Construction and Building Materials 251 (2020) 118954

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Construction and Building Materials

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

Strengthening mechanism of lightweight cellular concrete filled with fly

ash
Xin Liu a,b,⇑, Chengwei Ni a, Ke Meng a, Liye Zhang a, Dongxu Liu b, Lizhi Sun b,⇑
a
Key Laboratory of Ministry of Education for Geomechanics and Embankment Engineering, Institute of Tunnel and Underground Engineering, Hohai University, Nanjing 210098, China
b
Department of Civil and Environmental Engineering, University of California, Irvine, CA 92697-2175, USA

h i g h l i g h t s

Lightweight cellular concrete (LCC) filled with fly ash (LCCFFA) is developed.

Strengthening mechanism of LCCFFA is revealed from microstructure point of view.

25% content of fly ash is recommended with the Si/Ca ratio as a judging criterion.

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

Article history: Fly ash has been used to fill the lightweight cellular concrete (LCC) as the primary admixture to promote
Received 16 November 2019 comprehensive engineering applications. However, the strengthening mechanism of LCC resulted from
Received in revised form 7 March 2020 fly ash is not well understood. In this paper, the strengthening mechanism of LCC filled with fly ash
Accepted 30 March 2020
(LCCFFA) was investigated with respect to the microstructures including porosity and skeleton character-
istics. The variation rules of average pore size (PS), pore roundness value (PRV), and fractal dimension of
pore distribution (FDPD) with different fly ash contents were explained. The relationship between micro-
Keywords:
scopic parameters of PS, PRV, and FDPD and the overall compressive strength, along with the wet bulk
Lightweight cellular concrete
Fly ash
density was established. Furthermore, the difference of skeleton structure evolution mechanism between
Microstructure LCC and LCCFFA was investigated with the results showing that the difference comes from the effects of
Porosity ball and particle filling of fly ash when before 28 days. While after 28 days, the pozzolanic reaction of fly
Skeleton structure ash and hydration reaction of cement mutually promote the densification of skeleton structure. Finally,
Strengthening mechanism the SEM energy spectrum diagram was analyzed to further reveal the strengthening mechanism. From
the perspective of characteristic pore parameters and skeleton hydration products, the recommended
content of fly ash is approximately 25%. The ratio between Si and Ca (Si/Ca) can determine the degree
of reaction of fly ash, and can therefore be used as a judging criterion to determine whether the content
of fly ash is appropriate.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction
Since its first development in the 1920s [1] and as a subgrade
fill in Japan in 1980s for road engineering [2], lightweight cellular
concrete (LCC) [3] has been found as a new class of geotechnical
engineering materials with such attractive properties as light-
weight, high strength, good fluidity, and thermal insulation [4,5].
LCC has been applied in the underground pipeline landfill and cav-
⇑ Corresponding authors at: Key Laboratory of Ministry of Education for
Geomechanics and Embankment Engineering, Institute of Tunnel and Underground
Engineering, Hohai University, Nanjing 210098, China (X. Liu); Department of Civil
and Environmental Engineering, University of California, Irvine, CA 92697-2175,
USA (L. Sun).
E-mail addresses: liuxin100@hhu.edu.cn (X. Liu), lsun@uci.edu (L. Sun).
ity filling as well as in highway embankment filling [6], with good
engineering applications [7]. Experimental studies primarily focus
on the compressive strength, wet density, thermal insulation, pore
structure, material durability, and service life [8–10].
As a cement-based material, LCC forms a microstructure with
pores through the introduction of foam. The pore structure and
porosity affect the physical and mechanical properties of LCC.
Wee et al. [11] found that the compressive strength improved with
decreasing the average porosity. Kikuchi et al. [12] analyzed the
effect of foam content on the internal pore structure. Ma et al.
[13] acquired that a high foam and micropore content significantly
improved the thermal insulation and hygroscopic property, while
the compressive strength decreased as the inner pores became lar-
ger. Chen et al. [14], based on the microscopic characteristics of the

https://doi.org/10.1016/j.conbuildmat.2020.118954
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 X. Liu et al. / Construction and Building Materials 251 (2020) 118954
pore distribution in the river silt bubble-mixed soil, indicated that
the internal micro-structure had a significant impact on its local
stress distribution and final failure mode, while the properties of
internal pores affected the strength and durability of LCC. Mean-
while, Luo et al. [15] detected that adding multi-walled carbon
nanotubes could enhance the uniformity of foam distribution in
foamed cement and reduce the foam size. The above research
efforts all indicate that pores affect the properties of LCC.
In addition to pores, the effect of skeleton structure has been
investigated on the strength mechanism of LCC. Kamei et al. [16]
showed that the strength of LCC increases first and then decreases
with the addition of calcined gypsum. Wang et al. [17] conducted a
direct shear test and unconfined compressive strength test on the
sludge lightweight soil samples that were solidified by foam and
cement. The effect of the curing period and cement content on
the strength and failure mode was analyzed. To verify the
microstructure of LCC and its characters of compressive strength,
Qiu et al. [18] selected samples with different water-cement ratios
and scanned the microstructure characters by an electron micro-
scope. The results demonstrated that the water-cement ratio has
a prominent effect on the microstructure and compressive strength
of LCC. Gökçe et al. [19] studied the effects of foam content as well
as fly ash and silica fume inclusion on some physical and mechan-
ical properties of foam concrete, subjected to various curing
regimes. Besides, Liu et al. [20] proposed a durability assessment
method of LCC. The above studies indicate that the cement skele-
ton structure is the primary source of LCC strength.
Since the end of the last century, fly ash has become one of the
most reusable industrial waste materials [21–25]. As the primary
admixture, fly ash has been gradually added to LCC from the turn
of the century to improve the strength and fluidity, reduce the
use of cement, save cost, and decrease energy consumption. Specif-
ically, Kearsley et al. [26] observed that the foamed concrete with
high ash contents might need a more extended period to reach
their ultimate strength, which could be higher than that using only
cement. Krivenko et al. [27] used the alkali-activated fly ash as an
additive and obtained the heat resistance of cellular concrete.
Neramitkornburi et al. [28] and Horpibulsuk et al. [29] found that
adding a certain amount of fly ash can improve the wetting
strength and fluidity and thus improve the durability of LCC. Liu
et al. [30] proposed to use fly ash to improve LCC for bridge backfill
structures. Its weight is twice as light as fly ash as a single backfill,
while not affected by rolling and water permeability. Besides, Liu
et al. [31] studied the construction techniques and quality control
measures of LCC mixed with fly ash and verified the feasibility of
the optimal mixture ratio. The above investigations have consid-
ered fly ash as an improving material to be incorporated into
LCC. The different mixture ratio and fly ash content affect the
hydration process of cement, thereby affecting the cement skeleton
structure, and the incorporation of fly ash will change the proper-
ties of internal pores of LCC. However, studies on the strengthening
mechanism resulted from fly ash are not well understood.
In this paper, fly ash is used as the primary admixture to pre-
pare a new class of lightweight cellular concrete filled with fly
ash (LCCFFA) for subgrade filling, aiming to reveal the strengthen-
ing mechanism from following investigations. Microstructural
characterizations are carried out, including the pore and skeleton
tests. The pore test refers to the optical and X-ray microscopy
(XRM) nano-CT observations, and the skeleton test is conducted
with the scanning electronic microscopy (SEM). The microscopic
pore size (PS), pore roundness value (PRV), and fractal dimension
of pore distribution (FDPD) are characterized, followed by the anal-
ysis of the effects of pore structure parameters on the overall
strength of LCCFFA. The strength formation process with the
growth of age is further studied. Finally, the energy spectrum dia-
gram of the LCCFFA skeleton is investigated to reveal the strength-
ening mechanism of fly ash filled LCC.
2. Materials and methods
2.1. Constituents
The materials used in this study are as follows. 42.5R ordinary
Portland cement is produced from Zhonglian Cement Factory, Nan-
jing, China. Its specific gravity is 3.1 kg/m3, and its particular sur-
face area is 256 m2/kg. Fly ash is acquired from Henan Yulian
Power Plant, Zhengzhou, China. Its density is 2.05g/cm3. The chem-
ical compositions of cement and fly ash are shown in Table 1.
Specific information about fly ash is shown in Table 2. The com-
pound foaming agent is a light transparent liquid, made from a
combination of pollution-free animal and plant proteins with no
negative effect on the environment.
2.2. Mixing ratio of fly ash
According to the CJJ 177 Standard [32], the common mixing
ratio was selected when the wet density is 7.0 kN/m3, resulting
in the strength of 1.0 MPa. The test adopts the single factor test
method. The rate of water to cement and fly ash keeps constant
at 0.58, and foam usage is 703 L/m3. Only the mixing ratio of fly
ash to cement changes. Specific details are shown in Table 3.
In the process of sample preparation, we intended to keep the
wet density constant by controlling the mixing ratio, stirring time
and stirring rate. We took into account the reduction of foam due
to agitation and vibration. The defoaming time is approximately
10 min, about the same as the stirring time. Therefore, we slightly
increased the content of components of LCC so that the error with
the design density did not exceed 5%.
The LCC slurry was stirred in a circular container and the mixing
performance was operated by a special agitator. The rotating
radius of the agitator is about half the radius of the container. Dur-
ing mixing, stir the slurry counterclockwise along the sides of the
container, then in the middle to ensure the uniformity of the slurry.
2.3. Sample preparation
The samples were prepared in the following three steps.
(1) Preparing cement slurry and foam: The water, cement, and
fly ash were weighed, mixed, and then stirred well until
the slurry contains no large particles. The foaming liquid
used is a self-made compound foaming agent with a dilution
ratio of 40 times. With stirring of solution evenly, a foam
generator was applied to produce foam.
(2) Mixing and pouring: The foam measured in a beaker was
poured into the cement slurry, followed by the slurry stir-
ring for 5 min until it was homogeneous and stable. The
slurry was poured into the 100 mm  100 mm  100 mm
cubic cast iron molds covered with vaseline.
(3) Curing: The molds were covered with plastic wrap after
pouring to prevent moisture from fast evaporation. The sam-
ples were demoulded after curing for 24 h at a constant tem-
perature of (21 ± 6) °C, following the curing process outlined
in ASTM C495/C495M-12 [33]. The samples were sprinkled
water indoors to the design curing age after numbering.
The frequency of watering was once every five days.
 X. Liu et al. / Construction and Building Materials 251 (2020) 118954 3

Table 1
Material Chemical Compositions (%).

Material SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SO3

cement 20.32 4.86 4.99 65.45 1.25 0.15 0.4 2.10
fly ash 58 30 4.3 1.5 2.8 3.2 1.2 0.88

Table 2 factor. Through the statistical analysis of the binary image by GeoI-
Test items and results of fly ash (%). mage program, pore characteristics can be obtained.
45-lm sieve the ratio of water water ignition The self-compiled GeoImage program was utilized to analyze
residues demand content loss the microstructure image, and the threshold value method was
8.6 93.5 0.95 4.3 used to binarize the microstructure. In the binary image, the black
area represents the pores, while the white area represents the
skeleton, shown in Fig. 1. Through the statistical calculation of
Table 3 the binary image, the average pore size (PS), the pore roundness
Single-factor test protocol for mixing ratio of fly ash to cement. value (PRV), and the fractal dimension of pore distribution (FDPD)
No. Variable Cement Fly ash
can be obtained. The above parameters take the arithmetic mean of
(kg/m3) (kg/m3) three calculations.
A0 0% 400 0
The parameters were obtained after the samples were cured for
A15 15% 340 60 28 days. At the same time, the unconfined compression test was
A25 25% 300 100 carried out following the test procedure outlined in ASTM C495/
A35 35% 260 140 C495M-12 [33].
A45 45% 220 180
SEM test (S-3400 NⅡ, Hitachi, Japan) was employed to study the
A55 55% 180 220
skeleton structure of LCC and LCCFFA. The 5 mm  3 mm  1 mm
Note: Fly ash substitutes the same amount of cement. samples were naturally air-dried and then painted with metal to
increase the electrical conductivity and to obtain a clear and accu-
rate image. The microscopic images with a magnification of 1000
2.4. Microstructural characterization
times and 3000 times were used to extract the size parameters
of particles and pores, and analyze the evolution process of hydra-
The pore information on the surface and inside the sample was
tion products, respectively. Samples were taken at 7 days, 28 days,
captured by the optical test and X-Ray microscopy (XRM) nano-CT
56 days, and 90 days for the SEM test and the unconfined compres-
test, respectively. The image acquisition system of the optical test
sive strength test.
consists of a long-distance microscope, a CCD camera, a light
source, and an image capture card. It can enlarge the sample sur-
3. Results and discussion
face by 150 times and save the image as a BMP format. The XRM
nano-CT scanner is Zeiss/Xradia 410 Versa that has a spatial resolu-
3.1. Analysis of porosity test results
tion of 0.9 lm. In the present use, the resolution is 25 lm. It is
noted that the Mercury Intrusion Porosimetry can be suitable for
As mentioned above, surface and internal pores can be captured
the analysis of pore distribution. The technology considers both
by the optical and Nano-CT tests, respectively. The Nano-CT test
the large pores in the material and the tiny cracks between the
can provide an intuitive visualization of the interior pore structure
skeleton structure, while the latter has little effect on the current
of the sample, but the 16-bit grayscale image data is enormous,
study. To be precise, this research mainly studies the characteris-
which requires a lot of resources in post-image processing. From this
tics of pores introduced by the physical foaming method. Further-
perspective, the optical test can obtain the data of sample surface
more, X-Ray CT scans can provide an effective method to
pores more appropriately. To improve experiment efficiency and
characterize the pore structure of LCC, which can be used to char-
save cost, we selected sample A35 to do the optical test and Nano-
acterize the pore size distribution, macro porosity, and pore shape
CT test, then statistically analyzed its surface and internal pore struc-

Fig. 1. Microstructure (a) and its binary image (b) of the sample.
4 X. Liu et al. / Construction and Building Materials 251 (2020) 118954

Fig. 2. Slice selection and the binary representation of CT sample (First column images: A35 CT model and the surface of the sample with Nano-CT slice. Second column
images: (a), (b), and (c) are the binary image inside the sample with Nano-CT slices. Third column images: original grayscale image and its binarization image.

ture by GeoImage program. The binary image on the left in the Fig. 2
is the surface of the sample (with Nano-CT slice number 1), and (a),
(b) and (c) are the binary image inside the sample (with Nano-CT
slice number 117, 235 and 325 respectively). With the selected slices
and the GeoImage program to analyze the microstructure images,
the results are shown on the right of Fig. 2.
Through the statistical calculation of the binary image, the his-
tograms of PS and PRV are shown in Figs. 3 and 4, and FDPD in
Table 4. In particular, in the PRV distribution histogram, the range
of 1 to 1.2 represents PRVs = 1, meaning that the pore shape is
circular.

Fig. 4. PRV histogram of LCCFFA with different Slice.

Table 4
The change of FDPD with different slice.

Slice No. 1 117 235 352

Da 1.621 1.684 1.643 1.649

To compare the difference between the optical and Nano-CT

test results, the following formula was defined:
 
P  P 
 1 
dP ¼     100% ð1Þ
 P 
Fig. 3. PS histogram of LCCFFA with different Slice.
 X. Liu et al. / Construction and Building Materials 251 (2020) 118954 5

Fig. 5. PS distribution curves of LCCFFA with different fly ash contents.

where P 1 represents the pore parameter value of slice number 1 and inhomogeneity. In the samples with different fly ash contents, the

P represents the mean pore parameters value of slice number 1, Cu and Cc of A25 samples are closest to those of the A0 samples,
117, 235, and 325. According to Eq. (1), dPS ¼ 4:77% , indicating that its PS with 25% fly ash content is closest to that of
dPRV ¼ 2:19% and dFDPD ¼ 1:71% , all less than 5%. Therefore the the A0 sample.
sample can be considered homogeneous, and the pore structure of
sample surface can be fully representative of the whole sample. 3.1.2. Evolvement rule of PRV
Through the analysis of the binary images of pore structure on PRV refers to the degree that the shape of the pore deviates
the surface of the sample with different mixing ratios by the opti- from the circle in the two-dimensional plane. The closer the value
cal test, PS, PRV, and FDPD were obtained. Based on this, the fol- is to 1, the more the shape of the pore tends to be round. The more
lowing discussion can be made. circular the pore is, the more uniform the force is, and the higher
the resistance to pressure. PRV can be determined as:
3.1.1. Evolvement rule of PS Ra ¼ 4pSa =La 2 ð4Þ
Fig. 5 shows the PS distribution curves of LCCFFA with different
fly ash contents. According to the curves, two indexes are deter- where Ra is the pore roundness value, Sa is the pore area, and La is
mined, reflecting the uniformity of PS and the shape of the curve. the pore circumference.
Mathematically, the non-uniformity coefficient Cu and the curva- Fig. 6 shows the PRV histogram of LCCFFA with different fly ash
ture coefficient Cc are calculated from contents. It is found that the pore structure of A0 samples are the
most circle, the PRVs = 1, with a percentage of 61%. The PRVs of
d60
Cu ¼ ð2Þ A15 samples are primarily within the range of 0.8 to 1 and PRVs = 1.
d10 The percentages are almost equal, all slightly greater than 40%. The
percentage of A25 samples with PRV = 1 is 56%, slightly lower than
2
d30
Cc ¼ ð3Þ
d60  d10
where d10, d30, and d60 are the specific sizes when the number of
pores (which PS is smaller than this specific size) accounts for
10%, 30%, and 60% of the total number of pores, respectively. The
detailed information is shown in Table 5.
As shown from Table 5, the Cc is between 1.1 and 1.6; Cu of A0,
A15, A25, A35 samples is less than 5, while the Cu of the A45 and A55
samples is greater than 5. The results demonstrate that, as the fly
ash content increases, the number of big pores increases, while
the number of small pores decreases, indicating the rise of the pore

Table 5
Worksheet of average PS, Cu, and Cc.

NO. Cu Cc d
A0 2.39 1.105 0.075
A15 3.82 1.208 0.15
A25 3.05 1.168 0.105
A35 3.85 1.244 0.196
A45 5.17 1.464 0.277
A55 6.36 1.526 0.384

Note: d is the average PS of the sample Fig. 6. PRV histogram of LCCFFA with different fly ash contents.
6 X. Liu et al. / Construction and Building Materials 251 (2020) 118954

that of A0 samples. The PRVs of A35 and A45 samples are mainly dis- Based on the three microscopic parameters, it is found that the
tributed in the range of 0.8 to 1. The A55 samples’ PRVs are in the parameters of sample A25 are closest to sample A0. In other words,
range of 0.6 to 0.8, which are much higher than the other samples. when the fly ash content is 25%, the characteristic parameters are
Above all, with the increase of fly ash content, the PRV first relatively optimal.
decreases then increase and decrease at last. The results indicate
that the incorporation of fly ash generally increases PRV, and the
stress capacity decreases. However, when the fly ash content is 3.1.4. Effect of pore structure parameters on the strength of LCCFFA
25%, its PRV is closest to that of the A0 sample. The average PS, PRV, and the FDPD of all the samples were
arranged in ascending order, respectively. And then, the curves of
3.1.3. Evolvement rule of FDPD strength and wet density of 28 days’ curing time with the change
The FDPD is a microscopic characteristic parameter to describe of three microstructural parameters are drawn respectively, as
the uniformity of pore dispersion in three-dimensional space. The shown in Figs. 7 to 9.
smaller the FDPD is, the more uniform the distribution of pores will As seen from Figs. 7 to 9, with the increase of the average PS, the
be, and the greater the density and intensity will be. On the con- strength and wet density of LCCFFA decreases logarithmically,
trary, if the pore distribution is more concentrated, the weak sur- shown as:
face will be formed in the pore aggregation, which is unfavorable
to the strength. The method of calculating FDPD by the GeoImage qu ¼ 0:329lnðdÞ þ 0:343 ð6Þ
program is shown as follows. The image is divided into orthogonal
grids of (L/b)  (L/b) with a square of side length L. The number of
c ¼ 1:047lnðdÞ þ 0:624 ð7Þ
grids containing pores (including incomplete pores) is counted,
and denoted as N(b). The size of b is arranged from small to large, With the increase of PRV, the strength and wet density of
and the corresponding number of grids can be obtained. With Lnb LCCFFA decrease linearly as:
as the abscissa and LnN (b) as the ordinate, the curve of LnN
(b) ~ Lnb is drawn, namely: qu ¼ 1:984Ra þ 0:892 ð8Þ
LnN ðbÞ ¼ C  Da Lnb ð5Þ
c ¼ 6:252Ra þ 14:536 ð9Þ
where the slope factor Da is the FDPD, and C is constant.
Table 6 shows the change of FDPD under different fly ash con- With the increase of FDPD, the strength and wet density of
tents. It can be found that FDPD is close to each other, and is con- LCCFFA decrease linearly as:
centrated in the range of 1.64–1.72. It indicates that the effect of fly
ash content on FDPD is not obvious. When fly ash is added at 25%, qu ¼ 5:370Da þ 9:884 ð10Þ
the FDPD is minimal.
c ¼ 19:738Da þ 39:348 ð11Þ
Table 6
The change of FDPD. where qu is the 28-day strength of LCCFFA, cis the wet density of
Sample No. A0 A15 A25 A35 A45 A55 LCCFFA, d is the average of PS, Ra is the average of PRV, and Da is
the average of FDPD. Further, in Figs. 7 to 9, R2 is the value of coef-
Da 1.666 1.657 1.644 1.652 1.682 1.709
ficient of correlation.

Fig. 7. Average PS curves of strength and wet density of 28-day curing time.
 X. Liu et al. / Construction and Building Materials 251 (2020) 118954 7

Fig. 8. Average PRV curves of strength and wet density of 28-day curing time.

Fig. 9. FDPD curves of strength and wet density of 28-day curing time.

3.2. Analysis of SEM test results
The pore test results show that the LCCFFA with a 25% mixing
ratio of fly ash has better performance. As a result, samples of A0,
A25 are selected to explore the skeleton structures of LCC and
LCCFFA by SEM. Specifically, SEM images with 3000 magnification
were used to analyze the improvement of cement hydration prod-
ucts and fly ash. Further, SEM images with 1000 magnification
were used to quantify the evolvement rule of the hydrated agglom-
erate particles, pores and fly ash particle size with age increasing.
The parameter definition is shown in Table 7.
3.2.1. Skeleton microstructure of LCC
Fig. 10 shows SEM images of the A0 sample cured for 7 days. As
seen from Fig. 10 (a), the cement hydration products are mainly
acicular ettringite, C-S-H gel, and plate-like Ca(OH)2 crystals. At
this time, C-S-H gel has not yet hardened and is mainly reticular
or fibrous, with low strength and easy to break. Therefore, the
8 X. Liu et al. / Construction and Building Materials 251 (2020) 118954

Table 7
SEM parameter definition.

NO. Maximum pore length (lm) Maximum pore width (lm) Hydration particle diameter (lm) Fly ash particle diameter (lm)
A0 Lx0 Wx0 Gx0 \
A25 Lx25 Wx25 Gx25 Fx25

Note: The superscript  (unit: day) was the curing time, and the values were 7, 28, 56.

Fig. 10. SEM image of A0 cured for 7 days.

0 is 10 lm smaller than W0,

structure is fragile. There are many groups of agglomerate particles
in Fig. 10 (b). They are mainly in point contact, with clear bound-
aries and large pores. According to the size of SEM calibration, G70
is 10 lm, L70 is 30 lm, and W70 is 15 lm.
Fig. 11 shows SEM images of the A0 sample at 28 days. From
Fig. 11 (a), the newly formed hydration product gradually expands
into the intercalary space. Particles formed by the combination of
C-S-H gelled and Ca (OH)2 crystals are flocculated. The skeleton
has formed a close and stable microstructure. In Fig. 11 (b), com-
pared to 7 days, the boundaries between these hardened particles
become obscured. The bonging mode changes from point contact
to edge contact. According to the size of SEM calibration, G28 0 is
23 lm bigger than G70, which shows that cement hydration has
been going on from 7 to 28 days. The new hydration products con-
0 is 20 lm smaller
tinue to gather and harden into blocks finally. L28
than L70, which is a 33.33% decrease. W28 7
which is a 50% decrease. The results demonstrate that the intensity
of this period has increased significantly when compared to 7 days.
SEM image of the A0 sample at 56 days (Fig. 12 (a)) shows that
the hydration products overlap one another and gradually cover
the pores. In Fig. 12 (b), there are almost no single particles in
the structure, and the whole structure is lamellate. According to
the size of SEM calibration, both L560 and W0 are equal to 7 lm.
56
Compared to 28 days, the structure becomes more compact and
denser at this time. The intensity will also increase to a certain
extent.
3.2.2. Skeleton microstructure of LCCFFA
Fig. 13 shows SEM images of the A25 sample at 7 days. The sur-
face of particles is covered with C-S-H gelation and Ca (OH)2 crystal

Fig. 11. SEM image of A0 at 28 days.

X. Liu et al. / Construction and Building Materials 251 (2020) 118954 9

Fig. 12. SEM image of A0 at 56 days.

Fig. 13. the SEM image of A25 at the age of 7 days.

Fig. 14. A25 at 28-day age SEM image.

10 X. Liu et al. / Construction and Building Materials 251 (2020) 118954
(Fig. 13 (a)). The growing ettringite distributes among particles
(Fig. 13 (b)). At this stage, the fly ash does not participate in the
reaction. It is difficult to distinguish between fly ash particles
and cement hydration products. According to the size of SEM cali-
bration, both G725 and G70 are equal to 10 lm, which is similar to the
A0 sample. The F725 is between 7 lm to 18 lm. L725 is 27 lm, and
W725 is 10 lm, which is like the L70 and W70, respectively. Overall,
the number of pores in the A25 sample is larger than that in the
A0 sample, indicating that the pore size of the fly ash sample is
smaller than that of the sample without fly ash. However, the num-
ber of pores in the fly ash sample is larger because of the ball effect
of fly ash. Fly ash particles are smooth spherical beads. Under the
same conditions, the spherical particles flow better than any other
shape of the particles. Therefore, at the age of 7 days, the fly ash
particles mainly disperse the cement particles evenly and reduce
cement aggregation. Thereby, the hydration products are uni-
formly distributed, and the larger pores are subdivided into smaller
ones.
Fig. 14 shows the SEM images of the A25 sample at 28 days. It is
seen from Fig. 14 (a) that the fly ash has formed a hardened shell,
indicating that the volcanic ash reaction has taken place in fly ash.
The hardened shell is formed in two parts. On the outside, it is
made of cement-hardened C-S-H. In the interior, it is formed by
the C-S-H gelation of the fly ash generated by the volcanic ash reac-
tion. The hardening surface of the shell is also attached to the
uncured C-S-H gel. This phenomenon is called ‘‘etching”, which
occurs mainly because the calcium ions react with the active com-
ponents in the fly ash. In other words, the volcanic ash reaction of
the fly ash consumes calcium ions, resulting in a decrease in the
concentration of calcium ions in the slurry, thereby promoting fur-
ther hydration reaction. The further hydration products continue
to adhere to the surface of fly ash particles, providing calcium ions
for the following volcanic ash reactions:
Hydration reaction þ
Cement þ H2 O ! Ca2 þ C - S - H Gelling
þ Volcanic ash reaction
Fly ash þ Ca2 ! C - S - H Gelling
Fig. 14 (b) further shows an SEM image of A25 sample magnified
1000 times at 28 days. The sample is more compact at 28 days than
that in seven days. The fly ash is evenly distributed in the structure,
which causes the cement to disperse, reflecting the ball effect of fly
ash. According to ASTM C618 [34], the fly ash 45 lm sieve residue
shall not exceed 20%. Small fly ash particles can fill the pores of the
Fig. 15. A25 in the 56d age SEM image.
system to make the structure more compact, besides Fig. 14 (b) can
reflect the particle filling effect of fly ash. After the measurement,
for the A25 sample, L28 25 is 18 lm, and W25 is 6 lm, smaller than
28
L25 and W25, respectively, and smaller than L28
7 7 28
0 and W0 , respec-
tively. F28
25 is between 13 l m and 25 l m, which is larger than F725,
indicating that the hydration products on the surface of fly ash
become thicker and the hydration reaction continues.
Fig. 15 shows the SEM images of the A25 sample at 56 days. It
can be seen from Fig. 15 (a) that the hydration products are inte-
grated into one piece. The surface is still covered with uncured
C-S-H gel and ettringite. The phenomenon of ‘‘etching” is obvious.
Fig. 15 (b) shows that the volcanic ash reaction has been continu-
ously reacting. The structure of the A25 sample is full of newly
formed cement hydration products. The volcanic ash reaction of
fly ash and cement hydration complement each other. There are
fewer pores in the structure, and the strength is further increasing.
For SEM images of A0 and A25 samples at different ages, which is
magnified 1000 times, the GeoImage program is utilized for the
analysis. The curves of porosity and unconfined compressive
strength, along with curing days, were obtained, as shown in
Fig. 16. The porosity of the A25 sample was greater than that of
the A0 sample before 28 days. However, the above conclusion
shows that L725 < L70, W725 < W70, L28 28 28 28
25 < L0 , W25 < W0 , the size of a
single pore of A25 sample is smaller than that of the A0 sample.
The result indicates that the fly ash mainly reflects a ball effect
and a particle filling effect and plays a role of dispersing the hydra-
tion products and filling the pores in the first 28 days of curing.
After 28 days, the porosity of the A25 sample decreased signifi-
cantly more than that of the A0 sample. Until 56 days, it was smal-
ler than the A0 sample and continued to decrease. At the same
time, after 28 days, the trend of strength increase of A25 sample
is also greater than that of A0 sample until 56 days when it is
slightly stronger than A0 sample. The result shows that after
28 days, the volcanic ash effect and the hydration reaction of fly
ð12Þ ash jointly promote the strength increase so that the A25 sample
with less cement content obtains the same strength as the A0
sample.
ð13Þ
3.2.3. Energy spectrum diagram analysis of skeleton structure
To further study the influence of fly ash on chemical element
composition changes of LCCFFA and C-S-H gel, the energy spectra
of A0, A25, and A45 at the age of 7 and 90 days were analyzed,
and the chemical elements were semi-quantitatively calculated.
Figs. 17 to 19 are SEM energy spectra of samples with and without
 X. Liu et al. / Construction and Building Materials 251 (2020) 118954 11

Fig. 16. Curves of porosity and unconfined compressive strength along with the change of curing age.

Fig. 17. SEM energy spectrum of samples without fly ash.

fly ash at 7 and 90 days. Table 8 shows the calculation table of the
atomic percentage.
It can be seen from the test results that the samples without fly
ash are mainly composed of Ca, Si and O elements, and contain a
small amount of Al and S. With the increase of fly ash content, Si
increases, Al increases slightly, and Ca decreases. The results indi-
cate that the content of Si and Al in fly ash is relatively large, while
the content of Ca is relatively small. According to the molecular
formula of C-S-H gel, the ratio between Si and Ca(Si/Ca) is 2:3.
Therefore, if the Si/Ca rate is close to 2:3, Si and Ca are balanced,
meaning that the chemical reaction is sufficient, and more C-S-H
gels will be produced.
For the sample without fly ash, due to the low Si content of
cement, the imbalance of Si and Ca appears, Si/Ca is around 0.53.
When the fly ash content is 25% with the age being 90 days, Si/
Ca is close to 2:3, Si and Ca are balanced, and more C-S-H gels will
be produced, indicating that the ideal fly ash content is 25%. When
the fly ash content is 45%, Si/Ca is more than 0.7, Si and Ca are not
balanced again. Combined with the analysis of pore and skeleton
structure, the recommended fly ash content is approximately 25%.
Also, it can be seen from Table 8 that Si/Ca increases with the
increase of age and fly ash content. The phenomenon indicates that
in the reaction process, hydration products are constantly con-
verted to each other, so that Si/Ca is not fixed. However, when
the reaction is sufficient to form a stable structure, Si/Ca hardly
changes. If the fly ash content is appropriate, Si/Ca keeps at around
2:3. Therefore, it is considered in this paper that the sample with
25% fly ash content has sufficient pozzolana reaction at 90-day
12 X. Liu et al. / Construction and Building Materials 251 (2020) 118954

Fig. 18. SEM energy spectrum of samples with 25% fly ash.

Fig. 19. SEM energy spectrum of samples with 45% fly ash.

Table 8
Calculation table of atomic percentage.

atomic without fly ash 25% fly ash 45% fly ash
7d 90d 7d 90d 7d 90d
O 54.12 54.14 51.18 53.24 50.87 53.76
Al 2.65 2.10 2.89 3.08 3.70 3.42
Si 14.19 14.66 16.82 16.51 17.55 17.40
S 1.24 1.47 1.18 1.27 0.87 1.13
K 0.54 0.29 0.61 0.26 0.89 0.26
Ca 26.80 26.84 26.68 25.01 24.60 23.32
Fe 0.45 0.48 0.64 0.62 0.76 0.70
Si/Ca 0.5295 0.5462 0.6304 0.6601 0.7134 0.7461

age; the structure is stable, and the strength hardly increases with 4. Conclusions
the growth of age. In conclusion, Si/Ca can be used as a judge cri-
terion to measure the degree of reaction of fly ash, and determine This study regards fly ash as the primary admixture to mix with
whether the content of fly ash is appropriate. LCC for subgrade filling. The microstructure tests were carried out,
 X. Liu et al. / Construction and Building Materials 251 (2020) 118954
including the optical test, Nano-CT test, and skeleton SEM test. The
strengthening mechanism of fly ash filled LCC is revealed, and the
recommended mixing ratio is determined. The main conclusions
are as follows:
(1) The pore tests, including the optical and Nano-CT test, show
that, with the increase of fly ash content, the PS increases
initially, then decreases and increases afterward. The PRV
is opposite while the FDPD decreases initially and increases
eventually. The unconfined compressive strength and wet
bulk density of LCCFFA decrease logarithmically with the
increase of PS, while decreasing approximately linearly with
the rise of PRV and FDPD.
(2) The skeleton microstructures show that, with the increase of
curing age, the skeleton structure of LCC gradually hardens
into blocks from the clumps. The bonding mode changes
from point to edge contact, and finally grows in layers. Also,
the results of quantitative analysis and comparison of the
samples without fly ash and with 25% fly ash indicate that
fly ash mainly reflects the ball effect and particle filling
effect before 28 days. After 28 days, the pozzolanic reaction
of fly ash and hydration reaction of cement in LCCFFA mutu-
ally promote the densification of skeleton structure.
(3) Combined with the analysis of optical and SEM tests, the rec-
ommended mixing ratio of fly ash is approximately 25%. The
ratio between Si and Ca (Si/Ca) can measure the degree of
reaction of fly ash, which can also be used as a judge crite-
rion to determine whether the fly ash content is appropriate.
This research allows researchers and engineers to better grasp
the properties of LCC, so as to correctly guide the construction in
terms of quality control and construction technology. Through con-
trolling the mixing ratio, mixing process and curing measures,
more ideal physical and mechanical properties of LCC can be
obtained. In addition, it is easy to understand the cracks and dam-
age caused by the deterioration of pores and skeletons, so as to
make timely remedial measures and improve the construction
process.
CRediT authorship contribution statement
Xin Liu: Conceptualization, Methodology, Supervision, Funding
acquisition, Writing - original draft. Chengwei Ni: Formal analysis,
Resources, Writing - original draft. Ke Meng: Resources, Data cura-
tion, Visualization. Liye Zhang: Formal analysis, Data curation,
Visualization. Dongxu Liu: Investigation, Resources, Writing -
review & editing. Lizhi Sun: Conceptualization, Methodology,
Supervision, Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgments
This study was sponsored by the National Natural Science Foun-
dation of China (Grant No. 51609071) and the Fundamental
Research Funds for the Central Universities (Grant No.
B200202087, 2018B13714). In addition, Xin Liu’s study at UC Irvine
was supported by the China Scholarship Council (Grant No.
201806715014).
13
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