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Theoretical and Applied Fracture Mechanics 90 (2017) 133–141

Contents lists available at ScienceDirect

Theoretical and Applied Fracture Mechanics


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

Fractal analysis of crack paths into innovative carbon-based


cementitious composites
L. Restuccia a,⇑, A. Reggio a, G.A. Ferro a, R. Kamranirad b
a
Department of Structural, Geotechnical and Building Engineering, Politecnico di Torino, 10129 Turin, Italy
b
Department of Structural Engineering, Tarbiat Modares University, Tehran, Iran

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

Article history: Fractal geometry has been widely used in literature to characterize the mechanical behaviour of quasi-
Received 3 March 2017 brittle materials. In this work, innovative cementitious composites with carbon-based pyrolyzed
Revised 21 March 2017 micro-aggregates were tested until complete fracture and their fracture behaviour was studied in the
Accepted 21 March 2017
light of fractal geometry. Images of the crack paths across the tested specimens were acquired by
Available online 22 March 2017
Scanning Electron Microscopy (SEM) and their fractal dimension was calculated via the box counting
method. Results show that the pyrolyzed micro-aggregates, characterized by high strength and stiffness
Keywords:
due to their significant carbon content, are able to alter the crack path by increasing its tortuosity, thus
Cementitious composites
Crack path
inducing toughening mechanisms in the cementitious composites. This favourable behaviour is explained
Fractal dimension by means of fractal geometry: it is found that, the greater the fractal dimension of the crack path, the
Box counting higher the fracture energy.
Fracture energy Ó 2017 Elsevier Ltd. All rights reserved.
Fracture toughness

1. Introduction ture toughness, reporting a fractal dimension of 2.087 for cement


paste and of 2.117 for fine mortar; Saouma and Barton [12] showed
The word fractal, from the Latin adjective fractus, meaning bro- that cracked concrete surfaces are fractal and determined the frac-
ken, was coined by Mandelbrot in his fundamental essay [1] to tal dimension of their one-dimensional fracture profiles in the nar-
describe objects that were too irregular to fit into a traditional row range from 1.06 to 1.12. Fractal geometry has also been used
Euclidean geometrical setting, where points, lines, surfaces, and for explaining the size effects on the mechanical properties of
volumes have integer topological dimensions of 0, 1, 2, and 3, cementitious materials. In particular, a multifractal scaling law
respectively. Falconer [2] developed the fractal theory into the (MFSL) has been defined, according to which the decrease in the
mathematical field, giving prominence to the concept of fractal nominal tensile strength of concrete with the increasing size of
dimension, a measure of self-similarity and irregularity across specimen is due to the influence of the microstructure disorder
scales, which can assume fractional values. Since then, fractal [13–15]. Moreover, a similar approach has been used together with
geometry has been widely used in material science and engineer- fragmentation theory to account for size effects on dissipated
ing to quantitatively describe complex non-smooth objects, such energy density in compression [16]. Issa et al. [17] analyzed the
as rough surfaces [3] or grain boundaries [4], whose fractal dimen- fracture surfaces of normal strength concretes with four different
sion is usually greater than their topological dimension. Numerous maximum aggregate sizes, highlighting their fractal characteristics
fractographic studies have also reported that fracture surfaces [5] and deriving a linear correlation between the fractal dimension of
and crack paths [6] exhibit self-similar fractal nature and can be fracture surface, with values between 2.15 and 2.29, and the frac-
analyzed by fractal geometry in order to characterize their rough- ture toughness of concrete, represented by fracture energy; a sim-
ness and correlate it with mechanical properties [7]. This kind of ilar result was reported in [18], although a simple relation between
approach has been successfully applied to cement-based materials fractal dimension and fracture energy could not be established, and
[8]: the surface of hydrated Portland cement paste has been proved fractal dimension of crack paths was found to range from 1.03 to
to be fractal in character [9,10]; Lange et al. [11] demonstrated a 1.25 depending on the nature of aggregates and the resolution of
positive correlation between fracture surface roughness and frac- the processed images.
Following up previous studies concerning the mechanical beha-
viour and the manufacturing optimization of cementitious com-
⇑ Corresponding author. posites with carbon-based inerts [19–22], the aim of the present
E-mail address: luciana.restuccia@polito.it (L. Restuccia).

http://dx.doi.org/10.1016/j.tafmec.2017.03.016
0167-8442/Ó 2017 Elsevier Ltd. All rights reserved.
134 L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141

work is to apply fractal geometry to innovative composites with


pyrolyzed hazelnut shells added as micro-aggregates, in order to
explain the toughening mechanisms observed in their experimen-
tal fracture behaviour [23,24]. Three Points Bending (TPB) tests
until complete fracture were carried out on prismatic specimens
made of the innovative cementitious composites and of a plain
cement paste. The addition of a small amount of carbonaceous
micro-aggregates strongly influenced the mechanical perfor-
mances of the cement paste, resulting in a significant increase in
strength together with an increment in fracture energy, and then
in ductility. Images of the crack paths across the tested specimens
were acquired by Scanning Electron Microscopy (SEM), subse-
quently adjusted and binarized via image processing techniques
and later examined via fractal geometry. The fractal dimension of
the crack paths was calculated by implementing an algorithm
based on the box counting method and a relationship with the val-
ues of fracture energy computed from the experimental loading
curves was finally established. The analysis of the results shows
that the increment of the fracture energy due to the addition of
the carbonaceous micro-aggregates is strongly related to an incre-
ment of fracture surface tortuosity.

2. Materials and methods

2.1. Manufacturing of materials and specimens

Cementitious composites were manufactured by using ordinary


Portland cement (Type I, CEM I 52, 5R, light grey color), deionized
water and by adding to the cement paste carbon-based micro-
aggregates produced from the pyrolysis of hazelnut shells. Fig. 1. TPB test setup.
Pyrolysis was carried out into a hermetically sealed reactor,
where an inert environment was ensured by a continuous flowing A total of 32 prismatic specimens of dimensions 20 mm 
of nitrogen. A heating ramp of 6 °C/min was held for 1 h, reaching a 20 mm  75 mm were manufactured by casting the mixtures into
final temperature of 800 °C. After the pyrolysis process, the mate- acrylic molds and letting them mature for 24 h at room tempera-
rial was collected from the reactor, grinded for 10 min into a plan- ture in airtight plastic containers with 90% humidity level. After
etary mill to crush the bigger particles, and then milled for 1 h maturation, the specimens were removed from the molds and
using ethanol and alumina balls of 2 mm diameter. At the end of immersed in tap water for curing. At the end of a curing time of
the grinding cycle, the particle size was analyzed by laser granu- either 7 or 28 days, the specimens were notched by means of a
lometry using a Malvern Particle Sizer, obtaining an average value Remet type TR100S abrasive cutter with 2 mm thick diamond
in the range of a few nanometers to 10 lm. cut-off wheel, realizing a 6 mm deep U-shaped notch.
Mixing procedure is crucial for the performance of cementitious
composites [25], hence the same procedure described here was fol-
lowed to manufacture all the specimens. The pyrolyzed particles
were dispersed in a solution of water and superplasticizer (Mapei 2.2. Experimental tests
Dynamon SP1), the latter intended for limiting as much as possible
the re-agglomeration problem of the particles [26,27] and for keep- Each notched specimen was subjected to a crack mouth opening
ing the water to cement (w/c) ratio equal to 0.35. The solution was displacement-control Three Points Bending (TPB) test. TPB tests
sonicated in an ultrasonic bath for 15 min and then transferred were performed using a single column Zwick Line-Z010 testing
into the mixing bowl of a homogenizer. The cement was gradually machine equipped with a 1 kN load cell and a clip-on strain gauge
added to the solution while operating the homogenizer at 440 rpm to measure the Crack Mouth Opening Displacement (CMOD), as
for 2 min. Afterwards, the homogenizer speed was increased to shown in Fig. 1; a span length of 65 mm and a displacement rate
630 rpm for further 2 min, up to a total mixing time of 4 min. Var- of 0.005 mm/min were adopted.
ious percentages of addition of pyrolyzed particles with respect to Besides the mechanical tests, the chemical characterization of
the cement weight were considered, in agreement with previous pyrolyzed hazelnut shells was carried out using the X-Rays Fluo-
studies [28–30], and four different mixtures were obtained. The rescence (XRF) technique. The chemical composition reported in
weights of the materials used for each mixture are reported in Table 2 shows that the pyrolyzed particles are almost exclusively
Table 1. made of carbon and present very low percentages of impurities.

Table 1
Weights of the materials used for each mixture.

Mixture ID Cement (g) Water (g) w/c (–) SP1 (g) Pyrolyzed hazelnut shells (g) Pyrolyzed hazelnut shells (%)a
PLAIN CEM 214 74.9 0.35 3.21 – –
PY-HS_0.5% 214 74.9 0.35 3.21 1.07 0.5
PY-HS_0.8% 214 74.9 0.35 3.21 1.71 0.8
PY-HS_1% 214 74.9 0.35 3.21 2.14 1.0
a
Percentage with respect to the cement weight.
L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141 135

Table 2
Chemical composition of pyrolyzed hazelnut shells by XRF.

Components C Si Mg K Ca P Zn S Cr Cu Fe
Weight% 97.9 0.11 – 1.01 0.44 0.05 – 0.02 0.02 0.19 0.25

2.3. Analysis of fractal geometry 2.3.2. The box counting method


Box counting is one of the most effective and useful method for
2.3.1. Image processing obtaining fractal dimensions. The procedure is here applied by cov-
A prerequisite for the application of the box counting method is ering the image of the crack path by a mesh grid of characteristic
the detection of the crack path edge by means of image processing length rk and counting the number Nk of grid boxes needed to over-
techniques. lap the crack path. The count is repeated by increasing the box size
SEM images are in grayscale, with each pixel color specified by a until the largest box fits the whole image and trivially returns 1 for
number ranging from 0 (black) to 255 (white), while binary the box number. If the crack path exhibits fractal geometry, the
images, including pixel values equal to either 0 (black) or 1 (white), relationship between Nk(rk) and rk obeys a power law [2]:
are needed for the edge detection. To transform a grayscale image
into a binary one, the image quality must be first enhanced by
Nk ðr k Þ  cr D
k ð1Þ
adjusting contrast and sharpness and filtering the noise; after- where c is a constant and D is the fractal dimension of the crack
wards, a threshold level is set so that pixels with values smaller path. Taking logarithms of (1) and reporting the data points (log rk,
than the threshold are assigned to be equal to zero, while pixels log Nk) on a log-log plot, fractal dimension D can be estimated by
with values larger than the threshold are assigned to be equal to linear least squares as minus the slope of the regression straight line
unity. At the end of a number of iteration, the binarization process over a suitable range of rk.
leads to detect the ideally one pixel wide edge of the crack path, In the present work, the box size is parameterized as rk = kd
identified by the elements equal to 0 in the data matrix obtained where k = 1, 2, 4, . . . , 2n is a multiplying factor given in geometric
from the image matrix (Fig. 2). progression of ratio 2 and d is the size of a pixel point. In Fig. 3,

Fig. 2. Example of crack path detection in a binary image and the corresponding data matrix.

Fig. 3. Example of application of the box counting method on a binary matrix, three subsequent iterations: (a) k = 2, Nk = 14; (b) k = 4, Nk = 7 and (c) k = 8, Nk = 4.
136 L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141

of cementitious composite with the 0.8% addition of pyrolyzed


hazelnut shells (specimen ID: PY-HS_0.8% – #2). Comparing the
plots, it is apparent that the addition of pyrolyzed micro-
aggregates improves the mechanical behaviour of the cementitious
composite by significantly increasing both its flexural strength and
its ductility with respect to the plain cement paste. The differences
in the post-cracking behaviour are particularly remarkable: while
the plain cement paste undergoes brittle fracture, the cementitious
composite with pyrolyzed micro-aggregates shows an ultimate
displacement that is much greater than the value corresponding
to the appearance of the first crack, thanks to a slow crack propa-
gation and to the absorption of a large amount of energy before
incurring in complete fracture. Such an increase in fracture tough-
ness can therefore be quantified by evaluating the fracture energy
GF of the cementitious composites.
In this work, fracture energy GF is determined from the load-
Fig. 4. Load – CMOD curves from the TPB tests for plain cement paste (specimen ID: CMOD curves of notched specimens under TPB test by applying
PLAIN CEM – #1) and cement paste with 0.8% addition of pyrolyzed micro- the method provided by the Japan Concrete Institute Standard
aggregates (specimen ID: PY-HS_0.8% - #2).
JCI-S-001-2003 [31], whose recommendations, represented in
Fig. 5, are satisfied by the geometry of the tested specimens. Due
an example of three subsequent iterations of box counting is to the unconventional dimensions with which the tested speci-
shown. mens were manufactured, it is not possible to apply either the
standard RILEM TC-50 [32], to determine the fracture energy GF,
or the standard RILEM TC-89 [33], to determine the critical stress
3. Results and discussion intensity factor KSIc and the critical crack tip opening displacement
CTODc. According to the adopted method, it is
3.1. Fracture energy
0:75W 0 þ W 1
GF ¼ ð2Þ
In Fig. 4, a comparison between the load-CMOD curves obtained Alig
from the TPB tests for the cement paste without and with the pyr-
olyzed micro-aggregates after a curing time of 7 days is shown: the where GF is the fracture energy; Alig is the area subjected to rupture
thick line refers to the specimen of plain cement paste (specimen above the notch, referred to as the ‘‘ligament”; W0 is the area below
ID: PLAIN CEM – #1), while the thin line refers to the specimen the load – CMOD curve up to the rupture of the specimen; W1 is the

Fig. 5. Recommendations on the geometry of the notched specimens in JCI-S-001-2003 [31].

Table 3
Determination of fracture energy GF in accordance with standard JCI-S-001-2003 [31], specimens after 7 curing days.

Specimen ID JCI-S-001-2003
Mixture # W0 (Nmm) 0.75 W0 (Nmm) CMODc (mm) W1 (Nmm) GF (N/mm) GF mean value
PLAIN CEM 1 1.38 1.03 0.03 1.26 0.008 0.016
PLAIN CEM 2 1.44 1.08 0.04 2.03 0.011
PLAIN CEM 3 2.55 1.91 0.06 3.15 0.018
PLAIN CEM 4 3.96 2.97 0.09 4.69 0.027
PY-HS_0.5% 1 4.45 3.34 0.10 5.15 0.030 0.030
PY-HS_0.5% 2 4.14 3.11 0.10 5.16 0.029
PY-HS_0.5% 3 4.34 3.26 0.10 5.03 0.029
PY-HS_0.5% 4 4.14 3.11 0.11 5.26 0.029
PY-HS_0.8% 1 5.00 3.75 0.10 5.17 0.031 0.032
PY-HS_0.8% 2 5.03 3.78 0.11 5.24 0.032
PY-HS_0.8% 3 4.97 3.72 0.11 5.34 0.032
PY-HS_0.8% 4 4.97 3.73 0.10 4.88 0.030
PY-HS_1% 1 3.05 2.29 0.06 2.76 0.018 0.022
PY-HS_1% 2 3.04 2.28 0.07 3.65 0.021
PY-HS_1% 3 3.84 2.88 0.08 3.86 0.024
PY-HS_1% 4 3.65 2.74 0.08 3.74 0.023
L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141 137

work done by the deadweight of specimen and loading, evaluated in which l is the loading span, L is the total length of the specimen,
as m1 is the mass of the notched specimen, m2 is the mass of the load-
  ing arrangement part not attached to testing machine but placed on
l
W 1 ¼ 0:75 m1 þ 2m2 g  CMOCc ð3Þ the specimen, g is the acceleration due to gravity and CMODc is the
L
crack mouth opening displacement at rupture.

Table 4
Determination of fracture energy GF in accordance with standard JCI-S-001-2003 [31], specimens after 28 curing days.

SPECIMEN ID JCI-S-001-2003
Mixture # W0 (Nmm) 0.75 W0 (Nmm) CMODc (mm) W1 (Nmm) GF (N/mm) GF mean value
PLAIN CEM 5 2.83 2.12 0.05 2.48 0.016 0.018
PLAIN CEM 6 3.39 2.54 0.06 3.05 0.020
PLAIN CEM 7 2.72 2.04 0.08 3.98 0.022
PLAIN CEM 8 1.23 0.92 0.06 3.05 0.014
PY-HS_0.5% 5 4.69 3.52 0.09 4.27 0.027 0.031
PY-HS_0.5% 6 4.07 3.05 0.08 4.08 0.025
PY-HS_0.5% 7 9.04 6.78 0.11 5.31 0.043
PY-HS_0.5% 8 5.35 4.01 0.08 4.13 0.029
PY-HS_0.8% 5 5.46 4.09 0.05 2.66 0.024 0.033
PY-HS_0.8% 6 5.91 4.43 0.15 7.45 0.042
PY-HS_0.8% 7 5.94 4.46 0.10 5.14 0.034
PY-HS_0.8% 8 6.16 4.62 0.07 3.71 0.029
PY-HS_1% 5 3.54 2.66 0.11 5.62 0.029 0.029
PY-HS_1% 6 3.95 2.96 0.11 5.39 0.029
PY-HS_1% 7 3.92 2.94 0.10 5.11 0.028
PY-HS_1% 8 3.76 2.82 0.11 5.29 0.028

Fig. 6. Mean values of fracture energy GF evaluated from TPB tests, 7 days cured specimens.

Fig. 7. Mean values of fracture energy GF evaluated from TPB tests, 28 days cured specimens.
138 L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141

Results from the TPB tests reported in Tables 3 and 4 show an 3.2. Toughening micromechanisms and fractal geometry of the crack
increase of GF, with respect to the plain cement paste, for all the paths
percentages of pyrolyzed micro-aggregates added to the cementi-
tious composite, both after 7 and 28 curing days. In Figs. 6 and 7, The increase in fracture toughness and fracture energy due to
bar plots show the mean values of GF, calculated as average of four the pyrolyzed micro-aggregates can be explained by examining
specimens according to JCI-S-001-2003. It can be noticed that the the fractal characteristics of crack paths and fracture surfaces
0.8% addition improves the most the fracture toughness of the [10,17].
cementitious composites, with an increase, compared to plain Figs. 8 and 9 depict the crack paths and fracture surfaces across
cement paste, of 69% and 75% in 7 and 28 curing days, respectively. the specimens of plain cement paste (PLAIN CEM – #1) and of
Since the difference between the results after 7 and 28 curing days cementitious composite with 0.8% addition of pyrolyzed hazelnut
is not significant, the pyrolyzed micro-aggregates are proved to be shells (PY-HS_0.8% – #2), respectively. It is apparent that the crack
immediately able to confer a better mechanical behaviour to the in plain cement paste follows a linear path, as typical in brittle frac-
cementitious composites. ture, while the crack in cementitious composite progresses with a

Fig. 8. Plain cement paste, specimen ID: PLAIN CEM – #1. (a) Crack path and (b) fracture surface [24].

Fig. 9. Cementitious composite with 0.8% addition of pyrolyzed hazelnut shells, specimen ID: PY-HS_0.8% – #2. (a) Crack path and (b) fracture surface [24].

Fig. 10. SEM image of the crack path across the cementitious composite with 0.8% addition of pyrolyzed hazelnut shells, specimen ID: PY-HS_0.8% – #2.
L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141 139

more articulated and tortuous path. By examining by SEM the


paths at the microstructure level, it can be seen that the particles
of pyrolyzed hazelnut shells behave as attractors of fracture and
bifurcations (Fig. 10) and are responsible for toughening and
strengthening mechanisms [34,35]. In particular, the mechanism
known as crack-front spinning is observed (Fig. 11): the crack does
not possess enough energy to penetrate the high-strength carbon-
based particles, hence it tends to surround them, resulting in a
number of secondary crack paths.
SEM images of the crack paths were later treated by image pro-
cessing, in order to detect the crack edge and analyze its fractal
geometry in accordance with the methodology defined in Sec-
tion 2.3. As illustrated in Figs. 12 and 13, the linear least-squares
regression of the box counting data leads to values of the coeffi-
cient of determination R2 close to 1 for both the plain cement paste
(R2 = 0.9975) and the cementitious composite with 0.8% addition of
pyrolyzed hazelnut shells (R2 = 0.9959), proving a very good fit of
data points by linear regression and, hence, a distinctive fractal
Fig. 11. Crack-front pinning as a toughening micromechanism in the cementitious geometry of the crack paths. The values obtained for the fractal
composite with the 0.8% addition of pyrolyzed hazelnut shells, specimen ID: PY- dimension D are 1.055 for the plain cement paste and 1.234 for
HS_0.8% – #2.
the cementitious composite with pyrolyzed hazelnut shells. Since

(a) (b)

(c) (d)

Fig. 12. Image processing and box counting method for plain cement paste (specimen ID: PLAIN CEM – #1). (a) SEM image, (b) binary image, (c) edge detection of the crack
path and (d) box counting results and linear least-squares regression.
140 L. Restuccia et al. / Theoretical and Applied Fracture Mechanics 90 (2017) 133–141

(a) (b)

(c) (d)

Fig. 13. Image processing and box counting method for the cementitious composite with the 0.8% addition of pyrolyzed hazelnut shells (specimen ID: PY-HS_0.8% – #2). (a)
SEM image, (b) binary image, (c) edge detection of the crack path and (d) box counting results and linear least-squares regression.

the fractal dimension is a measure of the complexity of an object sion of the crack path showed an increment consistent with the
across different scales, the morphology and irregularity of a crack fracture energy, indicating an increment in tortuosity and, there-
path determine its fractal dimension: the crack path following a fore, an increment of the fracture surface. The presence of the
more linear pattern, in the plain cement paste, has indeed a fractal micro-aggregates, characterized by high strength and stiffness
dimension closer to 1, or the dimension of a straight line, while the due to their significant carbon content, forced the crack path to
more irregular and tortuous crack path, in the cementitious com- deviate its trajectory and surround them. Even if the quantity of
posite with pyrolyzed micro-aggregates, shows a higher fractal these micro-aggregates was very small, the specific surface area
dimension. The fractal dimension of the crack path is therefore was impressive, due to their micro-dimension, and the increase
related to the fracture toughness of the material: with increasing of fracture energy was significant.
fractal dimension, the crack consumes more energy to propagate
along a more complicated pattern, thus resulting in boosting up
the fracture toughness. References

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