aggregate results in a decrease in the mortar resistance to times the creep coefficient of plain concrete; however, in their
crack propagation. study, they used coarse recycled concrete aggregates. Similarly,

7
Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

Fig. 8. Residual panoramas after scratch testing on a) natural sand mortar and b) fine recycled concrete aggregate mortar. Energetic size effect law applied to scratch tests on
a) natural sand mortar, and b) fine recycled concrete aggregate mortar. rN is the nominal strength, D is the nominal size and Bf t and D0 are size effect law parameters.
0

Table 4 displays 1-lm wide semi-circular fracture surfaces 20-lm apart


Fracture characteristics of natural sand (NS) and fine recycled concrete aggregate on the residual groove. Fig. 9 c)-d) focuses on specific fracture pro-
(RCA) mortars. K c is the fracture toughness, D0 is the size effect law characteristic
length and RMSE is the root mean squared error.
cesses with magnification levels 5,000–20,000. The fracture
micro-mechanisms observed include: distributed micro-cracking,
NS mortar RCA mortar ligament bridging, debris bridging, and void creation. Similar frac-
D0 ; lm 0.82 ± 1.55 1.59 ± 2.26 ture processes have been observed on plain Portland cement con-
pffiffiffi
K c MPa m 0.86 ± 0.15 0.79 ± 0.15 crete following scratch testing [58]. Thus, similar fracture
RMSE 0.0356 ± 0.0169 0.0145 ± 0.0308
micromechanisms exist between fine recycled concrete aggregate

Table 5
Homogenized creep modulus C hom and plane strain modulus M hom for natural sand
(NS) and fine recycled concrete aggregate (RCA) mortars.

NS mortar RCA mortar

C hom , GPa 253.60 46.51


M hom , GPa 55.15 22.35

using a normal mixing approach, Tam & Tam [55] reported a creep
coefficient 2 times higher for concrete with fine recycled concrete
aggregates and natural coarse aggregates. Our findings agree with
cartuxo et al.’s study who found a 2.7 times increase in creep defor-
mation for a full replacement of natural sand by fine recycled con-
crete aggregate [9]. Moreover, our study shows that the higher
creep modulus of fine recycled concrete aggregate is due to the
higher levels of microporosity, the larger fraction of low-density
C-S-H and the lower volume fraction of hard aggregates. In the
future, we will use more sophisticated creep models [56,57] to
fully understand the influence of a complex microstructure and
chemistry on the creep response of fine recycled aggregate
concrete.

5.2. Fracture micromechanisms

Fig. 9 diplays the fracture micromechanisms of fine recycled


concrete aggregate mortar following scratch testing. Fig. 9 a) Fig. 9. Fracture micromechanisms in fine recycled concrete aggregate mortar.

8
Ange-Therese Akono, J. Chen, M. Zhan et al. Construction and Building Materials xxx (xxxx) xxx

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