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materials

Article
Characteristics of Lightweight Cellular Concrete and
Effects on Mechanical Properties
Wei Yu 1,2, *, Xu Liang 3 , Frank Mi-Way Ni 2, *, Abimbola Grace Oyeyi 2 and Susan Tighe 2
1 College of Traffic and Transportation, Chongqing Jiaotong University, Chongqing 400074, China
2 Department of Civil & Environmental Engineering, University of Waterloo, Waterloo, ON N2L 3G1, Canada;
a2olaleye@uwaterloo.ca (A.G.O.); sltighe@uwaterloo.ca (S.T.)
3 College of Architecture and Civil Engineering, Shangqiu Normal University, Shangqiu 476000, China;
jesselx1230@gmail.com
* Correspondence: changda.yuwei@gmail.com (W.Y.); fmni@uwaterloo.ca (F.M.-W.N.);
Tel.: +1-(226)-899-6429 (W.Y.)

Received: 20 May 2020; Accepted: 9 June 2020; Published: 12 June 2020 

Abstract: This study investigated the pore structure and its effects on mechanical properties of
lightweight cellular concrete (LCC) in order to understand more and detailed characteristics of
such structure. As part of investigation, environment scanning electron microscopes (ESEM) and
industrial high-definition (HD) macro photography camera were separately used to capture and
compare images of specimens. Physical properties of the pore structure, including pore area, size,
perimeter, fit ellipse, and shape descriptors, were studied based on the image processing technology
and software applications. Specimens with three different densities (400, 475, and 600 kg/m3 ) were
prepared in the laboratory. Firstly, the effects of density on the characteristics of pore structure were
investigated; furthermore, mechanical properties (compressive strength, modulus of elasticity and
Poisson’s ratio, flexural strength and splitting tensile strength of LCC) were tested. The relationships
among pore characteristics, density, and mechanical properties were analyzed. Based on the results
obtained from the lab test—comparisons made between specimens with high-densities and those
with low-densities—it was found significant variability in bubble size, thickness, and irregularity of
pores. Furthermore, the increase of density is accompanied by better mechanical properties, and the
main influencing factors are the thickness of the solid part and the shape of the bubble. The thicker of
solid part and more regular pores of LCC has, the better mechanical properties are.

Keywords: lightweight cellular concrete (LCC), pore structure; image processing; shape descriptors;
mechanical properties

1. Introduction
Lightweight cellular concrete (LCC) is a porous material with a typical density ranging from 300
to 1800 kg/m3 [1–6], which contains a homogeneous air bubble structure in the mix. Other academic
terms describing this material are foam concrete [7], low-density foam concrete, or cellular lightweight
concrete, etc. [8,9]. It was first patented in 1923 [10] as a void filler material. The textural surface and
microstructural cells make it widely used in the fields thermal insulation [11], sound absorbance [12],
and fire resistance [13]. It is also used for bridge abutment filling [14], building foundations [15,16],
and airport buffer systems [17]. Over the past 30 years, LCC has been widely used for bulk filling [4],
ditch repair, retaining walls [18], bridge abutment backfill [19], slab structures of concrete floors [20],
and housing insulation [21]. Nowadays, the LCC has been quickly promoted as civil engineering
construction materials with high flowability, low cement content, and high thermal insulation [13,22].

Materials 2020, 13, 2678; doi:10.3390/ma13122678 www.mdpi.com/journal/materials


Materials 2020, 13, 2678 2 of 17

Lightweight cellular concrete has been commonly used in construction applications in different
countries such as Germany, USA, Brazil, UK, and Canada [23]. Though there are limited studies
regarding the practical applications of LCC in civil engineering, several road construction projects
have been done with LCC due to its benefits as mentioned above. For example, LCC has been used as
a subbase material in an industrial zone in the UK to replace the original layer, which consists of peat.
Illinois also applies LCC in the road construction to provide a solution to the soft organic underlying
soil, and it benefits the contractor by lowering unit cost, reduced construction time, and higher quality
of material [19]. Applications of LCC are also found in Canada, and it was used as a subbase material
of bus-lane rural road and highway [24].
LCC’s properties for application in civil engineering have been deeply studied. A critical task in
LCC production is to control the nature, size, and distribution of pores, because the pore characteristic
is the key factor to determine the density and strength of LCC [7,21,23,25]. Over the past few years,
many studies have been done to improve LCC’s nature and its usage in structural applications [9,26–30].
These studies focus on the relationship between the microstructure and mechanical properties of LCC.
Most studies analyzed the relationship of microstructure with compressive strength and modulus of
elasticity, which are essential factors for the application of LCC in infrastructure construction. These
pores of LCC are composed of interlayer pores/spaces, gel pores, capillary pores, and air voids, with pore
sizes varying from nanoscale scale to millimeter scale [31]. Nguyen et al. [32] studied the influences of
pore-structure and mortar properties on the behavior of geopolymer foamed concrete. Results showed
that the pore-size has a profound effect on the material’s fracture resistance. Batool et al. [33] studied the
distribution features of pore size in cement-based LCC. The results showed that the narrower the pore
distribution is, the greater the conductivity and the smaller the density is. The investigation indicated
that LCC strength decreases with the voids increase [34,35]. The prediction models on compressive
strength were also investigated by some researchers. These findings are mainly based on the artificial
neural network [36], extreme learning machine, and regression analysis based empirical models [37].
Kearsley and Wainwright [28] examined the relationship between porosity and compressive strength.
They presented the mathematical models to reflect the influence of porosity on the compressive strength
of the material. Wee et al. [38] proposed a spacing factor parameter to characterize the air-void system
in concrete. It can be directly related to the average air void size. Results showed that the decrease of
spacing factor and increase of the average air-void size resulted in the reduction of the compressive
strength. Besides, Nambiar and Ramamurthy [5], along with Hilal et al. [1], examined the pore structure
inside LCC and demonstrated that porosity was not sufficient to regulate the characteristics of LCC.
Other pore characteristics—such as pore size, size distribution, shape, and cell thickness—should also
be considered for a more detailed understanding of LCC material.
Though LCC has been applied in road construction, there are still lacking a complete and thorough
guide of LCC. Mechanical properties of LCC at a specific low density (400 to 600 kg/m3 ) need to be
adequately examined. The relationship between the microstructure and the mechanical properties of
LCC also needs further analysis.
In order to obtain the microstructure of LCC, electron microscopes (EM)—such as secondary
electron (SE) and X-ray computed tomography (CT X-ray)—were widely employed [1,39–43]. SE can
be used to capture images with surface details, and CT X-ray can be used to view the three-dimensional
external shape of specimens. The biggest advantage of EM is that they have higher resolution and
higher magnification (up to 2 million times). While they have a range of disadvantages as well:
they are costly; sample preparation is often much more elaborate; the space requirements are high,
and operators require more training and experience. All these negatives mentioned above limit their
flexibility in use. Compared with EM, although optical microscope (OM) has a significantly lower
resolution, it is cheap to purchase, easy to operate small to carry. Some researchers have used a camera
connected to an optical microscope to capture images of foamed concrete mixes and identified air-voids
with diameters over 20 µm [1,40]. It means that OM can be used to capture the microstructure of LCC.
Materials 2020, 13, 2678 3 of 17

In this study, the correlation between pore characteristics and mechanical properties of LCC was
investigated using both image processing technology and experimental approaches. The effects of
local pore characteristics on the physical properties were examined from LCC samples with different
densities at a microstructure level. For that purpose, a set of LCC samples with low densities were
produced by using the Provoton foaming agent. In general, pores in LCC are secured by using either
the pre-foaming or mix foaming methods [1,4]; the LCC specimens used in this study were generated
using the pre-foaming method.
The pore characteristics, including pore distributions of LCC samples, were described using
environmental scanning electron microscope (ESEM), which was used to capture clear images. Machine
learning was used to identify pores, and then watershed segmentation method [44] was used to segment
and identify the pores with irregular shapes. Finally, pore characteristics (area, size, and shape) were
obtained. In order to capture the pore structure conveniently and fast, an industrial HD camera system
(IHDCS) was developed, which was used to replace ESEM to obtain image samples of pore-structure
in this study.
Mechanical properties of LCC with different densities—including compressive strength, modulus
of elasticity, flexural strength, and splitting tensile strength—were tested. Then, the relationship
between mechanical properties and pore characteristics (i.e., pore area, size distribution, and shape)
was investigated.

2. Preparation of LCC Specimens and Mechanical Test

2.1. LCC Specimens


LCC materials with different densities are prepared to investigate the effect of the pore
characteristics on the mechanical properties. CEMATRIX Inc. Canada (Calgary, Alberta, Canada)
provided all test LCC specimens, which were with different densities. The densities of specimens used
in this research are 400 kg/m3 , 475 kg/m3 , and 600 kg/m3 , and each specimen is denoted as D400, D475,
and D600, respectively. Foamed specimens are generated by the pre-foaming method, by which the
pre-foamed foams are added into a base cement slurry mix until it achieved target density. The base
mixes were composed by mixing general use Portland cement, Grade 80 NewCem slag [45], and water.
The composition is 80% cement to 20% slag by mass, and the water to binder ratio is 0.5. The density
of the base mix is 1823 kg/m3 .
Figure 1 shows the LCC samples with different densities. There are two types of samples used
in the study, cylindrical and beam samples. Here, these samples, which are used to measure the
pore structure characteristics, are obtained by slicing beam samples. Firstly, an Industrial HD camera
module connected to a computer was used to capture specimens’ images, and then the characteristics
of pore were studied, such as number, area, perimeter, and shape descriptors (circularity, aspect ratio,
roundness, and solidity). After that, all of specimens were cut into 10-mm cubes for scanning electron
microscope imaging for high-resolution ESEM images with optimized sample size. Images captured
by ESEM, which is a FEI Quanta 250 FEG at the Watlab of the University of Waterloo were also used to
study the characteristics of pore. The results of ESEM images were compared with that of Industrial
HD Camera images.
Materials 2020, 13, 2678 4 of 17
Materials 2020, 13, x FOR PEER REVIEW 4 of 17

D400 D475 D600

Figure
Figure 1.
1. Lightweight
Lightweight cellular
cellular concrete
concrete specimens
specimens with
with different
different densities.
densities.

2.2. Mechanical
Mechanical Properties
Properties Test
Test Method of LCC
LCC is
LCC is aa relatively
relatively newnew material,
material, andandcurrently,
currently, there
thereareareno notest
test standards
standards forfor itit in
in Canada.
Canada.
Most ofof the
thelaboratory
laboratoryteststestswere
wereperformed
performed in accordance
in accordance withwith
standard procedures
standard stated stated
procedures in ASTM in
or AASHTO
ASTM standards.
or AASHTO In the absence
standards. of standard
In the absence testing protocols
of standard for LCC,for
testing protocols testLCC,
methods that had
test methods
been had
that devised
beenfordevised
other materials,
for otherwhich are similar
materials, which to LCC in various
are similar contexts,
to LCC were adopted
in various contexts, based on
were
best practice
adopted based or expert
on bestopinion.
practiceInor this study,opinion.
expert compressive stress,
In this study, modulus of elasticity
compressive stress,and Poisson’s
modulus of
ratio, flexural
elasticity and strength,
Poisson’sand splitting
ratio, flexural tensile strength
strength, and of LCC were
splitting tested
tensile in the of
strength University
LCC were of tested
Waterlooin
Center for Pavement and Transportation Technology (CPATT) lab using
the University of Waterloo Center for Pavement and Transportation Technology (CPATT) lab usingthe Materials Testing System.
Samples
the were cured
Materials TestingforSystem.
28 days before
Samples testing
wereincured
the humidity
for 28 dayschamber of University
before testing inofthe Waterloo.
humidity
Compressive strength
chamber of University of Waterloo. was measured on four Φ 75 mm × 150 mm (Diameter × Height) cylindrical
specimens stated instrength
Compressive ASTM Standard C495/C495M-
was measured on fourStandard
Φ 75 Test
mmMethod× 150 formm Compressive
(Diameter Strength× Height)of
Lightweightspecimens
cylindrical Insulating Concrete
stated in [46]ASTM
per each density. C495/C495M- Standard Test Method for
Standard
ModulusStrength
Compressive of elasticity and Poisson’s
of Lightweight ratio were
Insulating measured
Concrete [46] perin accordance
each density. with ASTM Standard
C469/C469M—Standard
Modulus of elasticity Test Method
and for Static
Poisson’s ratio Modulus of Elasticity
were measured and Poisson’s
in accordance with Ratio
ASTM of Standard
Concrete
in Compression [47]. TheTest
C469/C469M—Standard standard
Method samplefor size
Staticis Φ 150 mm of
Modulus × 300 mm. A and
Elasticity total Poisson’s
of three specimens
Ratio of
were tested per each density.
Concrete in Compression [47]. The standard sample size is Φ 150 mm × 300 mm. A total of three
Flexural
specimens werestrength
tested was testeddensity.
per each using simple beams with third-point loading, and the use standard
was ASTM C78/C78M [48]. The samples
Flexural strength was tested using simple measured beams mm ×third-point
100 with 100 mm × loading,
400 mm, andwiththe
three
usespecimens
standard
per each
was ASTM density.
C78/C78M [48]. The samples measured 100 mm × 100 mm × 400 mm, with three
Splitting
specimens per tensile strength of LCC was also tested as the standard of ASTM C496/C496M [49].
each density.
FourSplitting
samplestensile
per each
strengthdensity
of LCC were
was used, and as
also tested thethedimension
standard ofofASTM cylindrical
C496/C496Msamples is
[49].
Φ 150samples
Four mm × 300 permm.
each density were used, and the dimension of cylindrical samples is Φ 150 mm ×
Figure 2 shows the experimental test set-ups of LCC.
300 mm.
Figure 2 shows the experimental test set-ups of LCC.
Materials 2020, 13, 2678 5 of 17

Materials 2020, 13, x FOR PEER REVIEW 5 of 17

(a) (b)

(c) (d)
Figure
Figure 2. 2. Experimental
Experimental test
test set-ups
set-ups of of LCC.
LCC. (a)
(a) Compressive
Compressive strength
strength test.
test. (b)
(b) Modulus
Modulus of
of elasticity
elasticity
test.
test. (c)
(c)Modulus
Modulusofofrupture
rupture test.
test. (d)
(d)Splitting
Splittingtensile
tensiletest.
test.

3. Image
3. ImageCapturing
Capturing System
System and
and Image
Image Processing
Processing Methodology
Methodology

3.1. Industrial HD Camera System (IHDCS)


3.1. Industrial HD Camera System (IHDCS)
Scanning electron microscopy is appropriate for the pore structure and microstructure analysis
Scanning electron microscopy is appropriate for the pore structure and microstructure analysis
of the foam concrete [50]. It can obtain clear photos of pores, and it is helpful to analyze the pore
of the foam concrete [50]. It can obtain clear photos of pores, and it is helpful to analyze the pore
characteristics. Most ESEMs are able to scan image materials from 1 cm to 5 microns in width; however,
characteristics. Most ESEMs are able to scan image materials from 1 cm to 5 microns in width;
sometimes, it is not big enough. Thanks to the development of technology, macro photography cameras
however, sometimes, it is not big enough. Thanks to the development of technology, macro
are an attractive solution when compared to traditional large ESEMs typically found in university
photography cameras are an attractive solution when compared to traditional large ESEMs typically
microscopy centers. In this study, an Industrial HD Camera System (IHDCS) was developed to capture
found in university microscopy centers. In this study, an Industrial HD Camera System (IHDCS)
the pore structure conveniently and fast. The system consists of capturing module (industrial HD
was developed to capture the pore structure conveniently and fast. The system consists of capturing
macro photography camera module), illumination part (LED light), transmission part (connection
module (industrial HD macro photography camera module), illumination part (LED light),
cables) and control component (Laptop). The capturing module and illumination part are fixed on
transmission part (connection cables) and control component (Laptop). The capturing module and
the top of a cylinder frame and connected with a laptop with cables. The HD macro photography
illumination part are fixed on the top of a cylinder frame and connected with a laptop with cables.
camera module, ZJHY-179-R-01 AF, is produced by Ceyuan Inc. China, and its parameters are shown
The HD macro photography camera module, ZJHY-179-R-01 AF, is produced by Ceyuan Inc. China,
in Table 1. Figures 3 and 4 separately show the capturing system and the captured images.
and its parameters are shown in Table 1. Figures 3 and 4 separately show the capturing system and
the captured images.

Table 1. Parameters of Industrial HD camera module

Parameter and
Name Parameter and Description Name
Description
Module Size 38 mm × 38 mm × 6 mm Sensitivity TBD
Focus AF F/NO 2.5
Object Distance 5 cm-infinity EFL 4.16 mm
Materials 2020, 13, 2678 6 of 17

Table 1. Parameters of Industrial HD camera module.

Parameter and Parameter and


Name Name
Description Description
Module Size 38 mm × 38 mm × 6 mm Sensitivity TBD
Materials 2020, 13,Focus
x FOR PEER REVIEW AF F/NO 2.5 6 of 17
Object Distance 5 cm-infinity EFL 4.16 mm
Materials 2020, 13, x FOR PEER REVIEW
Power 6 of 17
Power USBbus
USB buspower
power BFL BFL 3.4 mm3.4 mm
Sensor Type IMX179 FOV ◦
80 80°
Sensor Type IMX179 FOV
PowerArray Size USB 3264
bus power BFL 3.4 mm
<1.2%
Active Active
Array
Sensor TypeSize 3264 ××2448
IMX179
2448 TVTVdistortion
distortion <1.2%
Pixel Size 1.4 µm × 1.4 µm IRFOV
filter 650 ±80°
10 nm
Pixel
Active SizeSize
Array 1.4 μm××2448
3264 1.4 μm IR filter
TV distortion <1.2%± 10 nm
650
15 fps 3264 × 2448, 2592 × 1944
Maximum Pixel Image
Size 15 fps 32641.4×μm2448,
× 2592
1.4 μm××1944 Fixed IR
pattern
filter noise <0.03%
650 ± 10 nm
Maximum Image 30 fps 1920 × 1080, 1280 720 Fixed pattern noise <0.03%
30 fps
15 fps 1920××2448,
3264 1080, 1280× ×
2592 720
1944
Maximum Image Fixed pattern noise <0.03%
30 fps 1920 × 1080, 1280 × 720

Figure
Figure
Figure 3.Industrial
3.3. IndustrialHD
Industrial HDmacro
HD macrophotography
macro photography
photography image
image
image capturing
capturing
capturing system.
system.
system.

D400 D475 D600


D400 D475 D600
Figure 4. Images of specimens captured
Figure 4. Images of specimens capturedby
byIHDCS.
IHDCS.
Figure 4. Images of specimens captured by IHDCS.
Figure
Figure 4 shows
4 shows thethe pore
pore imagesofofsamples,
images samples,captured
capturedbybyIHDCS,
IHDCS,with
withdifferent
differentdensities.
densities. ItIt can
can be
be Figure 4 shows
observed that, the pore
relative to images
the of samples,
high-density captured(D600),
specimens by IHDCS,
the with different
bubble size of densities.
low-density It can
observed that, relative to the high-density specimens (D600), the bubble size of low-density specimens
be observed(D400
specimens that, and
relative
D475)to have
the high-density
greater specimens
variability. (D600),
Mostly, the bubble
large-size bubbles size
are of low-density
formed by
(D400 and D475) have greater variability. Mostly, large-size bubbles are formed by merging adjacent
specimens
merging (D400 small-size
adjacent and D475) have greater variability. Mostly, large-size bubbles are formed by
bubbles.
small-size bubbles.
merging adjacent small-size bubbles.
3.2. ESEM Imaging Method
3.2. ESEM Imaging Method
In this study, for a more detailed examination of the pore characteristics of samples,
environment scanning
In this study, forelectron
a moremicroscope
detailed (ESEM) imagesof
examination arethe
utilized
pore tocharacteristics
examine the pore sizes
of samples,
and distributions
environment of the electron
scanning LCC. Themicroscope
specimens are 1 cm cubes.
(ESEM) imagesFigure 5 showsto
are utilized theexamine
secondary
theelectron
pore sizes
images
and of the LCCofspecimens
distributions the LCC. performed by ESEM.
The specimens are 1 In
cmthese images,
cubes. numerous
Figure 5 showsspherical pores with
the secondary electron
images of the LCC specimens performed by ESEM. In these images, numerous spherical poresinwith
different sizes in each specimen are identified. Compared to Figure 4, bubbles have sharper edges
Materials 2020, 13, 2678 7 of 17

3.2. ESEM Imaging Method


In this study, for a more detailed examination of the pore characteristics of samples, environment
scanning electron microscope (ESEM) images are utilized to examine the pore sizes and distributions
of the LCC. The specimens are 1 cm cubes. Figure 5 shows the secondary electron images of the LCC
specimens performed by ESEM. In these images, numerous spherical pores with different sizes in
each specimen are identified. Compared to Figure 4, bubbles have sharper edges in the ESEM image.
Materials 2020, 13, x FOR PEER REVIEW 7 of 17
Similar to IHDCSs results, Pore sizes of specimens D400 and D475 are more variable compared with
D600. Particularly, lots of bubbles in D400 connected to form irregular bubbles. Besides, the thickness
compared with D600. Particularly, lots of bubbles in D400 connected to form irregular bubbles.
between pores of D600 is obviously larger than that of D400 and D475.
Besides, the thickness between pores of D600 is obviously larger than that of D400 and D475.

D400 D475 D600

Figure 5. ESEM images with different


Figure 5. different densities.
densities.

3.3. Image Processing Methodology


3.3. Image Processing Methodology
FiJi ImageJ [51] software was used for the image processing of photographed LCC. FiJi is an image
FiJi ImageJ [51] software was used for the image processing of photographed LCC. FiJi is an
processing package, and it bundles a lot of plugins that facilitate scientific image analysis. In this
image processing package, and it bundles a lot of plugins that facilitate scientific image analysis. In
study, the Trainable Weka Segmentation (TWS) plugin was used to segment the pores structure of LCC.
this study, the Trainable Weka Segmentation (TWS) plugin was used to segment the pores structure
TWS is an open-source project and combines a collection of machine learning algorithms with a set of
of LCC. TWS is an open-source project and combines a collection of machine learning algorithms
selected image features to produce pixel-based segmentations. Firstly, the pores and solid area of the
with a set of selected image features to produce pixel-based segmentations. Firstly, the pores and
LCC sample were selected separately, which were used to training and got a suitable classifier. Once
solid area of the LCC sample were selected separately, which were used to training and got a
the classifier was obtained, it was used to classify the pore and solid area and got the TWS segmentation
suitable classifier. Once the classifier was obtained, it was used to classify the pore and solid area
result, which is an 8-bit color image. Then, a threshold value was selected based on Otsu method [52]
and got the TWS segmentation result, which is an 8-bit color image. Then, a threshold value was
to transform the image into a binary image. In the binary image, black parts represent the voids or
selected based on Otsu method [52] to transform the image into a binary image. In the binary image,
pores, and the white parts represent the solid part. In addition, watershed segmentation method was
black parts represent the voids or pores, and the white parts represent the solid part. In addition,
used to enhance the image segmentation quality. In this way, the contacting pores could be successfully
watershed segmentation method was used to enhance the image segmentation quality. In this way,
segmented. The composite image of the original and watershed segmentation result was used to
the contacting pores could be successfully segmented. The composite image of the original and
verify the effect of segmentation (more detailed information can be found in Figure 6). The watershed
watershed segmentation result was used to verify the effect of segmentation (more detailed
segmentation result was used to obtain the feature data of pore for the subsequent analysis.
information can be found in Figure 6). The watershed segmentation result was used to obtain the
feature data of pore for the subsequent analysis.
black parts represent the voids or pores, and the white parts represent the solid part. In addition,
watershed segmentation method was used to enhance the image segmentation quality. In this way,
the contacting pores could be successfully segmented. The composite image of the original and
watershed segmentation result was used to verify the effect of segmentation (more detailed
information
Materials can
2020, 13, 2678be found in Figure 6). The watershed segmentation result was used to obtain
8 ofthe
17
feature data of pore for the subsequent analysis.

Figure6.6. Image
Figure Image processing
processingprocedure.
procedure.

4.
4. Results
Results
Materials
and
2020,and
Analysis
13, xAnalysis
FOR PEER REVIEW 8 of 17

4.1. ESEM Pore Characteristic Analysis


4.1. ESEM Pore Characteristic Analysis
Based on ImageJ software, parameters of the pore are easily obtained, such as area, perimeter,
Based on ImageJ software, parameters of the pore are easily obtained, such as area, perimeter,
primary axis, and secondary axis of the best fitting ellipse and shape descriptors (circularity, roundness,
primary axis, and secondary axis of the best fitting ellipse and shape descriptors (circularity,
and solidity). Firstly, the strength of the relationship between every two parameters was calculated,
roundness, and solidity). Firstly, the strength of the relationship between every two parameters was
and the results are shown in Figure 7.
calculated, and the results are shown in Figure 7.

Figure 7. Heat map of correlation coefficient result.

The heat map


The heat mapisishelpful
helpfulfor
forshowing
showing variance
variance across
across multiple
multiple variables,
variables, displaying
displaying whether
whether any
any
variables are similar to each other, and for detecting if any correlations exist in-between them.them.
variables are similar to each other, and for detecting if any correlations exist in-between The
The number
number on each
on each cell cell shows
shows the the correlation
correlation coefficient
coefficient of each
of each twotwo parameters.
parameters. TheThe value
value range
range is
is from −1.0 to 1.0. If correlation equals to 1.0, it shows a perfect positive relationship.
from −1.0 to 1.0. If correlation equals to 1.0, it shows a perfect positive relationship. If correlationIf correlation
equals to −1.0,
equals to −1.0, it
it also
also means
means aa perfect
perfect negative
negative correlation
correlation ofof two
two parameters.
parameters. NoNo matter
matter perfect
perfect
negative
negative oror positive
positive correlation,
correlation, they
they all
all show
show thatthat parameters
parameters have
have aa strong
strong correlation.
correlation. When
When
correlation equals zero, it means that there is no relationship between the two parameters. In this
study, correlation results were converted into non-negative values, which were used to consider the
correlation among different parameters. Because the results of different specimens have a consistent
trend, Figure 7 shows the result of D475 as an example. In Figure 7, a divergent color gradient
defined by three hues (from blue to white to red) made the low and high ends of the range visually
Materials 2020, 13, 2678 9 of 17

correlation equals zero, it means that there is no relationship between the two parameters. In this
study, correlation results were converted into non-negative values, which were used to consider the
correlation among different parameters. Because the results of different specimens have a consistent
trend, Figure 7 shows the result of D475 as an example. In Figure 7, a divergent color gradient defined
by three hues (from blue to white to red) made the low and high ends of the range visually distinct.
Increasing red hues represent stronger correlations between two parameters. In contrast, increasing
blue hues mean weaker correlations. Obviously, parameters of pore area, perimeter, major and minor
axis have a strong correlation between each other. Their lowest correlation coefficient value is 0.88.
It means that the trends of pore area, perimeter, major, and minor axis have highly consistent. It is
appropriate to adopt the pore area’s changing trend to represent those of the other three parameters.
Although the shape descriptors (circularity, roundness, and solidity) have a high correlation between
each other, the maximum of correlation is less than 0.8. Meaning that the changing trend of shape
descriptors has certain differences. It is better to consider the shape descriptors’ changing trend
separately. Therefore, the representative properties—area of pore, circularity, and solidity—were
considered in subsequent analyses.

4.1.1. Pore Size and Thickness of Solid Part


Figure 8 shows the pore size of specimens with different densities. Figure 8a clearly shows that
specimens of D400 and D475 have a similar distribution and which is different from that of D600.
Firstly, the pore numbers of D400 and D475 are more than two times that of D600. The order of pore
Materials 2020, 13, x FOR PEER REVIEW 9 of 17
numbers is D400 > D475 > D600. Although there are more pores in specimen D400 and D475 than that
of D600,
that most most
of D600, of them are small.
of them FigureFigure
are small. 8b presents that more
8b presents thatthan
more70% of pores
than 70% of in pores
D400 and D474and
in D400 are
less than
D474 200 µm,
are less thanwhile
200 μm,the while
percentage of D600 isof
the percentage only about
D600 36%.
is only On the
about other
36%. On hand, there
the other are also
hand, therea
considerable number of pores larger than 200 µm in D400 and D475. Besides, the
are also a considerable number of pores larger than 200 μm in D400 and D475. Besides, the numbernumber is similar to
that
is in D600.
similar Hence,
to that the variance
in D600. of pore
Hence, the size of
variance in D400 andin
pore size D475
D400 is and
higher than
D475 is D600.
higher than D600.

D400 D475 D600


100
Cumulative Frequency (%)

80

60

40

20

0 50 100 150 200 250 300 350 400


Pore Radius (um)
(a) (b)
Figure 8.
8. Box
Boxchart
chart and
and cumulative
cumulative frequency
frequency analysis
analysis of Equivalent
of Equivalent radius. radius. (a) Box
(a) Box chart chart of
of equivalent
equivalent
radius. (b) radius. (b) Cumulative
Cumulative frequency
frequency of of pore radius.
pore radius.

Figure 99 presents
Figure presents the
the average
average thickness
thickness results
results of
of the
the solid
solid part
part in
in specimens.
specimens. In In order
order toto obtain
obtain
the average
the average thickness
thickness of
of the
the solid
solid part,
part, firstly,
firstly, the
the watershed
watershed segmentation
segmentation resultresult binary
binary images
images ofof
specimens were inverted, which were used to calculate the total area of solid parts.
specimens were inverted, which were used to calculate the total area of solid parts. In the inverted In the inverted
binary images,
binary images, the
the white
white areas
areas are
are pores
pores and
and the
the black
black area
area is
is the
the solid
solid part,
part, as
as shown
shown inin Figure
Figure 9a.
9a.
Then, the
Then, the inverted
inverted image
image was
was skeletonized,
skeletonized, shown
shown in in Figure
Figure 9b. The Skeleton
9b. The Skeleton ofof the
the solid
solid part
part can
can be
be
obtained, which was considered to be approximately equal to the length of the solid
obtained, which was considered to be approximately equal to the length of the solid part. Once the part. Once the
total area
total area and
and length
length of
of the
the solid
solid part
part were
were obtained,
obtained, the
the average thickness was
average thickness was calculated,
calculated, and
and the
the
results are
results are shown
shown in in Figure
Figure 9c.
9c.
Materials 2020, 13, 2678 10 of 17
Materials 2020, 13, x FOR PEER REVIEW 10 of 17

(a) (b)

(c)

Figure
Figure9.9.Average
Averagethicknesses
thicknessesofofsolid parts.(a)
solidparts. (a)Inverted
Invertedbinary image.(b)
binaryimage. (b)Skeleton
Skeletonofofthe
thesolid
solidpart.
part.
(c)
(c)Average
Averagethickness
thicknessofofsolid
solidparts
partsand
andarea
arearatio
ratioasasaafunction
functionof
ofspecimen
specimendensity.
density.

AsAscancanbebeseen
seenfrom
fromFigure
Figure 9c,9c,
thetheaverage
average thickness
thicknesshashas
a positive
a positivecorrelation
correlationwithwith
density. It
density.
means
It meansthat,that,
when the density
when of the
the density of sample
the sampleis low, the average
is low, thickness
the average of theofsolid
thickness part ispart
the solid thinisand
thin
vice
andversa. Relative
vice versa. to higher
Relative density
to higher samples
density samples(D600), the the
(D600), average
averagethickness
thickness of of
thethe
solid
solidpart
partinin
low-density
low-densitysamples
samples (D400,
(D400, D475) is is reduced
reducedby byabout
about40%.
40%.A A small
small thickness
thickness value
value means
means a pore
a big big
pore area. The red curve in Figure 9c shows the trend of area ratio of pores with different
area. The red curve in Figure 9c shows the trend of area ratio of pores with different densities of LCC. densities of
LCC. It is clear
It is clear thatratio
that area area decreases
ratio decreases as density
as density increases.
increases. Areahas
Area ratio ratio has a negative
a negative correlation
correlation with the
with the density
density of sample.of sample.

4.1.2.Shape
4.1.2. ShapeDescriptors
Descriptors
Shapedescriptors
Shape descriptors include
include circularity,
circularity,roundness,
roundness,and andsolidity. Circularity
solidity. Circularityis used to describe
is used how
to describe
how close the pore should be to a true circle, and it is defined as the ratio of the area of the object the
close the pore should be to a true circle, and it is defined as the ratio of the area of the object to to
area
the of aofcircle
area with
a circle withthethe
same
sameperimeter.
perimeter. Roundness
Roundness is similar to circularity,
is similar andand
to circularity, thethe
difference is that
difference is
roundness does not consider the local irregularities. Roundness is defined as the ratio
that roundness does not consider the local irregularities. Roundness is defined as the ratio of the area of the area of an
of an object to the area of a circle with the major axis. Solidity is used to measure the density of pore.is
object to the area of a circle with the major axis. Solidity is used to measure the density of pore. It
Itdefined as the
is defined ratioratio
as the of the
of area of anofobject
the area to thetoarea
an object the of
areaa convex hull of
of a convex theof
hull object. FigureFigure
the object. 10 shows
10
results of shape descriptors with different densities.
shows results of shape descriptors with different densities.
Materials 2020, 13, 2678 11 of 17
Materials 2020, 13, x FOR PEER REVIEW 11 of 17

Figure
Figure 10.
10. Data
Dataof
ofshape
shapedescriptors
descriptorsof
ofspecimens
specimenswith
withdifferent
different densities.
densities.

Each
Each dot
dot in
in Figure
Figure 10 10 represents
represents aa pore.
pore. Comparing
Comparing with with the
the other
other two
two specimens,
specimens, D475 D475 hashas thethe
best
best distribution
distribution of of shape
shape descriptors,
descriptors, which is followed by D600, and the worst is D400.
By
By comparing
comparing circularity
circularity results
results of
of three
three specimens,
specimens, half half the
the pores’
pores’ circularities
circularities of of D475
D475 are are
between
between 0.621
0.621 and
and 0.732,
0.732, whereas
whereas thatthat of
of D400
D400 and
and D600
D600 are
are separately
separately fromfrom 0.438
0.438 toto 0.589
0.589 and
and from
from
0.588
0.588 to
to 0.73.
0.73. High
High circularity
circularity valuevalue means
means thatthat pore
pore is
is more
more close
close toto a true circle. Hence,
Hence, specimen
specimen
D475 has a better foam structure, which is good for its mechanical
D475 has a better foam structure, which is good for its mechanical properties. properties.
The
The results
results ofof roundness
roundness show show aa similar
similar trend
trend with
with that
that of circularity. The The difference
difference is is that
that
roundness values are
roundness values aregenerally
generallyhigherhigherthan
than values
values of circularity,
of circularity, because
because roundness
roundness ignoresignores the
the effect
effect of local irregularities of pore. Hence, circularity contains more shape information
of local irregularities of pore. Hence, circularity contains more shape information of pore, and in this of pore, and
in this study,
study, circularity
circularity is usedistoused to evaluate
evaluate the circletheshape
circleofshape of the pore.
the pore.
Solidity results of specimen D475 and D600
Solidity results of specimen D475 and D600 are obviously are obviously moremoresignificant
significant than thatthat
than of D400.
of D400.As
the pore
As the becomes
pore becomes solid, thethe
solid, pore area
pore and
area andconvex
convex hull
hullarea
areaapproach
approacheach eachother,
other,resulting
resultingin in aa
solidity
solidity value
value ofof one.
one. Thus,
Thus,ititmeans
meansthatthatpores
poresin inD475
D475 and
and D600
D600 areare closer
closer toto the
the true
true circle
circle than
than
that
that of D400. In
of D400. In addition,
addition, larger
largersolidity
solidityvalue
valuealso
alsoindicates
indicatesthat
that there
there areare fewer
fewer touching
touching porespores
in thein
the specimen.
specimen. ThisThis is consistent
is consistent withwith
thethe specimen’s
specimen’s photos
photos shown
shown in in Figure
Figure 5. 5.
InIn this
this study,
study, solidity
solidity is
is mainly used to evaluate the touching
mainly used to evaluate the touching pores. pores.

4.2. Image
4.2. ImageProcessing
Processing Results
Results Analysis
Analysis of
of ESEM
ESEM and
and IHDCS
IHDCS
There are
There are six
six parallel
parallel specimens
specimens of of each
each density,
density, obtained
obtained by by IHDCS,
IHDCS, andand test
test results
results of
of pore
pore
characteristics are
characteristics areshown
showninin Figure 11. 11.
Figure Figure 11a shows
Figure the results
11a shows of areaof
the results ratio andratio
area average
and thickness
average
as functions
thickness of the density
as functions of theof density
LCC. Area ratio of
of LCC. pore
Area andofaverage
ratio pore andthickness
averageofthickness
solid partsofare strongly
solid parts
correlated
are stronglywith the density
correlated withofthe
LCC. The increase
density of LCC. of Thedensity is accompanied
increase of density is by the increaseby
accompanied in the
the
average thickness
increase of the thickness
in the average solid part of
and a decrease
the solid partofand
the area ratio ofofpore.
a decrease It canratio
the area be observed
of pore. that there
It can be
are linear that
observed relationships
there are for arearelationships
linear ratio and average thickness,
for area ratio andwhere areathickness,
average ratio is negatively
where area correlated
ratio is
with density
negatively and average
correlated withthickness
density andis positively correlatediswith
average thickness density.
positively correlated with density.
Materials 2020, 13, 2678 12 of 17
Materials 2020, 13, x FOR PEER REVIEW 12 of 17

(a)

(b)
Figure
Figure 11.
11. Results
Results of
of pore
pore characteristic
characteristicbased
basedon
onIHDC.
IHDC.(a)
(a)Area
Area ratio
ratio and
and average
average thickness
thickness as
as aa
function of specimen density based on IHDCS images. (b) Shape descriptors of specimens with
function of specimen density based on IHDCS images. (b) Shape descriptors of specimens with different
different density
density based on based
IHDCS onimages.
IHDCS images.

Figure 11b
11bshows
showsthetheresults
results
of of circularity
circularity andand solidity.
solidity. Specimen
Specimen D475D475 has
has the theaverage
best best average
results
results of circularity
of circularity and solidity,
and solidity, whichthat
which means means that the
the shape shape in
of pores ofD475
poresisinmore
D475 is more
regular regular
and closer and
to a
closer to a true
true circle. circle. Furthermore,
Furthermore, compared tocompared to the
the other two other two
specimens specimens
with differentwith different
densities, D475densities,
contains
D475 contains
less number less number
of touching of On
pores. touching pores.
the other hand,On thehas
D400 other hand, results
the worst D400 has the worstand
of circularity results of
solidity.
circularity anddue
It means that, solidity.
to theItincrease
means that, due to
in bubble the increase
content, in bubble content,
the inter-bubble spacing the inter-bubble
is reduced, spacing
and adjacent
is reduced,
pores and adjacent
more easily contact pores more As
each other. easily contact
a result, neweach other.pores
irregular As a are
result, new irregular
generated, pores are
which causes the
generated,
circularity which causesto
and solidity the circularity
decrease. In and
ordersolidity to decrease.
to verify In order
the accuracy to image
of the verify the accuracyresults,
processing of the
image
resultsprocessing
of IHDCS are results, resultswith
compared of IHDCS
that of are
ESEM,compared withare
and results thatshown
of ESEM, and results
in Figure 12. are shown
in Figure 12.
Materials 2020, 13, 2678 13 of 17
Materials 2020, 13, x FOR PEER REVIEW 13 of 17

Figure
Figure 12.
12. Comparative
Comparative analysis
analysis of
of physical
physical parameter
parameter results
results between ESEM and IHDCS.

Figure 12 presents the comparison results of ESEM and IHDCS. In general, the results of IHDCS
and ESEM
and ESEM have have similar changes.
changes. In In particular,
particular, the
the absolute
absolute value
value ofof pores’
pores’ area
area ratio
ratio and
and solidity
results of IHDCS and ESEM are very close. Hence, Hence, IHDCS
IHDCS can can be
be used
used to analyze
analyze the bubbles’
bubbles’ area
ratio of LCC
LCC and andthe
thecondition
conditionofoftouching
touchingbubbles,
bubbles,which
whichcancan
obtain a conclusion
obtain a conclusionconsistent withwith
consistent that
of ESEM.
that On the
of ESEM. On other hand,
the other results
hand, of the
results of average distance
the average andand
distance circularity of IHDCS
circularity of IHDCSandandESEMESEMare
different,
are although
different, theythey
although show the same
show variation.
the same Results
variation. of IHDCS
Results of IHDCSare larger thanthan
are larger that that
of ESEM, and
of ESEM,
the deviations
and of average
the deviations distance
of average and circularity
distance are separately
and circularity from 19.65
are separately to 30.58
from 19.65µm to and
30.58from
μm0.126
and
to 0.179.
from 0.126The main The
to 0.179. reasons
mainfor the differences
reasons in resultsinisresults
for the differences that: on the one
is that: hand,
on the onerelative to ESEM,
hand, relative to
IHDCSIHDCS
ESEM, obtainsobtains
lower resolution images,images,
lower resolution and theandedgestheofedges
identified bubbles bubbles
of identified are relatively smooth
are relatively
which lead
smooth whichto higher
lead tovalue
higherofvalue
circularity; on the other
of circularity; on thehand,
otherimages
hand, captured by IHDCS
images captured by have
IHDCS a larger
have
arange than
larger rangethatthan
of ESEM,
that ofand eachand
ESEM, density
each considered six parallel
density considered six samples. It meansIt that
parallel samples. IHDCS
means that
obtained
IHDCS more bubble
obtained more samples than ESEM.
bubble samples thanItESEM.
may be It the
maycause
be theof cause
the difference in average
of the difference in distance
average
results between
distance results IHDCS
betweenand ESEM.and
IHDCS Furthermore, IHDCS results
ESEM. Furthermore, IHDCSthat results
considered
that more samples
considered are
more
more representative
samples than that of ESEM.
are more representative than that of ESEM.

4.3. Mechanical
4.3. Mechanical Analysis
Analysis
The unconfined
The unconfined compressive
compressive strength
strength (UCS),
(UCS), modulus
modulus of of elasticity
elasticity (MoE),
(MoE), modulus
modulus ofof rupture
rupture
(MoR), and splitting tensile strength as a function of density are separately shown in Figure
(MoR), and splitting tensile strength as a function of density are separately shown in Figure 13a–d. 13a–d.
The increase in density is accompanied by an increase in mechanical properties, which shows
The increase in density is accompanied by an increase in mechanical properties, which shows a a positive
correlation
positive betweenbetween
correlation mechanical properties
mechanical and density.
properties The values
and density. of mechanical
The values properties
of mechanical were
properties
approximated with linear functions, as shown in these figures.
were approximated with linear functions, as shown in these figures.
Materials 2020, 13, 2678 14 of 17
Materials 2020, 13, x FOR PEER REVIEW 14 of 17

Figure 13.
Figure Mechanicalproperties
13. Mechanical propertiesasasfunction
functionof
ofspecimen
specimendensity.
density. (a)
(a) UCS
UCS as
as aa function
function of
of specimen
specimen
density. (b) MoE as
density. as aa function
functionofofspecimen
specimendensity.
density.(c)(c)
MoR as as
MoR a function of specimen
a function of specimen density. (d) STS
density. (d)
as aas
STS function of specimen
a function of specimendensity.
density.

The batch 3 had the lowest mechanical properties, and it probably


The batch with
witha atarget
targetdensity
density of 400 kg/mkg/m
of 400 3 had the lowest mechanical properties, and it

reflected the fact that there was weak foam structure


probably reflected the fact that there was weak foam structure when specimens with lowwith
when specimens density,
lowon the other
density, on
hand, specimens with higher density would have better or stronger
the other hand, specimens with higher density would have better or stronger foam structure. foam structure.
Combining previous
Combining previousanalysis
analysisofof thethe
pore characteristics
pore characteristicsof ESEM and IHDC
of ESEM and image,
IHDC three
image, possible
three
factors are affecting the mechanical properties of LCC. The area ratio of pore
possible factors are affecting the mechanical properties of LCC. The area ratio of pore is an obvious is an obvious factor. It is
highly Itnegative
factor. is highly related
negativeto density,
related soto there
density,is aso
highly
therenegative
is a highlyrelationship between areabetween
negative relationship ratio of area
pore
and mechanical properties of LCC. When specimens with large area ratio
ratio of pore and mechanical properties of LCC. When specimens with large area ratio of the pore, of the pore, it means that
it
samples have less solid part in the cross-section. It also means that the average
means that samples have less solid part in the cross-section. It also means that the average thickness thickness between
pores is small.
between pores The decreased
is small. solid part solid
The decreased leads part
to weak
leads mechanical properties, because
to weak mechanical the because
properties, solid part theof
LCC is the main part to bear the load.
solid part of LCC is the main part to bear the load.
Another factor
Another factor isis the
the shape
shape of of the
the pore.
pore. Results
Resultsof ofcircularity
circularityandandsolidity
solidity have
haveshown
shownthat that D475
D475
and D600
and D600 have
have aa better
bettershape
shapeofofpore
pore than
thanthat of D400.
that of D400. Compared
Compared to D400, shapes
to D400, of bubbles
shapes of bubblesin D475in
and D600 are closer to true circle and furthermore, both of them contain less
D475 and D600 are closer to true circle and furthermore, both of them contain less touching bubbles. touching bubbles. Regular
bubble shapes
Regular bubbleand fewerand
shapes touching
fewerbubbles
touching are beneficial
bubbles are to the overall mechanical
beneficial to the overallproperties of the
mechanical
sample. Hence, the mechanical properties of D475 and D600 are better
properties of the sample. Hence, the mechanical properties of D475 and D600 are better than D400.than D400.
Although the
Although thecircularity
circularityand andsolidity of D475
solidity are slightly
of D475 better than
are slightly those
better thanof D600,
those itsofmechanical
D600, its
properties are
mechanical not better
properties arethan those of
not better thanD600.
those Theof main
D600.reasons
The main arereasons
that: onarethethat:
oneonhand, compared
the one hand,
with D475, D600 has a larger solid thickness, which improved the mechanical
compared with D475, D600 has a larger solid thickness, which improved the mechanical properties; properties; furthermore,
the distribution
furthermore, of its particle
the distribution size
of its is more
particle sizeconcentrated than D475,
is more concentrated thanwhich
D475, is also isbetter
which to its
also better
mechanical
to properties.
its mechanical properties.

5. Conclusions
Based on the above image processing and experimental results, the following conclusions can
be obtained.
Materials 2020, 13, 2678 15 of 17

5. Conclusions
Based on the above image processing and experimental results, the following conclusions can
be obtained.

(1) Based on the image processing results, IHDCS can obtain similar analysis results consistent with
ESEM. Besides, compared with ESEM, IHDCS can capture a larger range of pore structures faster
and more conveniently.
(2) There are strong correlations among pore area, perimeter, and major and minor axis. The lowest
correlation coefficient value is 0.88; shape descriptors also have high correlation coefficients,
but the maximum value is less than 0.8.
(3) Developed a method to calculate the average thickness of the bubble wall. The results show
that specimens with high densities have a significant average thickness value. In this study,
the average thickness value of D600 is more than 1.5 times that of low-density samples (D400,
D475).
(4) The lower the density of the specimen is, the higher the ratio of the bubble area to the total test
area. In this study, the pore area ratio of D400 is about 5% higher than that of D475. It is more
than 20% higher than that of D600.
(5) The pore area ratio, average thickness of bubble wall, and shape directors (circularity and solidity)
have strong correlations with the mechanical properties of LCC. These parameters could be useful
to have estimations of mechanical behavior of LCC.

Author Contributions: Conceptualization, W.Y., F.M.-W.N., and A.G.O.; Image processing, W.Y. and X.L.;
Experiments, F.M.-W.N. and A.G.O.; Image processing data curation, W.Y. and X.L.; Mechanical test data
curation, F.M.-W.N. and A.G.O.; Formal analysis, W.Y. and X.L.; Supervision, S.T.; Visualization, W.Y. and X.L.;
Writing—original draft preparation, W.Y. and X.L.; Writing—review and editing, W.Y., X.L., F.M.-W.N., and S.T.
All authors have read and agreed to the published version of the manuscript.
Funding: This research was funded by Chongqing Postdoctoral Science Foundation (grant number Xm2016126).
Acknowledgments: This research was supported by the Centre for Pavement and Transportation Technology
(CPATT) at the University of Waterloo and Chongqing Jiaotong University. The authors would like to express our
appreciation to CEMATRIX who provided lightweight cellular concrete specimens and experimental data.
Conflicts of Interest: The authors declare no conflict of interest.

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